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  • 1990-1994
  • 1985-1989  (1,737)
  • 1987  (1,737)
  • Analytical Chemistry and Spectroscopy  (1,177)
  • Biochemistry and Biotechnology  (560)
Source
Material
Years
  • 1990-1994
  • 1985-1989  (1,737)
Year
Keywords
  • 1
    Electronic Resource
    Electronic Resource
    Detection and identification of three thioether conjugates of 2-hydroxyacetanilide by liquid chromatography/electrochemistry (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 24-29 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The three 2-mercaptoethanol (ME) thioether conjugates of 2-hydroxyacetanilide (2HAA) are detected and identified using liquid chromatography/electrochemistry (LC/EC). The conjugates are produced either by incubations of 2HAA with liver microsomes in the presence of NADPH and ME or by chemically oxidizing a solution of 2HAA and allowing it to react with ME. Identification of the three isomers is based on retention time and comparison of the electrochemical behavior of model compounds.Production of the three isomers by microsomal protein occurs only in the presence of NADPH and shows that 2HAA proceeds through a cytochrome P-450 mediated pathway to a reactive intermediate similar to acetaminophen, possibly N-acetyl-o-quinoneimine.The relative percentages of each isomer produced were calculated as the percentage of the total peak areas of the isomers. Compound A (2HAA-5-ME) is produced in 53.7% and 24.6%, compound B (2HAA-4-ME) is produced in 16.2% and 70.3% and compound C (2HAA-3-ME) is produced in 30.1% and 5.1% by microsomal incubations and chemical oxidation respectively.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020108
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  • 2
    Electronic Resource
    Electronic Resource
    Determination of 3, 4-dihydroxyphenylglycol (DHPG) by HPLC with coulometric detection, and correlation with 3-methoxy-4-hydroxyphenylglycol (MHPG) in human plasma (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 30-33 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A method for determining plasma 3,4-dihydroxyphenylethyleneglycol (DHPG), a central noradrenaline (NA) metabolite, is described. The method used HPLC with dual coulometric detection set in screen mode of operation. The isolation of DHPG and related catecholamines (noradrenaline, dopamine and dihydroxybenzylamine) was performed on acid washed alumina extracted with 0.2 M HClO4 containing EDTA (0.2%), and reduced glutathione as stabilizer. A reversed phase column with an eluting system containing 0.025 M citric acid-sodium hydrogen phosphate buffer in the ratio 3:2 (v:v) and 5% methanol was used. The experimental results of plasma DHPG levels compared favourably with the results from the literature, and a positively significant correlation with plasma MHPG was found. This method could be used as an alternative in central NA assessment.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020109
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  • 3
    Electronic Resource
    Electronic Resource
    H. Danielsson and J. Sjövall. Sterols and bile acids. Elsevier Science Publishers, Amsterdam 1985 pp. 447. US $70.00 (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. i 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020113
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  • 4
    Electronic Resource
    Electronic Resource
    HPLC receptorassay of opioid peptides in the cerebrospinal fluid of lower back pain patients (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 47-52 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Total opioid peptide receptoractivity in human cerebrospinal fluid is measured in patients who are experiencing lower back pain. Desalted CSF is eluted from a C18 Sep-Pak and is subjected to a radioreceptorassay (RRA) that employs tritiated etorphin, which is aligand that is effectively displaced by opioids from several different types of opioid receptors. Three clinical groups have significantly different endogenous levels of 2.4, 4.5, and 6.4 pmol of methionine enkephalin-equivalents per mL CSF. Those three levels indicate that more opioid activity is correlated with the amount of drug to relieve the patient's perception of pain. When the total opioid content exceeds an empirical threshold, the sample is further fractionated with gradient reversed phase HPLC, and the opioid receptoractivity in each HPLC fraction is measured to determine the characteristics pattern of those receptoractive opioid peptides present in that patient's CSF. Different HPLC RRA patterns are found for different clinical categories. A possible interpretation of these two different sets of data-is that a lesion exists in one or several of the opioid peptidergic systems (metabolism, receptors) in this particular patient population.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020202
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  • 5
    Electronic Resource
    Electronic Resource
    Chromatographic studies of human lung elastin digestion products obtained by leucocyte elastase: Comparison between newborn and adult soluble fragments (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 57-61 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Human insoluble elastin was prepared from newborn lungs and digested by leucocyte elastase. The soluble fragments were compared to those obtained from adult lung elastin in a previous work (Smyrlaki et al., 1986).Gel filtration on a Bio-Gel P-100 column of newborn elastin allowed the separation of fraction F1N (Mr's 30 000-10 000) which was eluted later than the excluded fraction F1A (Mr's 80 000-30 000) previously isolated from adult elastin. The difference in the sizes of the large peptide fragments originating from both elastins was also shown on SDS-PAGE.Reversed phase HPLC was performed on a C18 column using a multi-step gradient elution procedure. Different patterns were observed for the high (F1N) and the low (F2N) molecular size fragments of newborn elastin. The same peak distribution was obtained with adult elastin. Comparison of the amino acid compositions of the most retained peaks (3, 4 and 5), derived from fractions F1N and F1A, showed analogies for the contents of the major nonpolar amino acids and crosslinks. Thus, this procedure allowed the separation of typical fragments of elastin which might be released in vivo by leucocyte elastase during pulmonary diseases.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020204
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  • 6
    Electronic Resource
    Electronic Resource
    Evaluation of vaginal malodor and efficacy of treatment by high performance ion exchange chromatography (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 76-78 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: High performance ion exchange chromatography was employed to evaluate the presence of short chain organic acids in the vaginal fluid of a woman troubled by persistent foul vaginal odor, but who did not have typical bacterial vaginosis. The vaginal secretions from this patient were collected on a weighed cotton swab and eluted into water and extracted by acidified ether. Salts of the acids were back-extracted into aqueous solution and chromatographed on an H-form resin column and compared to commercially available standards. A strikingly large amount of caproic acid was found. The caproic acid disappeared after metronidazole therapy, and a subsequent follow-up chromatogram showed a predominance of lactic acid. The success of this technique in evaluating the present case suggests that such a method may prove useful in other types of vaginal infection.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020208
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  • 7
    Electronic Resource
    Electronic Resource
    Product news (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. i 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020211
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  • 8
    Electronic Resource
    Electronic Resource
    Quantitative determination of adriamycin in rat hepatocytes using a volatile extraction buffer, HPLC and fluorescence detection (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 91-94 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A rapid and sensitive isocratic technique is described for the determination of concentrations of adriamycin and two of its metabolites, adriamycinol and adriamycinone, in freshly isolated rat hepatocytes. The drugs are easily and efficiently extracted from the cells with an organic mixture (chloroform-n-butanol) after proteolytic digestion with trypsin. Mean recoveries from spiked culture medium cell suspension are greater than 96%. The within run and day-to-day coefficients of variation are less than 7.5%.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020302
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  • 9
    Electronic Resource
    Electronic Resource
    Computerized chromatographic peak detection using the trigg tracking signal. An application devised for use with an online analog to digital converter connected between an amino acid analyser and a personal computer (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 104-109 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Manual integration of the amino acid peaks from physiological samples produced by conventional anion exchange liquid chromatography is a time-consuming process. This paper describes a combined unit, consisting of an analog to digital converter and a personal computer, which was connected in parallel with the chart recorder and the analyser's 570 nm channel of the colorimeter. The computer was programmed to log the digitized data, detect the start, maximum and end of each chromatographic peak, calculate the area under the peak and its retention time and provide a printoct of the results at the end of the elution program. The computer program successfully exploited the Trigg Tracking Signal as both a peak detection and as a moving baseline monitoring device. This approach proved to have an equivalent performance to the manual method for 17 out of the 19 amino acids normally quantitated in physiological samples. The automated detection and quantitation of arginine was unsatisfactory due to its characteristically low profile peak shape, and proline was not measured because the device was not connected to the 440 nm channel of the colorimeter. The automated system provided economic and analytically acceptable solutions to the problem of providing an online integrator versatile enough to be used with the 255 min long amino acid analysis of physiological fluids.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020305
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  • 10
    Electronic Resource
    Electronic Resource
    Studies on the chromatographic fractionation of metabolites of benzo[a]pyrene in faeces and urine from germfree and conventional rats (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 120-134 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Rats, germfree and conventional, were dosed with 14C-labelled benzo[a]pyrene. Faeces and urine were collected. Metabolites in faces were effectively extracted with a new method using a combination of solvents and solid sorbents. Metabolites in urine were extracted with octadecylsilane-bonded silica. The metabolites were fractionated into groups by chromatography on a cation exchanger (SP-LH-20 or SP-Sephadex C-25) and an anion exchanger (TEAP-LH-20). Some of the groups were further purified by column chromatography and analysed by HPLC and TLC. The analyses show a complex pattern of metabolism. A large part of the metabolites (9-24% depending on animal type and route of excretion) had amphoteric properties, e.g. like glutathione and cysteine conjugates. The abundance of conjugates sensitive to β-glucuronidase and sulphatase was low. The relative amount of acidic conjugates in faeces was much higher in the germfree than in the conventional rats indicating the influence of the intestinal flora on the metabolism. The results support the view that the mercapturic acid pathway is a quantitatively important metabolic route for benzo[a]pyrene in rats. The methods of extraction and group fractionation were designed to be generally applicable to the analysis of lipophilic xenobiotics and their metabolites.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020308
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  • 11
    Electronic Resource
    Electronic Resource
    Determination of galactose in human plasma by HPLC with electrochemical detection (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 95-98 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Galactose in plasma from patients with hepatic diseases who had undergone low level galactose infusion was determined by using HPLC with electrochemical detection (LCEC). Agreement between galactose concentration determined by the LCEC and a fluorometric method was remarkably good at moderate levels of galactose in plasma. However, the fluorometric method is not suitable for samples containing very small amounts of galactose (blood from hepatic veins) and even for a few samples at moderate galactose content (blood from peripheral veins), suggesting the presence of an endogenous interference. There was no interference for the quantitation of galactose by the LCEC method, by virtue both of the specificity involved in the electrochemical detection and the separation by liquid chromatography. The detection limit of the LCEC method was 0.4 mg galactose/L blood.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020303
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  • 12
    Electronic Resource
    Electronic Resource
