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  • 1985-1989  (8,905)
  • Analytical Chemistry and Spectroscopy  (5,836)
  • Engineering General  (2,473)
  • Life Sciences  (596)
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  • 1
    Electronic Resource
    Electronic Resource
    Separation of some antihistamines on impregnated TLC silica plates (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 46-47 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Different metal salts have been tried as impregnating reagents for developing TLC separation schemes for some antihistamines on silica gel ‘G’ plates, using a new solvent system benzene + dimethyl formamide + acetic acid (30:10:7). Spots were visualized by spraying with a solution of Dragendroff's reagent.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130030112
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  • 2
    Electronic Resource
    Electronic Resource
    Product news (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), 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.1130030114
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  • 3
    Electronic Resource
    Electronic Resource
    A simplified method for the preparation of wga-sepharose 4B and its use in the purification of MN blood group antigens (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 10-13 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simplified method for the preparation of wheat germ agglutinin(WGA)-Sepharose 4B by coupling highly purified WGA, prepared by improved affinity chromatography, with BrCN activated Sepharose 4B in a solution of high carbonate buffer is described. The amount of WGA linked to Sepharose 4B was 82.40% (3.07 mg WGA per ml Sepharose 4B). MN blood group antigens of human erythrocyte membranes purified with WGA-Sepharose 4B affinity chromatography showed a single band on sodium dodecyl sulfate/polyacrylamide gel electrophoresis (SDS/PAGE). The yield of the antigens from 400 mL fresh blood was 32-40 mg. The WGA-Sepharose 4B column could be used several times without loss of activity.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130030104
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  • 4
    Electronic Resource
    Electronic Resource
    A simple method for the characterization of photoproducts from DNA applied to the cis-syn thymine dimer (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 32-34 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A method for the unambiguous characterization of DNA photoproducts has been developed. It does not require radio-labelled DNA, or specialized techniques. In the preliminary step, UV-irradiated DNA is hydrolysed to its constituent bases and photoproducts. The photoproducts are then separated from nucleic acid bases using low pressure ion-exchange chromatography on a Dowex 1 × 8 200-400, and an Amberlite CG-50-H+ column. Further separation and purification of photoproducts is carried out on the HPLC Whatman Partisil ODS2 column, using 15% MeOH. The procedure is simple, reproducible and versatile.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130030108
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  • 5
    Electronic Resource
    Electronic Resource
    Improved TLC systems for rapid resolution of phenyl thiohydantoin amino acids (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 43-45 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Two new solvent systems, n-hexane + propionic acid (26:5, v/v) and chloroform + acetone (29:3, v/v), for the rapid resolution and identification of an 18-component mixture of phenylthiohydantoin amino acids are reported. Using these systems certain difficult combinations of phenylthiohydantoin amino acids are resolved. Two more solvent systems, viz chloroform+acetic acid (27:3, v/v) and chloroform + methanol (30:4, v/v), are developed to resolve phenylthiodantoin derivatives of aspartic and glutamic acids.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130030111
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  • 6
    Electronic Resource
    Electronic Resource
    Calendar of events (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), 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.1130030113
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  • 7
    Electronic Resource
    Electronic Resource
    Simultaneous measurement of ethosuximide and phenobarbital in brain tissue, serum and urine by HPLC (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 49-52 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple rapid method for simultaneous ethosuximide and phenobarbital assay in brain tissue, serum and urine has been developed. Extraction of samples from brain tissue and serum were performed with dichloromethane at low pH in the presence of an excess of ammonium sulfate. Glucuronide conjugates in urine samples were hydrolyzed by enzymatic cleavage with β-glucuronidase and then extracted with dichloromethane. The extracts were analyzed using a Spherisorb 5 ODS column and a mixture of acetonitrile, methanol and phosphate buffer (21: 24: 55, v/v) as eluent. No interference was encountered and the method is both precise and reproducible.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130030202
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  • 8
    Electronic Resource
    Electronic Resource
    Determination of halofuginone in bovine plasma by competing-ion high performance liquid chromatography after solid phase extraction (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 136-138 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A high performance liquid chromatographic (HPLC) method for the determination of the anticoccidial and antitheilerial drug halofuginone in bovine plasma was developed. Samples were diluted with acetic acid (10%, v/v) and cleaned up on a Bond Elut C8 column. The analyte was eluted from the extraction column and chromatographed by reversed-phase HPLC using decylamine as a competing-ion reagent. Detection was by UV at 243 nm. Recovery from plasma was 75%, and within-day and between-day coefficients of variation were 5.23 and 6.35% respectively. The specificity and sensitivity of this method (limit of detection in plasma, 1 ng/mL) were sufficiently high to enable us to characterize the time course of the drug in plasma after oral administration of therapeutic doses to cattle.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130030310
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  • 9
    Electronic Resource
    Electronic Resource
    Masthead (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989) 
    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.1130030401
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  • 10
    Electronic Resource
    Electronic Resource