    Comparison of iodinated [Nle15]- and [Met15]-gastrin17 prepared by reversed-phase HPLC (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 159-163 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: 125I-[Nle15]-gastrin17 prepared by the iodogen method can be separated by reversed-phase high performance liquid chromatography into two peaks, both of which elute after [Nle15]-gastrin17. Direct determination of the specific activities of the two derivatives by microbore reversed-phase HPLC indicated that they were the mono- and di-iodinated species. In contrast the two peaks obtained with [Met15]-gastrin17 iodinated under the same conditions eluted earlier, relative to the appropriate gastrin17 standard, than the [Nle15]-gastrin derivatives. Treatment of either peak with 0.75 M dithiothreitol at 56°C or 95°C resulted in progressive conversion to compounds migrating in relative positions similar to the 125I-[Nle15]-gastrin17 derivatives. Direct determination of the specific activity of the earlier eluting [Met15]-gastrin17 derivative before reduction indicated that it was the mono-iodinated species. It thus appears likely that iodination of [Met15]-gastrin17 by the iodogen method results predominantly in the formation of mono- and di-125I-[Met sulphoxide15]-gastrin17. To avoid problems arising from oxidation of the methionine residue of gastrin during iodination, the use of 125I-[Nle15]-gastrin17 in binding studies is therefore recommended.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020407
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  • 13
    Electronic Resource
    Electronic Resource
    Product news (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. ii 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020415
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  • 14
    Electronic Resource
    Electronic Resource
    Micro-scale sequence analysis from the N-terminus of peptides using the fluorogenic edman reagent 4-N, N-dimethylamino-1-naphthyl isothiocyanate (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 139-144 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The fluorogenic Edman reagent 4-N,N-dimethylamino-1-naphthyl isothiocyanate (DNTC) was reacted with amino acids and peptides, cyclized by acid and the liberated 4-N,N-dimethylamino-1-naphthyl thiohydantoin (DNTH) amino acids were then separated and detected by HPLC. The fluorescence intensities of DNTH-amino acids except DNTH-proline and -serine were dramatically increased in the alkaline solution and organic solvent. Thus, the postcolumn reaction with alkaline acetonitrile solution was adopted in HPLC. The polar and aromatic amino acids afforded two DNTH-amino acids on derivatization with DNTC and cyclization with acids. These were suggested to be stereoisomers of DNTH-amino acids. The sequence analysis of 0.5 nmol Leu-enkephalin was achieved by the double coupling method with DNTC and phenyl isothiocyanate followed by the proposed HPLC system.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020402
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  • 15
    Electronic Resource
    Electronic Resource
    Determination of plasma cytidine deaminase activity by HPLC (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 148-151 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Cytidine deaminase is an enzyme of nucleic acid metabolism, the measurement of which has been proposed as a useful test for the early detection of pre-eclamptic toxaemia in pregnancy. The enzyme converts the nucleoside cytidine to uridine, with the release of ammonia, and it is the measurement of this latter compound that forms the basis of the conventional methods for the assay of cytidine deaminase. The low activity of the enzyme requires long incubation times, which in turn increase the possibility of contamination by exogenous ammonia. We have developed a new method for determining cytidine deaminase activity, utilising high performance liquid chromatography to measure the production of uridine. This method uses much shorter incubation times and is unaffected by ammonia contamination. This paper describes the development of the method and its comparison with the established assay. The relative merits of each are discussed. Finally, the adaptation of incubation and chromatographic conditions, in order to measure other enzymes of nucleic acid metabolism which are of clinical interest, is briefly mentioned.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020404
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  • 16
    Electronic Resource
    Electronic Resource
    HPLC determination of polyamines in the femtomole range (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 173-176 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A new method for the chromatographic determination of polyamines is presented. The procedure consists of the reaction of 9-fluorenylmethyl chloroformate (FMOC-Cl) with polyamines at 50 ± 1°C for 10 min, followed by stepwise elution chromatography. The reaction is simple and the derivatives are stable. All the polyamine-FMOC derivatives can be separated within 13 min. The linearity of this method is satisfactory in the range of 0.5-100 pmol. The detection limits for putrescine, cadaverine, spermidine and spermine are 83.3 fmol, 109 fmol, 25.5 fmol and 22.7 fmol respectively.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020410
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  • 17
    Electronic Resource
    Electronic Resource
    Masthead (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987) 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020101
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  • 18
    Electronic Resource
    Electronic Resource
    Direct determination of vanillylmandelic acid in human urine by reversed-phase HPLC (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 1-3 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A reversed-phase HPLC method for the determination of epinephrine, norepinephrine, dopamine, and vanillylmandelic acid (VMA) has been developed. The concentration of VMA in the urine of hypertensive patients was measured by direct injection after centrifugation. The method is useful for the diagnosis of pheochromocytoma.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020102
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  • 19
    Electronic Resource
    Electronic Resource
    Analysis of p-aminobenzoic acid and its metabolites in urine and plasma by ion pair HPLC in the NBT-PABA pancreatic function test (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 13-16 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: An ion pair HPLC method which can simultaneously detect the major metabolites of an exocrine pancreatic function testing agent (NBT-PABA) in plasma and urine has been developed. This assay has been applied to a pharmacokinetic study of PABA and its metabolites in 3 healthy adult volunteers following the oral administration of 1 g NBT-PABA. The 6 h testing period currently used to collect urine following the NBT-PABA ingestion is adequate for the recovery of PABA and its metabolites. Plasma determination of these compounds may provide an improved evaluation of the pancreatic performance in patients with abnormal liver or kidney function.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020105
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  • 20
    Electronic Resource
    Electronic Resource
    Rapid purification of arrowhead proteinase inhibitors by high performance hydrophobic interaction chromatography on a PEG bonded phase column (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 20-23 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A new hydrophobic interaction HPLC column is used for the rapid purification of proteinase inhibitors isolated from arrowhead. The inhibitors, partially purified by DEAE-cellulose column chromatography, are resolved into three components with a mobile phase gradient of decreasing salt concentration from 1.1 M ammonium sulfate in 0.01 M phosphate buffer to phosphate buffer alone. This new HPLC column is found to be very useful for rapid, semipreparative purification of hydrophobic protein and sample loading of up to 1.6 mg of inhibitors can be fully resolved on an analytical column.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020107
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  • 21
    Electronic Resource
    Electronic Resource
    Reduction of quinones with zinc metal in the presence of zinc ions: Application of post-column reactor for the fluorometric detection of vitamin K compounds (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 4-8 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple and effective chemical method has been developed for quantitatively reducing quinones, which is based on their reaction with zinc metal and zinc ions. Comparison of this method with conventional electrochemical reduction revealed the chemical method to be considerably superior. The reduction of quinones to their corresponding hydroquinones was verified by ultraviolet spectrophotometry. The reduction methodology has been applied to derivatize phylloquinone and its metabolite, namely phylloquinone 2,3-epoxide, ‘on-line’, with subsequent fluorometric detection of the generated hydroquinones.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020103
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  • 22
    Electronic Resource
    Electronic Resource
    Simultaneous determination of gastrodin and its metabolite by HPLC (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 17-19 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A rapid and specific HPLC method for the simultaneous determination of gastrodin and its metabolite gastrodigenin (p-hydroxybenzyl alcohol) in rat plasma, bile, liver, urine and faeces is described. The separation was achieved by using a reversed phase column (YWG-C18) eluted with methanol-water (2.5:97.5 v/v). Phloroglucinolum was used as internal standard and the peaks were detected at UV 221 nm. The protein precipitation with ethanol was a very simple and rapid method for sample preparation. The gastrodin and gastrodigenin were quantitated by measuring the peak-height ratios. There was a linear concentration range of 10-320 μg/mL in the assay for both compounds. The coefficients of variation (within-day) for samples spiked with gastrodin and gastrodigenin were 2.94% and 3.08%, respectively. The method demonstrated a high specificity and was suitable for use in pharmacokinetic studies.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020106
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  • 23
    Electronic Resource
    Electronic Resource
    HPLC measurement of penticainide and desalkylpenticainide in biological fluids (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 34-37 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple HPLC method has been developed to measure the antiarrhythmic agent penticainide and its N-desalkyl metabolite in biological fluids. Solvent extraction of a small (200 μL) sample volume with direct analysis of the extract is used to measure the plasma and urinary concentrations of these compounds attained during chronic therapy, although a larger sample volume (1.0 mL) and prior concentration of the extract are required for single oral dose work. In each case chromatographic analysis is performed using a microparticulate (5 μm) silica column and methanolic ammonium perchlorate (10 mM, pH 6.7) as eluent with UV detection (260 nm). No endogenous sources of interference have been encountered and potential interference from other drugs is minimal.
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  • 24
    Electronic Resource
    Electronic Resource
    Product news (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. ii 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020114
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  • 25
    Electronic Resource
    Electronic Resource
    Calendar of events (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. ii 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020115
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  • 26
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    Determination of artemether in plasma and whole blood using HPLC with flow-through polarographic detection (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 53-56 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: An HPLC method with polarographic detection for the trace determination of artemether in plasma and whole blood was developed and applied to pharmacokinetic and clinical pharmacological studies. The method showed high sensitivity and selectivity because of the easy reduction of the peroxide linkage of artemether at the mercury drop electrode. The detection limit was 10 ng and the detector response was linear over the range of 10 ng to 1 μg artemether injected onto the column. The largest relative standard deviation of 10 replicate measurements of standard solutions (concentrations of 10 ng/mL-1 μg/mL) was 8%. The recovery from whole blood and plasma of added drug (concentrations of 15-48 ng/mL) was 71-100%.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130020203
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  • 27
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    HPLC determination of ferrochelatase activity in human liver (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 71-75 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A method utilizing HPLC to estimate ferrochelatase activity in human liver cells is presented. A partially purified homogenate of liver cells is incubated with mesoporphyrin IX and cobalt(II) ion. The ferrochelatase in the homogenate incorporates the cobalt(II) ion into the mesoporphyrin. After a fixed time (90 min) the porphyrins are extracted into an ethyl acetate-acetic acid mixture. The porphyrins are then separated using reversed phase HPLC with a mobile phase of methanol-acetonitrile-phosphate buffer pH 3.0 (200:60:30 v/v). The enzyme activity is estimated by measuring the rate of utilization of mesoporphyrin. The optimum pH and substrate concentration for the reaction have been determined.
    Additional Material: 8 Ill.
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  • 28
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    Identification of isoprenoid-type components in human expired air: A possible shunt pathway in sterol metabolism (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 66-70 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Expired air samples have been analyzed from three groups of human subjects (normal, liver dysfunction, lung cancer) and the baboon (Papio anubus). Of the several hundred compounds present, three compounds were of particular interest due to their structural relationship to the isoprenoid-type intermediates in the sterol pathway. These compounds were 1-methyl-4-(1-methyl-ethenyl)-cyclohexene, 6-methyl-5-hepten-2-one, and 6,10-dimethyl-5,9-undecadien-2-one. Hydroxyacetone was also found in all samples screened. The relationship of these compounds to the non-sterol pathway of mevalonate metabolism is discussed.
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  • 29
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    Hydrophobic interaction chromatography of autoproteolysis products of human seminal plasma (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 152-155 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Hydrophobic interaction chromatography was employed for the fractionation of the glycopeptide mixture obtained after autoproteolysis and delipidization treatment of normal human seminal plasma samples. This sequence of procedures led to the elimination of highly hydrophobic components and to the concentration of the carbohydrate-rich fractions. A partial separation between the O- and N-glycosidic-linked oligopeptides was also achieved after the chromatographic step.
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  • 30
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    Simultaneous determination of myocardial creatine phosphate and adenine nucleotides by reversed-phase HPLC (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 156-158 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: An isocratic HPLC system has been developed which allows for the rapid (single run of 20 min) measurement of creatine phosphate (PCr) and adenine nucleotides (ATP, ADP and AMP) in extracts from freeze-clamped and freeze-dried myocardial tissues. The separation was achieved at room temperature by using a RP18 column and a dual variable wavelength spectrophotometer, set at 210 and 254 nm. The solvent was 30 mM potassium dihydrogen phosphate, 15 mM tetrabutylammonium hydrogen sulfate, pH 6.7, 19% (v/v) acetonitrile. A distinct separation (confirmed with the retention time of standard sample) of these high energy compounds was achieved. Standard curves were linear. In isolated rat hearts the following values were obtained (μmol/g dry wt, mean ± SEM): ATP 21.5 ± 1.3, ADP 4.6 ± 0.2, AMP 1.5 ± 1.1 and PCr 32.5 ± 1.3; which are consistent with previously published values for high energy compounds in this tissue.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130020406
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  • 31
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    Peter Mohr and Klaus Pommerening. Affinity chromatography-practical and theoretical aspects. Marcel Dekker, New York, 1986. $79.75, 312pp (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. i 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020413
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  • 32
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    Fluorometric analysis of urinary chondroitin sulfate isomers by HPLC using dansylhydrazine as a prelabeling reagent (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 169-172 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Chondroitin sulfate isomers (ChS isomers) were digested with chondroitinase ABC, and the unsaturated disaccharides produced were converted into fluorescent dansylhydrazine derivatives and analyzed by HPLC. The proposed method was applied to the determination of relative amounts of ChS isomers in normal human urine and analytical results showed that chondroitin-6-sulfate and chondroitin-4-sulfate were excreted in large amounts. Moreover, this method was used for the identification of urinary ChS isomers which were extracted from a cellulose acetate strip after carrying out electrophoresis.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130020409
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  • 33
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    An HPLC assay for rat liver ferrochelatase activity (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 164-168 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A rapid, reliable, sensitive and reproducible HPLC method was developed for the assay of ferrochelatase activity in rat liver. The assay was carried out aerobically with Zn2+ and mesoporphyrin or protoporphyrin IX as substrates. Zn-porphyrins formed were extracted with dimethyl sulphoxide/methanol (30:70, v/v) containing Zn-deuteroporphyrin as the internal standard for separation and quantification by reversed-phase chromatography. The Km for mesoporphyrin was 5.9 μM, for protoporphyrin IX 8.8 μM and for zinc 6.0 μM. The specific activities were 33.1 ± 5.0 nmol Zn-mesoporphyrin or 13.4 ± 2.0 nmol Zn-protoporphyrin formed per hour per mg of protein for mitochondria and 12.3 ± 2.2 nmol Zn-mesoporphyrin or 4.6 ± 0.9 nmol Zn-protoporphyrin per hour per mg of protein for liver homogenate.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130020408
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  • 34
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    HPLC measurement of diltiazem and desacetyldiltiazem in serum or plasma (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 180-182 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130020412
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  • 35
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    A rapid method for the determination of benzylpenicillin in serum by reversed-phase HPLC (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 177-179 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple procedure for the determination of benzylpenicillin in serum is described. The assay involves the extraction of the drug and the internal standard (phenoxymethylpenicillinic acid) from the sample into dichloromethane, using tetrabutylammonium hydrogen sulfate neutralized with NaOH and buffered with citrate as an ion-pairing reagent. RP-HPLC was performed on a Spherisorb 5 ODS column, eluting the drugs isocratically with 14% acetonitrile in 10 mM ammonium acetate buffer. Monitoring was by UV detection at 208 nm. Our results show that the method is accurate and reproducible, permitting quantification of serum levels of benzylpenicillin without interference from other drugs commonly used in therapy. Analytical recovery was greater than 79.2%.
    Additional Material: 1 Ill.
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  • 36
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    Calendar of events (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. i 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020512
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  • 37
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    Masthead (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987) 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020601
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  • 38
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    Study of doxorubicin photodegradation in plasma, urine and cell culture medium by HPLC (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 242-244 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: An HPLC method was used to monitor the chemical stability of doxorubicin-HCI (DXR) to light in plasma, urine and cell culture medium at room temperature. The results indicated that DXR was very unstable in cell culture medium and urine when exposed to light. It was more stable in plasma under the same conditions. In all the cases, the decrease in the amount of DXR is greatly dependent on light intensity (no noticeable degradation was observed after 8 h in the dark). These observations may be important for the correct interpretation of the effects and the toxicity of doxorubicin on cells incubated in cell medium, and for determination of urinary or plasma pharmacokinetic parameters.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130020603
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  • 39
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    HPLC analysis of polyamines and their acetylated derivatives in the picomole range using benzoyl chloride and 3,5-dinitrobenzoyl chloride as derivatizing agent (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 254-257 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Analytical methods are described for the quantitative determination of putrescine, cadaverine, spermidine, spermine and the acetylated derivatives of spermidine and spermine in biological fluids using pre-column derivatization with either benzoyl chloride or 3,5-dinitrobenzoyl chloride, which were added to each sample as solutions in diethyl ether. Putrescine, spermidine and spermine can be analysed in seminal plasma at nanogram levels when benzoyl chloride is used as derivatizing agent. In the analysis of putrescine, cadaverine, spermidine and acetyl derivatives of spermidine and spermine, higher sensitivity is obtained with 3,5-dinitrobenzoyl-chloride. This method can readily be used in the determination of acetylated polyamines in urine samples.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130020606
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  • 40
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    MicroHLPC determination of amygdalin in Semen pruni armeniacae and Semen pruni persicae (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 271-273 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The application of micro HPLC to the determination of amygdalin in Semen pruni armeniacae and Semen pruni persicae is described. Amygdalin is separated at ambient temperature on a reversed phase column of U-Finepak SIL C18(150×0.5 mm) with methanol + water (25: 75 v/v) as the mobile phase at a flow rate of 10 μL/min. The results are calculated by the internal standard method. The linear range is 1-7 μg. The CV and recovery of pure amygdalin are 1.47% (n = 10) and 98.13%, respectively. The results of analysis are lower than those obtained by TLC, but microHPLC is much simpler, faster, and more sensitive and reproducible than TLC.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130020609
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  • 41
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    Determination of 4-methylpyrazole in plasma using solid phase extraction and HPLC (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 226-227 
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    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A rapid method for the determination of 4-methylpyrazole in plasma is described. Internal standard (3-methylpyrazole) is added to the plasma which is subsequently applied to a BondElut SCX column. After washing the column the 3- and 4-methylpyrazoles are eluted with a phosphate buffer and analyzed by isocratic reversed-phase high performance liquid chromatography with UV detection. The concentration of 4-methylpyrazole is calculated from the 4-methylpyrazole/3-methylpyrazole peak high ratio. The method is linear between 2.5 and 100 μmol/L with a within-day precision (CV) of 2.2% (n = 10) and a day-to-day precision of 2.8% (n = 30). The sensitivity is sufficient for analysis of plasma levels in the low micromolar range.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130020511
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  • 42
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    Purification of streptococcal protein g expressed by Escherichia coli by high performance liquid affinity chromatography using immobilized immunoglobulin G and albuminThis work was supported by the Crafoord Foundation, the Swedish Medical Research Council (proj. no. 3362, 7144, 7486), the Medical Faculty, University of Lund, Gustav V:s 80-year Foundation, Österlunds Foundation, Stiftelsen JO Nauclers Minnesfond and Excorim KB. (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 221-225 
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    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A one-step HPLC method was developed for the purification of protein G, a cell wall molecule from group C and G streptococci with immunoglobulin G- and albumin-binding properties. Lysed Escherichia coli bacteria infected with lambda-phages containing the protein G gene from group G streptococci were used as a starting material for the preparations. The lysate was applied to a column with immobilized human immunoglobulin G or human serum albumin. Protein G was selectively bound and eluted at pH 2.0. A 750-fold purification was achieved. Sodium dodecylsulfate + polyacrylamide gel electrophoresis showed that the highly purified protein G consisted of three sets of doublets with the apparent molecular weight of 64 and 67, 56 and 58, and 45 and 47 kilodaltons, respectively. A specific method for quantitation of small amounts of protein G was developed and used for specific tracing of the protein after the affinity chromatography. Goat polyclonal antibodies were bound to an antigen coated to the plastic walls of microtiter plates, causing the Fc-region of the immunoglobulins to be directed outwards. Unknown samples of protein G were then allowed to compete with radio-iodinated protein G (solid phase radioassay) or protein G coupled to alkaline phosphatase (enzyme linked sorbent assay) for the Fc-regions.