    Determination of total and free concentration of propranolol in human plasma by displacement electrophoresis in a two-layer polyacrylamide gel using fluorimetric detection (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 161-165 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A new method based on displacement electrophoresis has been developed for the determination of the total and free concentration of propranolol, a β-adrenergic blocker drug, in plasma. To determine the total concentration the drug is extracted from human plasma into a chloroform + heptane mixture in the presence of ammonia. After evaporation of the solvent mixture the residue is submitted to displacement electrophoresis in a glass tube containing a two-layer polyacrylamide gel. When the propranolol electrophoretically leaves the gel column it is transferred by a buffer flow to the cuvette of a fluorimeter for continuous detection and quantification. The concentration of the free non-protein bound drug can be determined by the same displacement electrophoresis technique following extraction of the plasma sample into the above organic solvent mixture in the absence of ammonia. Alternatively the extraction procedure can be exchanged for dialysis for 1 h. To decrease the risk that large size material might comigrate with propranolol two layers of polyacrylamide are used, one having small pores to retard such material. In addition, we use fluorimetric detection which means that many possible contaminants are not recorded and therefore do not affect a quantitative determination of propranolol.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130030405
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  • 11
    Electronic Resource
    Electronic Resource
    Multidimensional chromatographic separation of estrogen receptors (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 255-261 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Analyses of estrogen and progesterone receptors in biopsies of breast carcinoma play a vital role in the selection of patients likely to respond to hormone manipulation. Sucrose density gradient centrifugation has been the reference method in the determination of estrogen receptors in human breast carcinoma cytosols. To reduce assay time and circumvent prolonged manipulation of labile receptor preparations, high performance liquid chromatography techniques in the size-exclusion and ion-exchange modes were compared as potential alternate methods for the rapid separation of receptor isoforms. Multidimensional analyses were performed by reapplying estrogen receptor isoforms obtained from high performance size-exclusion and ion-exchange chromatography to sucrose density gradients and vice versa. This confirmed that the estrogen-binding components identified by high performance liquid chromatography appear to correspond to estrogen receptor species from sucrose density gradients.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130030606
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  • 12
    Electronic Resource
    Electronic Resource
    Rapid determination of the benzodiazepine antagonist flumazenil, Ro 15-1788, by high performance liquid chromatography (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 269-271 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A sensitive (2 ng/mL) and specific method for the determination of the benzodiazepine antagonist Ro 15-1788 or flumazenil is described. Following a simple extraction, the compound is analyzed by reversed phase high performance liquid chromatography (HPLC) and detection at 245 nm. The method was applied to plasma specimens collected from patients receiving a single dose of this drug.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130030609
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  • 13
    Electronic Resource
    Electronic Resource
    Capillary gas chromatographic determination of epomediol in human plasma and urine using a rapid solid-phase extraction (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 199-202 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple and precise method for the quantitation of epomediol in human plasma and urine is described. Each biological sample is added with the internal standard and applied directly to an Extrelut-1 solid-phase column. After absorption the column is eluted with chloroform and the eluate is evaporated to dryness. The residue, reconstituted in ethanol, is analysed by capillary gas chromatography. No interferences from possible metabolites or endogenous constituents can be noted. The method has been applied to human pharmacokinetic studies: the results of a subacute administration to volunteers are presented.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130030505
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  • 14
    Electronic Resource
    Electronic Resource
    High performance liquid chromatography stability study of malonyl-coenzyme A, using statistical experimental designsThis paper is dedicated to Prof. P. De Moerloose on the occasion of his 65th birthday. (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 213-216 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Malonyl-CoA is a biochemically important compound, formed by an acetyl-coenzyme A carboxylase catalysed reaction. The stability of this short-chain coenzyme A derivative under various experimental conditions is discussed in this article. High-performance liquid chromatography was used for the analysis of the reaction mixture because of its excellent selectivity and sufficient sensitivity. Several variables were investigated as possible stability-influencing factors: pH, magnesium and buffer concentration, reaction temperature and time. The Plackett-Burman screening design was first used for selecting the most important variables, with which a central composite design was constructed. In this way, a response surface was obtained with the percentage remaining malonyl-CoA as a function of magnesium concentration, reaction temperature and time. The usefulness of this approach is demonstrated by obtaining kinetic data from the mathematical function and by the evaluation of the stopping of reaction procedure in the activity assay of acetyl-coenzyme A carboxylase.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130030508
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  • 15
    Electronic Resource
    Electronic Resource
    Isolation of glycoprotein D from herpes simplex virus type 1 by gel filtration high performance liquid chromatography (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 221-225 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Rabbit kidney (RK-13) and human jejunum and ileum (I-407) cells infected with herpes simplex virus type 1, strain F, were radiolabelled with [14C]glucosamine or [35S]methionine for 24 h. The cells were extracted with 1% Triton X-100 and the extracts were separated by gel filtration high performance liquid chromatography. Monoclonal antibody immunoprecipitation of the fractions collected from the column revealed a monomeric glycoprotein D (gD) of 52 - 56 000 molecular weight from RK-13 cells and two monomeric forms of gD, 54 000 and 58 000 molecular weight, from I-407 cells. Densitometry scanning of the autoradiograms from SDS-PAGE showed gD from the RK-13 host cells to be 98.7% pure with the [35S]methionine label and 97.0% pure with the [14C]glucosamine. On the other hand, gD from the I-407 host cells was only 78.6% with the [35S]methionine label and 96% pure with the [14C]glucosamine. This method could provide a means for the isolation of native gD for structural and immunological studies.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130030510