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  • 43
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    Calendar of Events (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. iii 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020611
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  • 44
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    Determination of guanine plus cytosine bases in bacterial DNA hydrolysate by reversed phase HPLC (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 89-90 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130020210
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  • 45
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    Masthead (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987) 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020301
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  • 46
    Electronic Resource
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    Calendar of events (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. i 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020414
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  • 47
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    Masthead (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987) 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020501
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  • 48
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    The effect of storage on rat tissues and human plasma amino acid levels determined by HPLC (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 195-196 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Tissue concentrations of the amino acids tryptophan, methionine, valine, phenylalanine, isoleucine and leucine were determined in rat liver, skeletal muscle and brain tissue and human plasma. The effect of storage at -20°C for up to 21 days was examined. Significantly elevated levels after 7 and 21 days of storage were observed in liver and brain tissue but no changes were found in muscle and plasma. Minimal changes occurred in liver tissue stored up to 6 hours at -4°C. This study emphasizes the need for rapid deporteinization of tissues to avoid changes in the free pool of amino acids.
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  • 49
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    Development of a selective clean-up method using immobilized antibody and its application to HPLC and GC/MS determination of a carbacyclin derivative, CS-570, in plasma (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 203-208 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Methods for the determination of CS-570, a chemically stable prostacyclin analogue, in plasma were developed by using an immobilized antibody column followed by fluorescence HPLC and GC/MS. The CS-570 antibody, obtained from rabbit plasma by giving CS-570-BSA for a few months, was coupled to Sepharose 4B and used as extraction phase for sample clean-up and extraction of the drug. A plasma sample was applied to this column, washed with water and the drug was eluted with 90% acetonitrile. 0.02% (w/v) 9-anthryldiazomethane (ADAM) was added to the extract to form a fluorescent derivative. The CS-570-ADAM adduct exhibited high sensitivity when applied to HPLC with fluorescence detection and column switching. The detection limit was 1 ng/mL when 1 mL of plasma was available. Additionally, a pentafluorobenzyltrimethylsilyl derivative of CS-570 showed excellent sensitivity when determined by capillary GC interfaced to negative ion chemical ionization MS using a stable isotope labelled analogue as an internal standard.
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    URL: http://dx.doi.org/10.1002/bmc.1130020507
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  • 50
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    Improved HPLC determination of urinary neopterin (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 183-188 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: In order to improve the urinary neopterin measurement, the reversed-phase HPLC method has been reevaluated. The parameters which influence the chromatographic behavior of 12 pteridines were studied: nature of buffer, pH,ionic strength, addition of organic modifier to the mobile phase. Accordingly, an isocratic HPLC method is described which offers a good compromise between specificity and analysis time. This method is well-suited to automation in routine clinical laboratory use. Using this HPLC method, urinary neopterin related to creatinine was determined in lung diseases (neoplasm, sarcoïdosis and bronchial asthma) and in kidney allografts. This method was shown to be useful in the diagnosis and in the monitoring of treatment of rejection episodes.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130020502
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    Thin-layer chromatography - the forgotten alternative for the quantitative determination of steroids (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 189-192 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: We have developed a high performance thin layer chromatography (HPTLC) system for quantitative determination of androgens, corticosteroids, mineralocorticoids and gestagens on silicagel KG-60 HPTLC-plates with different solvent systems. A complete separation of androgens, gestagens and metabolites was achieved with dichlormethane/cyclohexane/acetone (70:25:5). Corticosteroids, mineralocorticoids and their derivatives were completely separated with diethylether/isooctane/isopropanol (70:25:5). The quantitative in situ fluorescence determination was carried out after post-chromatographic derivatization with cinnamic aldehyde, 4-dimethylaminobenzaldehyde and sulfuric acid. The sensitivity of detection was found between 500 pg and 1 ng per spot.The steroid metabolism as catalysed by rat liver microsomal oxidoreductases was measured by these procedures, and was compared with determination of steroids by gas chromatography (GC). According to HPTLC, steroids were reduced by NADPH-5α-reductase (EC 1.3.1.4) in the order progesterone 〉 testosterone 〉 aldosterone 〉 cortisol 〉 corticosterone. The enzyme activities as measured by HPTLC agree well with those obtained by GC (r = 0.94). When turnover of enzyme assays, speed of determination, detection limit, application to labile steroids and costs of steroid determination are considered, all points speak in favour of HPTLC.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130020503
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    The determination of cysteamine in physiological fluids by HPLC with electrochemical detection (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 216-220 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Cysteamine, an amino thiol, was separated by rapid isocratic cation exchange chromatography and detected by electrochemical oxidation at a platinum electrode maintained at +0.45 V relative to an Ag/AgCl reference electrode. Eluent pH and electrode working potentials were optimized and the effects of alternative buffers and organic modifiers have been examined. On column sensitivity for cysteamine was 1.5 pmol at a signal-to-noise ratio of 5. Although the specificity was good, plasma samples required maximal sensitivity whereas urine samples required greater selectivity, which was achieved by use of lower working potentials. Cysteamine concentrations were determined in serial samples of plasma and urine from volunteers who had received a single oral dose of 200 mg of the drug. Cysteamine was rapidly oxidized in vivo, and detection required prior reduction with dithiothreitol before analysis.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130020509
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    Product news (1987)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. iii 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130020612
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    Masthead (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987) 
    Details
    ISSN: 0887-3585
    Keywords: Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prot.340020101
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    Detection of human somatic cell structural gene mutations by two-dimensional electrophoresis (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 13-19 
    Details
    ISSN: 0887-3585
    Keywords: two-dimensional electrophoresis ; ethylnitrosourea ; somatic mutations ; structural variants ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The feasibility of detecting human somatic structural gene mutations by two dimensional electrophoresis has been investigated. A lymphoblastoid cell line was grown as a mass culture in the presence of ethylnitrosourea, after which cells were regrown as single cell clones. A total of 257 polypeptide spots were analyzed in gels derived from 186 clones. Four structural mutations were detected by visual analysis of the gels. Computer analysis of gels corresponding to the mutant clones was also undertaken. At a spot size threshold of 200 spots to be matched using a computer algorithm, all four mutant polypeptides were detected. These results indicate the usefulness of the two-dimensional approach for mutagenesis studies at the protein level.
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    URL: http://dx.doi.org/10.1002/prot.340020103
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  • 56
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    Estimation of uncertainties in X-ray refinement results by use of perturbed structures (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 1-12 
    Details
    ISSN: 0887-3585
    Keywords: protein crystallography ; protein refinement ; empirical energy simulations ; error analysis ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The uncertainties in the refined parameters for a 1.5-Å X-ray structure of carbon-monoxy (FeII) myoglobin are estimated by combining energy minimization with least-squares refinement against the X-ray data. The energy minimization, done without reference to the X-ray data, provide perturbed structures which are used to restart conventional X-ray refinement. The resulting refined structures have the same, or better, R-factor and stereochemical parameters as the original X-ray structure, but deviate from it by 0.13 Å rms for the backbone atoms and 0.31 Å rms for the sidechain atoms. Atoms interacting with a disordered sidechain, Arg 45 CD3, are observed to have larger positional uncertainties. The uncertainty in the B-factors, within the isotropic harmonic motion approximation, is estimated to be 15%. The resulting X-ray structures are more consistent with the energy parameters used in simulations.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/prot.340020102
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    Predicted calmodulin-binding sequence in the γ subunit of phosphorylase b kinase (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 20-33 
    Details
    ISSN: 0887-3585
    Keywords: calmodulin ; peptide ; calmodulin-binding peptide ; peptide design ; hydrophobic moment ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A basic, amphiphilic α helix is a structural feature common to a variety of inhibitors of calmodulin and to the calmodulin-binding domains of myosin light chain kinases. To aid in recognizing this structural feature in sequences of peptides and proteins we have developed a computer algorithm which searches for sequences of appropriate length, hydrophobicity, helical hydrophobic moment, and charge to be considered as potential calmodulin-binding sequences. Such sequences occurred infrequently in proteins of known crystal structure. This algorithm was used to find the most likely site in the catalytic (γ) subunit of phosphorylase b kinase for interaction with calmodulin (the δ subunit). A peptide corresponding to this site (residues 341-361 of the γ subunit) was synthesized and found to bind calmodulin with approximately an 11 nM dissociation constant. A variant of this peptide in which an aspartic acid at position 7 in its sequence (347 of the γ subunit) was replaced with an asparagin was found to bind calmodulin with approximately a 3 nM dissociation constant.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/prot.340020104
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    Subunit assembly and metabolic stability of E. coli RNA polymeraseThis is paper No. 10 in the series entitled “Subunit of RNA polymerase in Function and Structure.” Paper No. 9 is ref. 65. (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 42-53 
    Details
    ISSN: 0887-3585
    Keywords: proteolytic cleavage ; immunological cross-reaction ; amber fragment ; temperature-sensitive mutant ; stationary growth-phase ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Immunological cross-reaction was employed for identification of proteolytic fragments of E. coli RNA polymerase genered both in vitro and in vivo. Several species of partially denatured but assembled RNA polymerase were isolated, which were composed of fragments of the two large subunits, β and β′, and the two small and intact subunits, α and σ. Comparison of the rate and pathway of proteolytic cleavage in vitro of unassembled subunits, subassemblies, and intact enzymes indicated that the susceptibility of RNA polymerase subunits to proteolytic degradation was dependent on the assembly state.Using this method, degradation in vivo was found for some, but not all, of the amber fragments of β subunit in merodiploid cells carrying both wild-type and mutant rpoB genes. Although the RNA polymerase is a metabolically stable component in exponentially growing cells of E. coli, degradation of the full-sized subunits was found in two cases, i.e., several temperature-sensitive E. coli mutants with a defect in the assembly of RNA polymerase and the stationary-phase cells of a wild-type E. coli. The in vivo degradation of RNA polymerase was indicated to be initiated by alteration of the enzyme structure.