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  • 16
    Electronic Resource
    Electronic Resource
    Thin layer chromatography of dansyl and dinitrophenyl derivatives of amino acids. A review (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 233-240 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The dinitrophenyl (DNP) derivatives of amino acids have found continual application in protein sequencing since Sanger used them for the first time for the sequencing of insulin. Dansyl derivatives of amino acids have been widely used in protein sequencing because of their fluorescent nature. The success of protein sequencing largely depends upon correct identification of such derivatives. The choice for the method of identification is related to cost, the availability of instrumentation and to the sensitivity needed for the analysis. Thin layer chromatography (TLC) is simple and has several advantages over other chromatographic methods. Therefore the literature after 1972 is reviewed for TLC analysis of dansyl- and DNP-amino acids, the two important amino acid derivatives required for identifying protein sequences. Additionally, the literature on the TLC resolution of enantiomeric mixtures of dansyl amino acids is reviewed. Application of various adsorbents, composition of solvent systems and other experimental conditions together with successful resolution data have been discussed. TLC provides a direct and inexpensive method for the resolution of enantiomers, and is fast becoming a sensitive instrumentalized quantitative analytical technique.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130030602
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  • 17
    Electronic Resource
    Electronic Resource
    Simultaneous determination of some organophosphorus pesticides by high performance liquid chromatography (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 272-273 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: An HPLC method for the simultaneous detection of six organophosphorus pesticides (Dimethoate, Ethion, Malathion, Phorate, Phosalone and Parathion) on a Zorbex ODS column using methanol + water (80: 20) as solvent is described.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130030610
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  • 18
    Electronic Resource
    Electronic Resource
    High performance liquid chromatography of biological polyamines using immobilized enzyme as post-column reactor followed by electrochemical detection (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 187-191 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A novel analytical method for biological polyamines (putrescine, spermidine and spermine) was developed. Polyamines were separated by ion-pair reversed phase chromatography using a polymer-based octadecyl bonded column. A polyamine oxidase immobilized column worked effectively as a post-column reactor to convert polyamines to hydrogen peroxide which was eventually detected by electrochemical oxidation on platinum electrode. This method required neither tedious derivatization nor gradient elution, permitting us to perform simple and rapid analysis of polyamines. The detection limits were 0.3, 0.6, and 4 pmol injected for putrescine, spermidine, and spermine, respectively with a linear range of two to three orders of magnitude. Chromatograms obtained with samples from human urine and rat brain homogenates demonstrated the high sensitivity and selectivity of the method.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130030502
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  • 19
    Electronic Resource
    Electronic Resource
    High performance ion exchange chromatography of human plasma lecithin: Cholesterol acyltransferase (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 276-278 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Highly purified monomeric human plasma lecithin:cholesterol acyltransferase (LCAT), completely free of apolipoprotein D, has been chromatographed on a MonoQ HR 5/5 anion exchanger. LCAT eluted as symmetrical peaks after 12.8 min and 14.8 min at pH 5.0 and pH 6.0, respectively, using a linear NaCl gradient. The corresponding concentrations of NaCI effecting desorption of LCAT from the anion exchanger were 125 mM and 175 mM. At both pH values human serum albumin eluted earlier and was well separated from the enzyme. Rechromatography of LCAT in the eluates from these experiments at acid pH, on high performance gel filtration, demonstrated absence of aggregation. The nonspecific adsorption during anion exchange chromatography at pH 5.0 and pH 6.0 was negligible, as demonstrated by a linear relationship between injected amounts of LCAT and recorded peak areas for a 2-20 μg protein range. Zone immunoelectrophoresis assay indicated unaltered immunoreactivity of the eluted LCAT.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130030612
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  • 20
    Electronic Resource
    Electronic Resource
    Reversed phase HPLC of different membrane-bound variant surface glycoprotein preparations from Trypanosoma brucei brucei (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 53-57 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The chromatographic behaviour of the membrane-attached variant surface glycoprotein (mfVSG) of bloodstream forms of Trypanosoma brucei brucei AnTat 1.1 A preparations were studied by reversed phase high performance liquid chromatography (RP-HPLC). Among the different preparation procedures used, only the trifluoroacetic acid extraction gave a mfVSG preparation which was eluted from the RP-HPLC column. As well as for the soluble variant surface glycoprotein (sVSG) it was found that different mfVSG forms were eluted at different organic solvent concentrations from the RP-HPLC column. In addition, in preliminary studies, we have attempted to characterize the factors responsible for the trypanosome surface coat assembly. Using chromatographic techniques (RP-HPLC and thin layer chromatography), the results suggest a close relationship between the content of lipid-containing species and the heterogeneity of mfVSG preparation.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130030203
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  • 21
    Electronic Resource
    Electronic Resource
    Masthead (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989) 
    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.1130030101
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  • 22
    Electronic Resource