    Additional Material: 9 Ill.
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    URL: http://dx.doi.org/10.1002/prot.340020106
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  • 59
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    Characterization of a slow folding reaction for the α subunit of tryptophan synthase (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 54-63 
    Details
    ISSN: 0887-3585
    Keywords: domain association ; protein folding ; viscosity dependence ; solvent effects ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The equilibria and kinetics of ureainduced unfolding and refolding of the α subunit of tryptophan synthase of E. coli have been examined for their dependences on viscosity, pH, and temperature in order to investigate the properties of one of the rate-limiting steps, domain association. A viscosity enhancer, 0.58 M sucrose, was found to slow unfolding and accelerate refolding. This apparently anomolous results was shown to be due to the stabilizting effect of sucrose on the folding reaction. After accounting for this stabilization effect by using linear free-energy plots, the unfolding and refolding kinetics were found to have a viscosity dependence. A decrease in pH was found to stabilize the domain association reaction by increasing the refolding rate and decreasing the unfolding rate. This effect was accounted for by protonation of a single residue with a pK value of 8.8 in the native state and 7.1 in the intermediate, in which the two domains are not yet associated. The activation energy of unfolding is 4.8 kcal/mol, close to the diffusion limit. The negative activation entropy of unfolding, -47 cal/deg-mol, which controls this reaction, may result from ordering of solvent about the newly exposed domain interface of the transition state. These results may provide information on the types of noncovalent interactions involved in domain association and improve the ability to interpret the folding of mutants with single amino-acid substitutions at the interface.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/prot.340020107
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    Structural analysis of purified beta-adrenergic receptors (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 34-41 
    Details
    ISSN: 0887-3585
    Keywords: adrenergic receptors ; affinity chromatography ; electron microscopy ; oligomeric structure ; target size analysis ; HPLC digest mapping ; receptor evolution ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: We have characterized the structure of purified beta-adrenergic receptors by a combination of photoaffinity labeling, high performance liquid chromatography (HPLC)-tryptic mapping, CNBr fragmentation, target size analysis, and electron microscopy of purified receptor molecules. Guinea pig lung beta-adrenergic receptors purified by affinity chromatography, ion exchange chromatography, and HPLC size exclusion chromatography or photoaffinity labeled with [125]-iodocyanopindolol diazirine displayed mobilities on sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) that corresponded to Mr = 68,000. Purified, radioiodinated guinea pig lung beta-receptors were subjected to complete trypsin digestion and subsequent reverse-phase HPLC analysis, which revealed nine peptides. Active site labeling and tryptic digestion of partially purified hamster lung beta-receptors produced one peptide, whereas CNBr digestion of the same material produced two labeled fragments, yielding information about the location of the active site within the primary sequence. Purified guinea pig lung receptors were examined with transmission electron microscopy. Electron micrographs revealed slightly asymmetric, rod-shaped structures with an average length of 13 nm and width of 3.4 nm. Many receptors were arranged as apparent dimeric structures. These findings confirm data obtained from target size analysis of guinea pig lung beta-receptors in situ which suggest that receptors may exist as oligomeric arrays in the native membrane. Taken together, these data provide information about putative functional domains of the beta-adrenergic receptor and its quaternary structure.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/prot.340020105
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    Ion pairs in alpha helicesPresented in part at the Amer. Crystallogr. Assn. Meetings, Hamilton, Ontario, June 22-27, 1986. Abstract S5, p. 73. (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 64-71 
    Details
    ISSN: 0887-3585
    Keywords: intrahelical ion pairs ; frequency of ion pairs in exposed helices ; alpha-helix stabilization ; protein tertiary structure stabilization ; protein-folding pathway ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A survey of 47 globular proteins was made to determine the probability of occurrence of ion pairs separated by 1, 2, 3, … and 8 residues in the alpha helices. As a control, the probability of occurrence of like charged pairs was also determined. The survey showed that ion pairs of the type i, i±3 and i, i±4 are the most predominant. Such a preference was not observed for like charged pairs. The observed frequency of ion pairs is significantly greater than their expected frequency. The normalized frequencies of occurrence of the ion pairs were also found to increase generally with the helix length. These results indicate that the ion pairs may contribute to the stability of solvent-exposed alpha helices. Since the stabilization of protein secondary structure, these results may throw light on the mechanism of protein folding.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/prot.340020108
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    Masthead (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987) 
    Details
    ISSN: 0887-3585
    Keywords: Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prot.340020201
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    Comment: Protein hydrophobicity: Is it the sum of its parts? (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 79-80 
    Details
    ISSN: 0887-3585
    Keywords: Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prot.340020202
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    Contribution of arginine (HC3) 141α to the Bohr effect of the fourth binding step in the reaction of ligand with human hemoglobin (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 72-77 
    Details
    ISSN: 0887-3585
    Keywords: CO equilibrium constants ; des-(Arg 141α)HbA ; heme proteins ; high-affinity state ; kinetics ; ligand binding ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A few years ago we reported that histidine (HC3) 146β plays a major role in the pH-dependent propeties of the R-state of human hemoglobin, accounting for close to 50% of the R-state Bohr effect. We have extended these studies by examining the role of arginine 141α, another group known to affect the overall Bohr effect. We have compared the pH dependencies of the rate constants for the dissociation and combination of the fourth carbon monoxide molecule, I4 and I′4, respectively, for native hemoglobin A (HbA) and a control reconstututed HbA, and des-(Arg 141α) HbA, the hemoglobin molecule resulting from the enzymatic removal of the C-terminal arginine of the α-chain of human Hb. From these kinetic contants the pH dependence of L4, by about 80% between pH 6 and 8, where the aldkaline Bohr effect normally occurs, The sum of the effects of the removal of His 146β and of Arg 141α is grater than 100%. This suggests that at least one of these modifications altrs the contrubutions of other residues of this Bohr effect.
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    URL: http://dx.doi.org/10.1002/prot.340020109
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    Hybrid immunoglobulin isotypes of identical specificity produced by genetic recombination in Escherichia coli and expression in lymphoid cellsThis work was performed at the Department of Biological Sciences, Stanford University and Becton Dickinson Immunocytometry Systems, Mountain View, CA. (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 81-89 
    Details
    ISSN: 0887-3585
    Keywords: hybrid immunologlobulin ; compatible plasmids ; transfection ; mouse IgG1 ; mouse IgG2a ; dansyl ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: We have produced a series of hybrid IgG1-IgG2a mouse immunoglobulins with identical light chains (L) and variable regions to facilitate the identification of structural features associated with functional differnces between immunoglobulin isotypes. Hybrid heavy chain (H) constant region gene segments were generated by genetic recombination in Escherichia coli between plasmids carrying mouse γ1 and γ2a gene segments. Crossovers occured through out these segments although the frequency was highest in regions of high nucleotide sequence homology. Eleven variant immunoglobulins produced by transfected hybridoma cell lines are assembled into H2L2 tetramers and properly glycosylated. In addition, all 11 immunoglbulins have identical antigen combining sites specific for the fluorescent hapten ε-dansyll-L-lysine. Protein A binding was used as probe of the structural integrity of the Fc portion of the variant antibodies. Differeneces in protein A binding between IgG1 and IgG2a appear to be due to amino acid differances at postions 252 (Thr→Met) and 254 (Thr→Ser) of the heavy chain (EU numbering).
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    Three-dimensional structure of neuraminidase of subtype N9 from an avian influenza virus (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 111-117 
    Details
    ISSN: 0887-3585
    Keywords: crystallography ; antigen ; glycoprotein ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Neuraminidases from different subtypes of influenza virus are characterized by the absence of serlogical cross-reactivity and an amino acid sequence homology of approximately 50%. The three-dimensional structure of the neuraminidase antigen of subtype N9 from an avian influenza virus (A/tern/Australia/G70c/75) has been determined by X-ray crystallography and shown to be folded similarly to neuraminidase of subtype N2 isolated from a human influenza virus. This result demontrates that absence of immunological cross-reactivity is no measure of dissimilarity of polypeptide chain folding. Small differences in the way in which the subunits are organized around the molecular fourfold axis are observed. Insertions and deletions with respect to subtype N2 neuraminidase occur in four regions, only one of which is located within the major antigenic determinants around the enzyme active site.
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    Continuous compact protein domains (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 90-110 
    Details
    ISSN: 0887-3585
    Keywords: compact units ; coefficient of compactness ; folding intermediates ; protein structural hierarchy ; primitive units ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The coefficient of compactness was recently introduced and used to locate domains in lysozyme and ribonuclease (Zehfus and Rose: Bio-chemistry 25:5759-5765, 1986). Nineteen additional proteins now have been analyzed by using this measure. Complete listings of compact units and plots showing their hierarchic organization are presented for all twenty-one proteins. Large compact units correspond well to protein domains; however, many smaller compact structures of equal or better compactness are also found. Since small compact units could represent subdomains or protein-folding intermediates, their structural composition is further examined.