    Electronic Resource
    Product news (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), 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.1130030214
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  • 23
    Electronic Resource
    Electronic Resource
    Product news (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), 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.1130030312
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  • 24
    Electronic Resource
    Electronic Resource
    Quantification of midodrine and its active metabolite in plasma using a high performance liquid chromatography column switching technique (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 153-156 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: An automated column-switching HPLC system is described for the simultaneous determination of midodrine, an alpha-adrenergic stimulating drug, and its active metabolite, ST-1059. Serum or plasma (850 μ L) is directly injected onto a RP 18 (30 μm particle size) pre-column (9 × 4 mm ID) which acts as an on-line liquid-solid extractor and analyte enrichment system. The injection is followed by washing steps. The fraction containing the analytes is transferred onto an analytical RP18 column via step gradient elution where the final analysis is performed. Fluorescence detection is used (λex 290 nm and λem 322 nm), and method detection limits of 0.8 ng/mL plasma were reached. These were sufficiently low to determine the plasma concentration-time profiles for both compounds following oral administration of 2.5 mg and 5 mg midodrine hydrochloride. The assay in serum or plasma was linear in the range of 1 to 15 ng analyte/mL, the recovery was 〉95%, and the reproducibility was sufficient. The assay was rugged and was maintained by routinely changing the home-made, dry packed pre-column every 20th serum injection.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130030403
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  • 25
    Electronic Resource
    Electronic Resource
    High performance liquid chromatographic determination of fluvoxamine in human plasma (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 177-179 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A method has been developed for the separation and measurement of fluvoxamine in human plasma by high performance liquid chromatography. The method uses metapramine as an internal standard and provides a limit of detection of about 1.5 ng/mL for fluvoxamine. At a concentration of 25 ng/mL, fluvoxamine could be measured within a coefficient of variation of ±5.82 of the mean and at 100 ng/mL within a CV of ±2.78 of the mean. The method has been applied to the analysis of plasma from patients undergoing fluvoxamine therapy.
    Additional Material: 1 Ill.
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    ‘In situ’ Edman degradation of protein(s) blotted to immobilon membranes suitable for unblocking reversible chemical modification and elimination of coomassie blue in sodium dodecyl sulfate-polyacrylamide gel electrophoresisWe dedicate this paper to Professor G. Biserte, Director of IRCL, deceased suddenly in December 1988. (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 173-176 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Conditions for unblocking reversible chemical modifications such as maleylation or citraconylation ‘in situ’ at the N-terminus of proteins after transfer of proteins to immobilon membranes from SDS-PAGE are described. Demaleylation or decitraconylation occurred at 55°C in 70% formic acid (pH 1.50) during 60 min. During the unblocking reaction, Coomassie blue dye was completely removed, resulting in superior high performance liquid chromatographic separation of phenylthiohydantoin-amino acid (PTH-AA) after Edman degradation (automatic gas phase sequencer). The protein fixed on the matrix after demaleylation and removal of Coomassie blue was not degraded. The possible cleavage at the aspartyl-prolyl peptide bonds was considered, but no side reaction was observed. Furthermore, the incubation time in 70% formic acid at 55°C could be reduced to 10 min in the absence of maleylation of the starting material, and this was suitable for the removal of Coomassie blue and the quantification of phenylthiolhydantoin-amino acids (PTH-AAs) by HPLC. The yield from the starting protein through SDS-PAGE, blotting, and Edman degradation to quantitative analysis of PTH-aminoacid(s) by HLPC was established.
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    Brian A. Bidlingmeyer (ed.). Preparative liquid chromatography. Journal of Chromatography Library 38. Elsevier, Amsterdam, 1987. ISBN 0-444-42832-1. 341 pp. £60.00 (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), 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.1130030411
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  • 28
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    Masthead (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989) 
    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.1130030501
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  • 29
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    Analysis of drug in tissue homogenates by high performance liquid chromatography with direct injection and column switching (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 192-195 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: An HPLC method with direct sample injections and column switching was investigated for the analysis of drugs in tissue homogenates. The appropriate precolumn packings and analytical column packings were surveyed in order to obtain quantitative recovery. The use of a large bore end-fitting filter for the precolumn avoided the interference due to minute tissue particles. A minicolumn was used to trap the analyte or clean up the sample. The method was applicable to hydrophilic as well as hydrophobic drugs in liver, kidney or heart tissues, and has been extensively used in the determination of drugs in centrifugal cell fractions such as the nucleus, mitochondria and microsome.
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  • 30
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    Determination of estriol and creatinine in urine by high performance liquid chromatography (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 196-198 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A quantitative method for the determination of estriol (E3) and creatinine (C) in random urine by high performance liquid chromatography is described. The mobile phase was a mixed solution of methanol and phosphate buffer (0.025 M, pH 6.5) and the detection wavelength was at 205 nm. The method was simple, rapid and accurate. The OCV for E3 and C using this method were 1.7 - 3.4% and 2.2 - 2.5%, respectively. The RCV for E3 and C were 6.2 - 7.0% and 4.5 - 6.9%, respectively. The recoveries were 87 - 104% for E3 and 98 - 103% for C, respectively. The method has been used for clinical determinations.