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    Prediction of secondary structure by evolutionary comparison: Application to the α subunit of tryptophan synthase (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 118-129 
    Details
    ISSN: 0887-3585
    Keywords: homologous proteins ; hydropathy index ; chain flexibility ; α/β barrels ; tryptophan ; synthase aplha subunit ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The amino acid sequences of the α subunits of tryptophan synthase form ten different microorganisms were alingned by standard procedures. The α helics, β strands and turns of each sequence were predicted separately by two standard prediction algorithms and averaged at homologous sequence positions. Additional evidence for conserved secondary structure was derived form profiles of average hydropathy and chain flexibility values, leading to a joint prediction. There is good agreement between (1) predicted β strands, maximal hydropathy and minimal flexibility, and (2) predicted loops, great chain flexibility, and protein segments that accept insertions of various lengths in individual sequences. The α subunit is predicted to have eight repeated β-loop-α-loop motifs with an extra N-terminal α helix and an intercalated segment of highly conserved residues. This pattern suggests that the teritiary structure of the α subunit is an eightfold α/β barrel. The distribution of conserved amino acid residues and publilshed data on limited proteolysis, chemical modification, and mutagenesis are consistent with the α/β barrel structure. Both the active site of the α subunit and the combining site for the β2 subunit are at the end of the barrel formed by the carboxyl-termini of the β strands.
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    URL: http://dx.doi.org/10.1002/prot.340020206
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    Distribution of accessible surfaces of amino acids in globular proteins (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 153-161 
    Details
    ISSN: 0887-3585
    Keywords: accessbility ; hydrophobic effect ; protein conformation ; Boltzmann statistics ; maximum likelihood ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Globular proteins fold into compact particles with interior amino acid residues shielded from the surounding aqueous environment. An early hypothesis holds that entropic hydophobic forces dirve this phenomenon. However, previous analyses based on a binary description of the accesible surfaces of amino acid residues in proteins did not support theis hypothesis. This report shows that a complete description of accessible surface areas is given by parametric distribution fuctions with three modes. The modes are formed by partitioning the available accessible surface area of the amino acids into three segments; the data for each segment are characterized by a mode-specific model. In the “repulsive” mode, probabilities of accessibility decrease exponentially with exposed surface area, as predicted by the hydrophobic hypothesis. A distinct “buried” mode is needed to account for an excess of residues at or near zero accessibility for most amino acids, consistent with the use of binary descriptions of accessibility. A third mode exists which is termed “near neutral” because it is described by a nearly uniform distribution of accessibility for the hydrophiliic amino acids. Empirical energies calculated for the repulsive mode correlate well with measured free energies of transfer of amino acids from water to organic solvents, while those from the buried mode correlate well with measured free energies of hydration of the side chains. Poor cross correlations between these energies give an explanation for the previous conflict in interpreting these data.
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    Prediction of the three-dimensional structure of human growth hormone (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 162-166 
    Details
    ISSN: 0887-3585
    Keywords: protein folding ; secondary structure prediction ; tertiary structure prediction ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: In recent years, the protein-folding problem has attracted the attention of molecular biologists. Efforts have focused on developing heuristic and energy-based algorithms to predict the three-dimensional structure of a protein from its amino acid sequence. We have applied a series of heuristic algorithms to the sequence of human growth hormone. A family of five structures which are generically right-handed fourfold α-helical bundles are found from an investigaion of ∼108 structures. A plausible receptor binding site is suggested. Independent crystallographic analysis confirms some aspects of these predictions. These methods only deal with the “core” structure, and conformations of many residues are not defined. Further work is required to identify a unique set of coordinates and to clarify the topological alternatives available to α-helical proteins.
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    URL: http://dx.doi.org/10.1002/prot.340020209
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    Extension of the fragment method to calculate amino acid zwitterion and side chain partition coefficients (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 130-152 
    Details
    ISSN: 0887-3585
    Keywords: amino acid hydophobicity scale ; QSAR ; amino acids ; peptide side chains ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The fragment method of calculation partition coefficients (P) has been extended to include the common amino acids (AAs). The results indicate that polar and charged side chains influence the hydrophobicity of atoms in the side chain in a predictable manner. Feild effects, as evidenced through polar proximity factors and bond factors, need to be considered for accurate estimation of transfer phenomena. The calculated log P and ΔG°′ values of the 20 AAs agree well with the observed values. Pro calculates to be more hydrophilic than the observed log P. Hydrophobicity scales for peptide side chain residues are compared and evaluated in terms of suitability. Calculated π values for nonpolar side chain residures agree well with the observed values; calculated values for uncharged polar side chain residues deviate by about 0.6 log units except for Gln and Cys; and polar side chain residues with charged side chains calculate as too hydorphilic. Reasons for the differences are explored. We also suggest that tightly bound water to polar moieties in amino acids and peptides may be transferred into the octanol phase during partitioning experiments. A quantitative methodology is persented which characterizes the thermodynamic partitioning of groups and individual atoms in amino acids and proteins.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prot.340020207
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    Masthead (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987) 
    Details
    ISSN: 0887-3585
    Keywords: Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prot.340020301
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  • 73
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    Intron/exon structure of the human gene for the muscle isozyme of glycogen phosphorylase (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 177-187 
    Details
    ISSN: 0887-3585
    Keywords: evolution ; protein structure ; nucleotide binding domain ; gene sequence ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The intron/exon organization of the human gene for glycogen phosphorylase has been determined. The segments of the polypeptide chain that corresponds to the 19 exons of the gene are examined for relationships between the three-dimensional structure to the protein and gene structure. Only weak correlations are observed between domains of phosphorylase and exons. The nucleotide binding domains that are found in phosphorylase and other glycolytic enzymes are examined for relationships between exons of the genes and structures of the domains. When mapped to the three-dimensional structures, the intron/exon boundaries are shown to be widely distributed in this family of protein domains.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/prot.340020303
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    Determination of three-dimensional protein structures from nuclear magnetic resonance data using fragments of known structures (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 188-201 
    Details
    ISSN: 0887-3585
    Keywords: NMR ; NOE ; protein conformation ; structure data base ; structure fragments ; modelling ; distance matrices ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A method to build a three-dimensional protein model from nuclear magnetic resonance (NMR) data using fragments from a data base of crystallographically determined protein structures is presented. The interproton distances derived from the nuclear Overhauser effect (NOE) data are compared to the precalculated distances in the known protein structures. An efficient search algorithm is used, which arranges the distancs in matrices akin to a Cα diagonal distance plot, and compares the NOE distance matrices for short sequential zones of the protein to the data base matrices. After cluster analysis of the fragments found in this way, the structure is built by aligning fragments in overlapping zones. The sequentially long-range NOEs cannot be used in the initial fragments search but are vital to discriminate between several possible combinations of different groups of fragments. The method has been tested on one simulated NOE data set derived from a crystal structure and one experimental NMR data set. The method produces models that have good local structure, but may contain larger global errors. These models can be used as the starting point for further refinement, e.g., by restrained molecular dynamics or interactive graphics.
    Additional Material: 12 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prot.340020304
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  • 75
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    Structure of an insect virus at 3.0 Å resolution (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 167-176 
    Details
    ISSN: 0887-3585
    Keywords: icosahedral ; insect ; virus ; structure ; evolution ; nodavirus ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: We report the first atomic resolution structure of an insect virus determined by single crystal X-ray diffraction. Black beetle virus has a bipartite RNA genome encapsulated in a single particle. The capsid contains 180 protomers arranged on a T = 3 surface lattice. The quaternary organization of the protomers is similar to that observed in the T = 3 plant virus structures. The protomers consist of a basic, crystallographically disordered amino terminus (64 residues), a β-barrel as seen in other animal and plant virus subunits, an outer protrusion composed predominantly of β-sheet and formed by three large insertions between strands of the barrel, and a carboxy terminal domain composed of two distorted helices lying inside the shell. The outer surfaces of quasi-threefold related protomers form trigonal pyramidyl protrusions. A cleavage site, located 44 residues from the carboxy terminus, lies within the central cavity of the protein shell.The structural motif observed in BBV (a shell composed of 180 eight-stranded antiparallel β-barrels) is common to all nonstatellite spherical viruses whose structures have so far been solved. This highly conserved shell architecture suggests a common origin for the coat protein of spherical viruses, while the primitive genome structure of BBV suggests that this insect virus represents an early stage in the evolution of spherical viruses from cellular genes.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/prot.340020302
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    Association of calmodulin and smooth muscle myosin light chain kinase: Application of a lable selection technique with trace acetylated calmodulin (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 202-209 
    Details
    ISSN: 0887-3585
    Keywords: myosin light chain kinase ; trace acetylation ; label selection ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A method is described for rapidly surveying the effects of modifying individual amino acid residues of a protein on its ability to interact specifically with another macromolecule. The procedure has been used to examine the individual roles of the seven lysyl residues of calmodulin in its ability to bind to smooth muscle myosin light chain kinase; previous studies by Jackson et al. (J. Biol. Chem. 261:1226-12232, 1986) have suggested that certain lysines may be located close to the interaction site. Trace [3H]-acetylated calmodulin, consisting predominantly of molecules acetylated at single sites together with unmodified protein, was incubated in excess (five- to 20-fold) with smooth muscle MLC kinase to allow the modified and unmodified molecules to compete for binding to the enzyme. Subsequently, the calmodulin-enzyme complex was separated from unbound calmodulin, and the level of acetylation of each of the seven lysines of the bound fraction of calmodulin was determined and compared to that of each corresponding group of the starting preparation. Significant changes were found at only two of the lysines, 21 and 75, where the extent of acetylation in the bound fraction was three- and fivefold lower, respectively, than that in the original preparation. These results were reproducible in three separate selection experiments employing both chicken and turkey gizzard MLC kinase. It is concluded that acetylation of calmodulin at either lysine 21 or 75 markedly reduces its affinity for MLC kinase, but acetylation at any of the other lysines (13, 30, 77, 94, or 148) has only minor effects. This finding supports the proposal that the face of the central helix containing lysine 75 is involved in interaction with MLC kinase and suggests also that additional contact near Ca2-binding site 1 occurs.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prot.340020305
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    Prediction of the tertiary structure of the α-subunit of tryptophan synthase (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 210-224 
    Details
    ISSN: 0887-3585
    Keywords: protein folding ; circular dichroism ; protein secondary structure ; heuristic prediction of protein structure ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The tertiary structure of the α-subunit of tryptophan synthase was proposed using a combination of experimental data and computational methods. The vacuum-ultraviolet circular dichroism spectrum was used to assign the protein to the α/β-class of supersecondary structures. The two-domain structure of the α-subunit (Miles et al.: Biochemistry 21:2586, 1982; Beasty and Matthews: Biochemistry 24:3547, 1985) eliminated consideration of a barrel structure and focused attention on a β-sheet structure. An algorithm (Cohen et al.: Biochemistry 22:4894, 1983) was used to generate a secondary structure prediction that was consistent with the sequence data of the α-subunit from five species. Three potential secondary structures were then packed into tertiary structures using other algorithms. The assumption of nearest neighbors from second-site revertant data eliminated 97% of the possible tertiary structures; consideration of conserved hydrophobic packing regions on the β-sheet eliminated all but one structure. The native structure is predicted to have a parallel β-sheet flanked on both sides by α-helices, and is consistent with the available data on chemical cross-linking, chemical modification, and limited proteolysis. In addition, an active site region containing appropriate residues could be identified as well as an interface for β2-subunit association. The ability of experimental data to facilitate the prediction of protein structure is discussed.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prot.340020306
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    Modeling the biochemical differences between rabbit muscle and human liver phosphorylase (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 225-235 
    Details
    ISSN: 0887-3585
    Keywords: allosteric ; tissue-specific isozymes ; protein structure ; AMP ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Glycogen phosphorylases catalzye the regulated breakdown of glycogen to glucose-1-phosphate. In mammals, glycogen phosphorylase occurs in three different isozymes called liver, muscle and brain after the tissues in which they are prefer entially expressed. The muscle isozyme binds and is activated cooperatively by AMP. In contrast, the liver enzyme binds AMP noncooperatively and is poorly activated. The amino acid sequence of human liver phosphorylase is 80% identical with rabbit muscle phosphorylase, and those residues which contact AMP are conserved. Using computer graphics software, we replaced side chains of the known rabbit muscle structure with those of human liver phosphorylase and interpreted the effects of these changes in order to account for the biochemical differences between them. We have identified two substitutions in liver phosphorylase potentially important in altering the cooperative binding and activation of this isozyme by AMP.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prot.340020307
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  • 79
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    Stability of wild-type and mutant RTEM-1 β-lactamases: Effect of the disulfide bond (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 290-297 
    Details
    ISSN: 0887-3585
    Keywords: mutants ; structural function relationships ; protein folding and stability ; catalysis ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Uniquely among class A β-lactamases, the RTEM-1 and RTEM-2 enzymes contain a single disulfide bond between Cys 77 and Cys 123. To study the possible role of this naturally occurring disulfide in stabilizing RTEM-1 β-lactamase and its mutants at residue 71, this bond was removed by introducing a Cys 77 → Ser mutation. Both the wild-type enzyme and the single mutant Cys 77 → Ser confer the same high levels of resistance to ampicillin in vivo to Echerichia coli; at 30°C the specific activity of purified Cys 77 → Ser mutant is also the same as that of the wild-type enzyme. Also, neither wild-type enzyme nor the Cys 77 → Ser mutant is inactivated by brief exposure to p-hydroxymercuri-benzoate. However, above 40°C the mutant enzyme is less stable than wild-type enzyme. After introduction of the Cys 77 → Ser mutation, none of the double mutants (containing the second mutations at residue 71) confer resistance to ampicillin in vivo at 37°C; proteins with Ala, Val, Leu, Ile, Met, Pro, His, Cys, and Ser at residue 71 confer low levels of resistance to ampicillin in vivo at 30°C. The use of electrophoretic blots stained with antibodies against β-lactamase to analyze the relative quantities of mutant proteins in whole-cell extracts of E. coli suggests that all 19 of the doubly mutant enzymes are proteolyzed much more readily than their singly mutant analogues (at Thr 71) that contain a disulfide bond. Thus, the disulfide bond of the RTEM-1 β-lactamase seems able to reduce the destabilizing effect of mutations at Thr 71. These results also emphasize the unique and essential role that Thr 71 performs in the stable folding of RTEM-1 β-lactamase and presumably the other class A β-lactamases.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prot.340020405
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    Synthetic peptides corresponding to sequences of snake venom neurotoxins and rabies virus glycoprotein bind to the nicotinic acetylcholine receptor (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 298-307 
    Details
    ISSN: 0887-3585
    Keywords: α-bungarotoxin ; neurotropism ; rhabdo-virus ; α-subunit ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Peptides corresponding to portions of loop 2 of snake venom curare-mimetic neurotoxins and to a structually similar region of rabies virus glycoprotein were synthesized. Interaction of these peptides with purified Torpedo electric organ acetylcholine receptor was tested by measuring their ability to block the binding of 125I-labeled α-bungarotoxin to the receptor. In addition, inhibition of α-bungarotoxin binding to a 32-residue synthetic peptide corresponding to positions 173-204 of the α-subunit was determined. Neurotoxin and glycoprotein peptides corresponding to toxin loop 2 inhibited labeled toxin binding to the receptor with IC50 values comparable to those of nicotine and the competitive antagonist d-tubocurarine and to the α-subunit peptides with apparent affinities between those of d-tubocurarine and α-cobratoxin. Substitution of neurotoxin residue Arg37, the proposed counterpart of the quatenary ammonium of acetylcholine, with a negatively charged Glu residue reduced the apparent affinity about 10-fold. Peptides containg the neutotoxin invarint residue Trp29 had 10- to 100-fold higher affinites than peptides lacking this residue. These results demonstrate that relatively short synthetic peptides retain some of binding ability of the native protein from which they are derived, indicating that such peptides are useful in the study of proetin interactions. The ability of the peptides to compete α-bungarotoxin binding to the receptor with apparent affinites comparable to those of other cholinergic ligands indicates that loop 2 of the neurotoxins and the strucually similar segment of the rabies virus glycoprotein act as recognition sites for the acetylcholine receptor. Invarient toxin residues Arg37 and Trp29 and their viral homologs play important, although not essential, roles in binding, possibly by interaction with complementary anionic and hydrophobic subsites on the acetylcholine receptor. The α-subunit peptide most likely contains all of the determinants for binding of the toxin and glycoprotein peptides present on the α-subunit, because these peptides bind to the 32-residue α-subunit peptides with the same or greater affinity as to the intact subunit.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prot.340020406
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    Normal modes of vibration in bovine pancreatic trypsin inhibitor and its mechanical property (1987)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 2 (1987), S. 308-329 
    Details
    ISSN: 0887-3585
    Keywords: conformational dynamics ; normal mode analysis ; Young's modulus ; rigid structural elements ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The normal mode analysis of conformational fluctuation is carried out for a small globular protein, bovine pancreatic trypsin inhabitor. Results are analyzed mainly to reveal the mechanical construction of the protein molecule. We take dihedral angles, including peptide ω angles, as independent variables for the normal mode analysis. There are 306 such angles in this molecule. Motions in modes with frequencies lower than 120 cm-1 are showned to involve atoms in the whole protein molecule, and spatial change of displacement vectors is continues, i.e., those of atoms near in space are similar. To quantitate the observation of the continuity, a correlation function of direction vectors of atomic displacement is calculated. From this function we define a Quantity that is interpreted as the wave length of an equivalent elastic plane wave. From this Quantity we deduce eefective young's modulus for each mode. For the mode with the lowest frequency 4.4 cm-1, it terned out to be 0.8 × 109 dyn cm-2, the value two orders magnitude softer than, for instance, α-helices. Prompted by this observation, the four lowest frequency modes and also the harmonic motions in the thermal equilibrium are analyzed further mainly to detect relatively rigid structural elements in the molecule. From this analysis emerges a mechanical picture of the protein molecule that is made up of relatively rigid elements held together by very soft parts.
    Additional Material: 15 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prot.340020407
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    Gas chromatography mass spectrometry of some thermally labile urea pesticides (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 39-42 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The application of gas chromatography/mass spectrometry to three thermally labile phenylurea pesticides is reported. Using alcohols as solvents the decomposition of the pesticides is followed by a reaction in which esters of N-(3,4-dichlorophenyl)carbamic acid are formed. As these reactions occur during the gas chromatographic analysis, it is the esters which are identified in the mass spectrometer. The methyl ester is itself a pesticide so an erroneous conclusion about the original pesticide could be reached when methanol is the solvent.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140109
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    252Cf plasma desorption fourier transform ion cyclotron resonance mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 43-45 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The ions produced by 252Cf plasma desorption are detected by Fourier transform ion cyclotron resonance techniques. Results for CsI and N,N,N-trimethyl-p-aminophenolate iodide show the feasibility of the technique with high resolution (up to 11 000 at m/z 23) and good signal-to-noise ratio (up to 726).