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  • 31
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    Application of high performance liquid chromatography combined with diode-array detection for analysis of proteins and peptides in human cerebrospinal fluid (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 203-208 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Different strategies for HPLC separation, including molecular sieving, ion-exchange, and hydrophobic interaction as well as reversed phase chromatography, were used to study molecular components in human cerebrospinal fluid (CSF). The separations were followed by photodiode-array UV detection, which is a recently developed technique allowing a direct and rapid discrimination between peptides and proteins differing in their content of aromatic amino acids. By the various HPLC techniques in conjunction with diode-array detection it was possible to identify and characterize several protein and peptide components present in CSF. The procedure also allowed quantitative analysis of CSF proteins using minute amounts of the fluid.
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    URL: http://dx.doi.org/10.1002/bmc.1130030506
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  • 32
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    Unconjugated methoxylated catecholamine metabolites in human saliva. Quantitation methodology and comparison with plasma levels (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 217-220 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A newly developed method for the simultaneous extraction and quantitation of the unconjugated levels of the catecholamine metabolites vanilmandelic acid (VMA), 3-methoxy-4-hydroxyphenylethylene glycol (MHPG) and homovanillic acid (HVA) in plasma by high performance liquid chromatography with electrochemical detection was modified and applied to studies of human saliva. The assay had a mean coefficient of variation under 3% for each of the metabolites. Levels of plasma VMA, MHPG and HVA were measured in 28 normal subjects and compared to their saliva levels, obtained before and after stimulation by mastication. Significant correlations were found between plasma and saliva MHPG and HVA, but there was no correlation between plasma and saliva VMA. Salivary MHPG and HVA can be reproducibly assayed and may be useful tools for indications of changes in central and peripheral catecholamine metabolism.
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  • 33
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    Analysis of leukotrienes by liquid chromatography/electrochemistry after conversion to dinitrobenzoate derivatives (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 5-9 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A sensitive liquid chromatography method has been developed using electrochemistry for the determination of leukotrienes in biological fluids. Biological specimens are treated with 3,5-dinitrobenzoyl chloride in acetonitrile which undergoes rapid reaction with hydroxyl groups of non-peptidic leukotrienes in the presence of pyridine and with amino groups of peptidic leukotrienes in the presence of potassium tetraborate buffer. The resulting dinitroben-zoate derivatives of leukotrienes are highly electroactive, suitable for reduction or oxidation at moderate potentials by an electrochemical detector. In reductive mode at -0.7 V or oxidative mode at + 1.15 V potentials, the lower limits of detection for leukotriene derivatives were approximately 8±3 pg and 70 ± 16 pg respectively, with a signal-to-noise ratio of 5 to 1. This method was applied to the detection of leukotrienes in plasma, nasal and bronchial fluids of patients with asthma.
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    Compositional analysis of the three main gangliosides from adult human myometrium by a rapid capillary gas chromatographic method (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 29-31 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A new capillary GC method is described for the compositional analysis of the three main gangliosides isolated from adult human myometrium. The sample was subjected to methanolysis, acetylation and trimethylsilylation which allows all the constituents to be analyzed simultaneously. The predominant ganglioside was found to be GD3, with GM3 and GT1b the next most abundant.
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  • 35
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    Determination of Δ1-tetrahydrocannabinol in human fat biopsies from marihuana users by gas chromatography-mass spectrometry (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 35-38 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A gas chromatographic-mass spectrometric (GC/MS) method for analysis of Δ1-tetrahydrocannabinol (Δ1-THC) in human fat samples is described. The fat sample, obtained from heavy marihuana users 1 week before and 4 weeks after smoking, is homogenized in hexane + 2-propanol, centrifuged, and the supernatant mixed with Lipidex 5000. The solvent is evaporated and the dried gel is packed in a glass column. Δ1 -THC is eluted from the column with methanol + water + acetic acid, diluted with water and the eluent is passed through a bed of Octadecylsilanebonded silica. After washing and drying, the retained Δ1-THC is eluted with hexane, derivatized with N-methyl-N-(t-butyl-dimethysilyl)trifluoroacetamide (MTBSTFA) and finally purified by HPLC on an Octadecyl SI 100 column in methanol. The amount of Δ1-THC is determined by GC/MS, using selected ion monitoring, and a deuterated internal standard. The recovery of Δ1-THC is about 80%, and the concentration of Δ1-THC in the fat samples analysed ranged between 0.4 and 193 ng/g wet tissue.
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  • 36
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    High-performance liquid chromatography/chemiluminescence determination of biological thiols with n-[4-(6-dimethylamino-2-benzofuranyl)phenyl]maleimide (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 39-42 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The peroxyoxalate chemiluminescence detection of biological thiols combined with high-performance liquid chromatography (HPLC) is described. SH groups of the thiol compounds including glutathione (GSH), cysteine, N-acetylcysteine, cysteamine, and D-penicillamine were labelled with N-[4-(6-dimethylamino-2-benzofuranyl)phenyl]maleimide (DBPM), a specific fluorogenic reagent for SH group. The labelling reaction was carried out at 60°C for 30 min and at pH 8.5 and a sample of the resulting reaction mixture was subjected to HPLC. Five kinds of labelled thiols were separated within 12 min on ODS-80 column (150 × 4.6mm ID; 5 μm) and detected in the ranges from 500 fmol to 2 pmol/100 μL (cysteamine and N-acetylcysteine), to 3 pmol/100 μL (cysteine) and to 5 pmol/100 μL (GSH and D-penicillamine). The lower detection limits were from 7 fmol (cysteamine) to 113 fmol (GSH) per 100 μL (S/N = 2). The method was applied to the determination of thiols in a rat liver. The amounts of glutathione and cysteine were 1.23±0.15 μmol/g (n = 5) and 0.15±0.04 μmol/g (n = 5), respectively.
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  • 37
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    Masthead (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989) 
    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.1130030201
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  • 38
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    Determination of catechol-O-methyltransferase activity in erythrocytes by high performance liquid chromatography with electrochemical detection (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 64-67 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A rapid assay employing HPLC with electrochemical detection for catechol-O-methyltransferase (COMT) activity in red blood cells is described. Enzyme activity is determined from erythrocyte lysates using S-adenosyl-L-methionine as methyl donor and 3,4-dihydroxybenzoic acid as substrate. The 3-O- and 4-O-methylated reaction products are measured by high-performance liquid chromatography with electrochemical detection. Human erythrocyte soluble form of COMT had Km values of 6.1 μM and 26.0 μM for S-adenosyl-L-methionine and dihydroxybenzoic acid, respectively. The mean O-methylation ratio for the soluble form of COMT was 5.3. An O-methylation ratio of 15.5 was estimated in the membrane fraction of an erythrocyte pool from three samples. The activities of soluble COMT in erythrocytes of some animal species are also reported. The procedure is easily automated, and a large number of samples can be processed during one working day.
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    URL: http://dx.doi.org/10.1002/bmc.1130030205
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  • 39
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    HPLC separation and characterization of chlorin derivatives with intact ring V from acid degradation products of silkworm excrement crude chlorophyll mixture (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 72-74 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A reversed-phase HPLC system with 88% methanol in 1 M ammonium acetate buffer pH 5.35 as the mobile phase on an ODS column was used to analyse pheophorbides a, a', b, b' and pyropheophorbides a and b. Pyropheophorbides a and b were found in samples obtained from silkworm excrement but not from spinach leaves though the preparation methods used were the same. This difference suggests that chlorophylls undergo metabolism in the body of silkworm to give pyrochlorophyll derivatives.
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  • 40
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    Rapid purification of detergent-solubilized bovine hormone-sensitive lipase by high performance hydrophobic interaction chromatography (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 82-87 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Hormone-sensitive lipase (HSL), the enzyme controlling the rate of adipose tissue lipolysis and also possibly involved in the regulation of steroidogenesis, has been purified from bovine omental adipose tissue. Partially detergent-solubilized, delipidated and purified HSL was obtained through step-elution at conventional DEAE ion-exchange chromatography, followed by concentration on hydroxylapatite. High performance hydrophobic interaction chromatography (HPHIC) on phenylsilica then resulted in an increase of HSL protein purity from 2% to more than 70%. Final purification of the enzyme to apparent homogeneity (〉95% protein purity), concentration and removal of most of the detergent was obtained by high performance cation exchange chromatography on Mono S. At least 0.5 mg of highly stable HSL was obtained from 5 kg of bovine omental fat within four working days. The purified lipase had a lower specific activity than previously reported for the corresponding rat enzyme but the preparations have proved very useful for enzyme structure studies and as an antigen.
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    Calendar of events (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), 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.1130030311
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    Thin layer chromatography of peptides and proteins: A review (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 95-104 
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    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 3 Ill.
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    Rapid assay of β-galactosidase and sialyltransferase by lectin affinity high performance liquid chromatography with fluorescence detectionThis study was entrusted to the Hohen Oil Company Ltd, by the Science and Technology Agency (STA) using the Special Coordination Funds for Promoting Science and Technology. (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 110-113 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Fluorescein isothiocyanate (FITC)-labelled asialotransferrin and pyridyl aminated oligosaccharides were prepared from asialotransferrin and human milk using affinity chromatography and high performance liquid chromatography (HPLC), respectively. These substances were incubated with galactosidase or sialyltransferase and then examined by lectin affinity HPLC. The elution patterns changed according to the period of incubation and amount of enzyme. This analytical method using lectin affinity HPLC with fluorescence labelled glycoprotein or oligosaccharides as the substrates has great value for detecting these enzyme under the same chromatographic conditions. In addition, differences were noted in the activity of β-galactosidase toward oligosaccharides having the Gal β(1 → 3)GlcNAc or Gal β(1 → 4)GlcNAc structure at reducing termini.