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140110
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    Camera-ready BEMS short communications - guidelines for authors (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 47-48 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140111
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    BEMS short communication (camera-ready example) (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 49-50 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140112
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    Forthcoming events (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 51-51 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140113
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    Fast atom bombardment mass spectrometry of butyloxycarbonyl protected (BOC) peptides (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 53-61 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The fast atom bombardment positive ion mass spectra and the [M + H]+ collisional activation spectra of t-butyloxycarbonyl protected peptides and the unprotected analogues have been compared. It is concluded that sequence information, especially from the collisional activation spectra, can better be derived from the underivatized peptides than from the BOC-peptides.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140202
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    Profiling and quantification of biogenic amines in wine by constant B2E linked scan mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 229-233 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The constant B2E linked scan is shown to be an excellent tool for the profiling of biogenic amines in wine samples. The fragment ion at m/z 169 of the dansylated amines is used for the precursor ion search in combination with direct sample evaporation. Besides the profile a semi-quantification may be achieved when using suitable amines as internal standards with standard deviations of 12-17%. More accurate results with standard deviations of 3-5% are obtained when using deuterated analogues as internal standards. Both methods are applied to the analysis of biogenic amines in synthetic mixtures and actual wine samples.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140506
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    252-Californium plasma desorption mass spectrometry of glycerophospholipids (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 241-246 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 252-Californium plasma desorption mass spectrometry was applied to the study of five different classes of phospholipids namely phosphatidylcholine, phosphatidylethanolamine, phosphatidylglycerol, phosphatidylserine and phosphatidylinositol. Positive and negative ion spectra were compared to spectra obtained using other ionization techniques. Plasma desorption mass spectra provide useful information on the molecular weight of compounds from all classes, particularly in the case of phosphatidylserine - a class that has failed to show satisfactory quasimolecular ions with either Fast atom bombardment, FAB or Field desorption, FD. The observed fragmentation is also indicative of the structure of the studied compounds.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140508
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  • 90
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    Quantitative analysis of S3341 in human plasma and urine by combined gas chromatography - negative ion chemical ionization mass spectrometry: 15 month inter-day precision and accuracy validation (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 289-293 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new quantitative assay for the determination of S3341, an alpha-2 agonist antihypertensive drug, has been developed using combined gas chromatography-negative ion chemical ionization mass spectrometry. The [M]-. ions from TFA derivatives of S3341 (m/z 276) and the internal standard (2H4)S3341 (m/z 280) are monitored simultaneously by selected ion monitoring. For S3341 concentrations ranging from the limit of detection (0.2 ng ml-1 using 1 ml of plasma) to 5 ng ml-1, the average assay precision (CV) is approximately 7% while the average assay accuracy (percentage of error) is 4%. Validation of the day-to-day precision and accuracy was realized after analysing control plasma samples (n = 295) concurrently with the biological samples collected during the pharmacokinetic studies conducted over 15 months. The average day-to-day precision (CV) and accuracy (percentage of error) are 10% and 6% respectively, thus indicating that this assay procedure routinely provides reliable analytical data.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140608
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  • 91
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    Improvement in sensitivity of fast atom bombardment mass spectrometry of amino acids by di-isopropylphosphorylation (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 331-333 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Positive ion fast atom bombardment mass spectrometric sensitivities of seven amino acids and the corresponding di-isopropylphosphorylated derivatives were carefully compared. Results showed that an improvement in sensitivity by factors of 4-29, mostly above 10, were achieved after the derivatization. The chemical noise derived from glycerol matrix was also greatly reduced by this derivatization.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200140706
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  • 92
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    Analysis of cholesterol, cholesterol-5,6-epoxides and cholestane-3β,5α,6β-triol in nipple aspirates of human breast fluid by gas chromatography/mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 335-338 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method has been developed for the quantitative determination of cholesterol and three of its major oxidative metabolites (the 5α,6α-epoxide, the 3β,5α,6β-triol, and the 5β,6β-epoxide) in a single sample of human breast fluid (2-50 μl), using gas chromatography/mass spectrometry with selected ion monitoring. High specificity and reliable quantification is achieved by the use of the inverse stable isotope dilution method, employing deuterium-labeled variants of the compounds as internal standards.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140707
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  • 93
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    Simultaneous determination of pool sizes and fractional turnover rates, of deoxycholic acid, cholic acid and chenodeoxycholic acid in man by isotope dilution with 2H and 13C labels and serum sampling (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 609-611 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This paper describes a method for simultaneous determination of the kinetics of the three major bile acids in man using (2,2,4,4-2H4) deoxycholic acid, (24-13C) cholic acid and (24-13C) chenodeoxycholic acid. The gas chromatographic/mass spectrometric-selected ion monitoring technique used provided complete separation of deoxycholic acid, cholic acid and chenodeoxycholic acid, which permitted simultaneous measurement of isotope ratios for all three bile acids. Since measurement of all three pool sizes and fractional turnover rates in a single experiment requires different isotopic labels for deoxycholic acid and cholic acid, we investigated the in vivo stability and applicability of (2,2,4,4-2H4) deoxycholic acid as a stable isotope marker for isotope dilution studies in man. No consistent differences were observed between deoxycholic acid pool sizes and fractional turnover rates determined in serum samples after administration of (2,2,4,4-2H4) deoxycholic acid and (24-13C) deoxycholic acid. Simultaneous administration of (2,2,4,4-2H4) deoxycholic acid (24-13C) cholic acid and (24-13C) chenodeoxycholic acid and isotope ratio measurements in serum permitted determination of pool sizes and fractional turnover rates of the three major bile acid and the 7α-dehydroxylation fraction. Pool sizes, fractional turnover rates and synthesis rates (input rates) agreed well with data obtained previously with (24-13C) labels in independent studies.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141106
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  • 94
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    Identification of new steroids in patients with 17α-hydroxylase deficiency by capillary gas chromatography/mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 633-637 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Urines of two children with 17α-hydroxylase deficiency contained a number of 5-pregnane- and pregnenediols, -triols and -tetrols with a hydroxy or oxo group in position 11 of the steroid ring. They are formed mainly from progesterone via 11-hydroxyprogesterone, pregnanolone and corticosterone, respectively, or from pregnenolone. Three metabolites not previously described, 16-hydroxypregnenolone, 6,21-dihydroxypregnanediol and 6-hydroxytetrahydrocorticosterone, were identified.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141111
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  • 95
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    Gas chromatographic/mass spectrometric studies of the urinary metabolites of male rats given indan (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 649-651 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The identified urinary metabolites of male rats exposed to indan are: 1- and 2-indanone; 1-, 2- and 5-indanol; 2-and 3-hydroxyl-1-indanone; and cis- and trans-indan-1,2-diol. Indan causes kidney damage in male rats in a manner similar to the cyclic hydrocarbons cis- and trans-decalin and JP-10. Lesions produced by indan occur only in male rats and not in female or control rats.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141114
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  • 96
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    Routine gas chromatographic/mass spectrometric analysis of urinary organic acids. Results over a three-year period (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 663-668 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Organic acidaemias are an important part of inborn errors of metabolism. The biochemical diagnosis is based on gas chromatographic/mass spectrometric identification of urinary organic acids. Since 1973 we have used gas chromatographic analysis of the methyl esters of urinary organic acids. Mass spectral identification was performed only when an abnormal gas chromatographic profile was suspected. In 1983 we introduced routine gas chromatographic/mass spectrometric analysis organic acids. More than 1500 urine samples from 1000 children have been analysed and we encountered more than 40 abnormal profiles: 18 classical organic acidaemias (propionic, methyl-malonic, isovaleric, glutaric type I and 3-hydroxy-3-methyl glutaric acidaemias); 6 aminoacidopathies with excretion of branched chain keto acids (leucinosis) or succinylacetone (tyrosinosis type I); 14 massive dicarboxylic acidurias with excretion of suberyl and hexanoyl glycine and deficiency of the medium chain acyl CoA dehydrogenase in four patients. The use of gas chromatography/mass spectrometry routinely allows the identification of abnormal metabolites excreted in small amounts: β-methyl-crotonyl glycine indicative of biotin deficiency: γ-hydroxybutyric acid; and 3-methyl-glutaconic + 3-methy-glutaric acid is in a 3-methyl-glutaconic aciduria type II. Abnormal profiles due to metabolites of drugs as valproate, salicylate and barbiturate can be recognized immediately. This simple gas chromatographic/mass spectrometric system can lead to diagnosis, in one day, of rare but severe diseases needing a specific and early treatment.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141117
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  • 97
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    Determination of serum cortisol by thermospray liquid chromatography/mass spectrometry: Comparison with gas chromatography/mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 717-722 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The determination of serum cortisol by thermospray liquid chromatography/mass spectrometry (LC/MS) has been assessed. The method incorporates stable isotope dilution and innumoadsorption extraction. [M + H]+ ions are monitored during LC/MS. The within-assay reproducibility is satisfactory (coefficient of variation 7% at a concentration of 190 ng ml-1), though inferior to that achieved with the (more lengthy) procedure of gas chromatography/mass spectrometry (GC/MS). Satisfactory agreement between LC/MS (y) and GC/MS (x) data was observed (y = 0.934x + 12.4 ng ml-1; r = 0.968; n = 14). It is concluded that the generation of precise reference data for the assessment of routine cortisol assays is at present better achieved by GC/MS. LC/MS, however, provides satisfactory quantitative data via a more simple and rapid method.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141205
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  • 98
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    The alkylthio-isoindole derivatives of biogenic amines: A mass spectrometric study (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 737-738 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141208
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  • 99
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    Sequence analysis of unprotected tri-deoxyribonucleoside diphosphates by 252Cf-plasma desorption mass spectrometryThis paper is part III of a series ‘252Cf-Plasma Desorption Mass Spectrometry of oligonucleotides’. Part II corresponds to Ref. 12. (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 83-90 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The negative Plasma Desorption Mass Spectra of ten unprotected tri-deoxyribonucleoside diphosphatesHereafter termed tri-deoxyribonucleotides. have been observed and analysed in detail. They all exhibit molecular ions as well as a characteristic fragmentation pattern. The ten trinucleotides selected were chosen in order to understand, in terms of sequence, the main features of the experimental spectra. It is shown that the structure and the sequence of the oligomers can be rapidly and easily derived from their PD Mass Spectrum.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140206
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  • 100
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    Redox reactions occurring during secondary ion mass spectrometry of some heteroanthracycline antitumor antibiotic precursors (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 91-96 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Positive and negative secondary ion mass spectra of the title compounds were produced by bombardment of solid deposits by 13 and 23 KeV cesium ions, respectively, and analyzed with a time-of-flight mass spectrometer. In addition to familiar protonation and alkali (mainly sodium) ion addition processes observed in the positive ion spectra and proton abstractions in the negative ion spectra (which enable determination of molecular weight) there is evidence from both spectral modes for oxidation-reduction processes in which species such as [M - H]+, [M - H + Na]+. and [M + 1]- are formed. It is argued that these may be formed rapidly from pre-associated molecules during bombardment/ionization rather than as a result of radiation damage. Sodium ion addition is apparently facilitated by the presence of electron pair donor groups, especially if chelation is possible.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140207
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