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    Lactoferrin from human breast milk and from neutrophil granulocytes. Comparative studies of isolation, quantitation, characterization and iron binding properties (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 121-126 
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    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The isolation and properties of lactoferrin from human breast milk and from neutrophilic granulocytes were investigated. Human breast milk lactoferrin was purified by means of heparin-sepharose or Cibacron Blue affinity chromatography. Quantitative recovery using these two methods was comparable but Cibacron Blue affinity chromatography allowed for isolation of a more homogenous protein. Lactoferrin could only be isolated from human neutrophilic granulocytes by sequential use of antibody affinity followed by non-specific affinity chromatography. Both breast milk lactoferrin and granulocyte lactoferrin were separated into apo and iron-rich species by SDS polyacrylamide gel chromatography. Iron binding is accompanied by a conformational change in tertiary structure associated with more rapid electrophoretic migration. The isoelectric point of both human breast milk lactoferrin and human granulocyte lactoferrin is 5.5 - 6.2. Both types of lactoferrin have similar iron binding properties with release of iron from the one binding site occurring at pH 5.2 - 6.0 while the other binding site holds on to iron down to pH 3.6 - 3.2. Despite the high affinity for iron the percentage saturation of native lactoferrin is low, that for breast milk lactoferrin averaging 12 - 25% and that for granulocyte lactoferrin 〈 10%.
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    Evidence for the overestimation of molecular masses of proteins after chemical modification and chemical crosslinks on sodium dodecyl sulfate/polyacrylamide gel electrophoresis (SDS-PAGE)This work is the partial fulfilment of the Exchange programs between French Medical Research Council (French INSERM) and Academia Sinica (University of Nanjing). Grants No. CS-RN-739, HN-CP-1.045, and CS-RN-842 during the years of 1984, 1986, 1987 and 1989 for the tenure of four 3 months trips to China by Dr Kia-Ki Han.This work is the partial fulfilment of the short visit of Prof. De-Xu Zhu to Lille, France during the month of September 1988 via French Association Recherche sur le Cancer's Channel (ARC Grant No. 6.715 to Dr Kia-Ki Han). (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 131-135 
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    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Human trypsin inhibitor (home prepared), lactalbumin, trypsinogen, carbonic anhydrase, and bovine serum albumin were submitted to succinylation and their molecular masses were determined by SDS-PAGE according to the method of Weber and Osborn (1969 J. Biol. Chem. 244, 4406) before and after chemical modification. High estimates of their molecular masses were obtained. The monomer and dimer of arrowhead inhibitor proteinase-B (Chinese vegetable legume) obtained after chemical crosslink(s) were also submitted to SDS-PAGE and their apparent molecular masses were also determined and compared to the native arrowhead inhibitor proteinase-B. Abnormally high estimates of their molecular masses were obtained. Our results agree with those in the literature.
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  • 46
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    Masthead (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989) 
    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.1130030301
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  • 47
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    Determination of urinary 5-hydroxy-3-indoleacetic acid by an automated HPLC method (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 114-117 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A HPLC method for the quantitative determination of 5-hydroxy-3-indoleacetic acid (5-HIAA) in urine is described. The method is based on ion-pair chromatography, reversed phase (RP) column material and specific fluorimetric detection at 300 nm and 355 nm. Sample preparation and gradient elution were avoided by using a column-switching technique. The sensitivity of the assay was excellent for clinical routine analysis, with a detection limit of 0.2 mg/L 5-HIAA. No endogenous or exogenous interference problems arose. Intra- and interassay precision was good, with observed coefficients of variation of 1.5 to 2.6% and 2.1%, respectively. Recoveries were 93 to 98%. The system described can be used for clinical diagnosis and therapy follow-up of carcinoid tumors. It has been running for over a year without disturbances and with a minimum of technical attendance.
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  • 48
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    Purification of rat liver soluble catechol-O-methyltransferase by high performance liquid chromatography (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 127-130 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The soluble form of catechol-O-methyltransferase (EC 2.1.1.6.) from rat liver was purified to homogeneity by high-performance anion-exchange chromatography and high-performance gel-filtration chromatography. The specific activity of the final pool was 270 U/mg protein. The purification was 1180-fold and recovery of the enzyme activity was 15%. During this rapid and gentle purification there were no problems with loss of activity, and the estimated half life of the final purified enzyme pool was 5.5 days at +4°C. The only additive used was phenylmethylsulfonylfluoride in the homogenizing buffer.
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    URL: http://dx.doi.org/10.1002/bmc.1130030308
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    High performance liquid chromatographic analysis of time-dependent changes in urinary excretion of indoleamines following tryptophan administration (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 157-160 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Analytical conditions of prepurification extraction and HPLC separation were optimized for determination of urinary serotonin and tryptamine. Under optimal conditions, serotonin, tryptamine and an internal standard were extracted with 15% v/v n-propanol in diethyl ether from urine samples alkalized with a phosphate buffer (0.75 mol/L, pH 10.0), and then they were re-extracted into an HCI solution (0.1 mol/L). Purified indoleamines were simultaneously separated by reversed-phase ion-pair HPLC with native fluorescence detection. Urinary serotonin and tryptamine were selectively determined within about 45 min per sample for the whole procedure. Analytical recovery, reproducibility and detection sensitivity were satisfactory for pursuing time-dependent changes in indoleamine levels. Urinary excretion profiles of serotonin and tryptamine in subjects dosed with L-tryptophan were successfully analyzed by our method.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130030404
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  • 50
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    Masthead (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989) 
    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.1130030601
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  • 51
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    Reversed phase high performance liquid chromatography of glycopeptides (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 241-245 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A practical procedure for isolating and purifying glycopeptides is described, viz. enzymatic hydrolysis - gel permeation chromatography - ion exchange chromatography - reversed phase HPLC. Using this procedure 28 glycopeptides from hen ovalbumin have been isolated some of which hitherto have not been identified. Water was a suitable mobile phase for preparing pure glycopeptides, and control of column temperature was important for good separations and reproducible retention times. Structural confirmation was by fast atom bombardment mass spectrometry.
    Additional Material: 4 Ill.
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  • 52
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    A rapid method for isolation of human hemoglobin benzo[a]pyrene diol epoxide derived adducts using high performance liquid chromatography (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 266-268 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A method is described to isolate rapidly human hemoglobin-benzo[a]pyrene diol epoxide adducts. A combination of 300 Å pore size C4 reversed phase HPLC to effect separation of adducted protein from native protein, and μ-bore C18 reversed phase HPLC to isolate and partially characterize proteolytic peptide adducts (by UV), was used.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130030608
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  • 53
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    Quantitative determination of itazigrel in rodent diet by reversed-phase HPLC and evaluation of its stability at 20°C (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 180-182 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple, accurate and precise procedure for the quantitation of itazigrel (a potent lipophilic inhibitor of collagen and arachidonic acid-induced aggregation being studied for its effects on peripheral vascular disease) from granulated rodent diet is presented. The drug was extracted from rodent diet using methanol + water (80:20) following dissolution of the diet in water. Samples of the supernatant were injected into the HPLC and the eluent was monitored with a fluorescent detector (λex = 320 and λem = 430) to achieve analytical specificity. Interday coefficients of variation of the calibration curve slope were ±6% on standards between 0 and 1000 μg/g. Potency and homogeneity of the drug spiked diet prepared over a 1 year interval at 70,200 and 600 μg/g was 99.3 ± 2.5%, 100 ± 1.8%, and 101 ± 1.9% of label, respectively. Samples prepared for chromatography were stable for 24 h at 20°C, and drug in diet was stable for 102 days when protected from light and stored at 20°C.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130030409
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  • 54
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    Calendar of events (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), 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.1130030412
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  • 55
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    A high performance liquid chromatography/electrochemical assay for glutamatergic neurotransmitters in the rat brain (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 183-185 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The release and content of the excitatory amino acid neurotransmitters glutamate and aspartate in rat striatum were determined by liquid chromatography/electrochemistry. This determination was based on precolumn off-line derivatization of the amino acids with o-phthaldialdehyde and 2-mercaptoethanol (OPT/2-MCE), and the adducts formed were separated under isocratic conditions and oxidized on a glassy carbon electrode at moderate potential (+0.6 V). The standard and the extracted glutamate when derivatized with OPT/2-MCE produced similar electrochemical and chromatographic characteristics. The detection limit of glutamate was 0.5 pmol. Depolarization induced by the high potassium medium (40 mmol/L) enhanced the release of glutamate and aspartate from superfused rat striatum, whereas the efflux of glutamine remained unchanged. Perfusion (for 60 - 70 min) removed 50 - 80% of the free amino acid content of striatal tissue. The method described here is useful in neurochemical investigations of the brain amino acid neurotransmitters.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130030410
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  • 56
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    High performance liquid chromatography determination of cyanide in urine by pre-column fluorescence derivatization (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 209-212 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A method for the determination of cyanide in human urine has been developed. The method is based on the reaction of cyanide with 2,3-naphthalenedialdehyde and taurine to give a fluorescent product for reversed-phase HPLC separation and fluorometric detection. After centrifugation followed by dilution of urine samples, the specimens could be analysed directly by this method. The recovery of cyanide added to urine at concentration levels of 50 - 1000 pmol/mL was 85 - 96%. The detection limit of cyanide was 30 pmol/mL in urine. The method was successfully applied to the analysis of urine from smokers and nonsmokers. The mean concentrations of cyanide were found to be 215 pmol/mL for the former and 84 pmol/mL for the latter.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130030507
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  • 57
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    Calendar of events (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), 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.1130030512
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  • 58
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    Solid phase extraction for an improved assay of physostigmine in biological fluids (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 226-232 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple, selective and very sensitive assay is described for the quantification of physostigmine in blood, plasma and urine. The most appropriate solid phase column was selected after a systematic investigation of nine types of phase. The conditions for solid phase extraction were optimized using [3H]physostigmine so that the overall recoveries were 〉90%. Physostigmine was retained on alkaline treated cyanopropyl columns and eluted into the minimum volume of methanol, obviating the need for an evaporation step. Extracted samples were quantified by HPLC with a three electrode coulometric detection system. The limit of detection was 50 pg/mL for a 0.5 mL plasma sample. The precision (CV) for 0.5 mL plasma samples containing 50 pg was 8.1%. Application of the method to plasma, blood and urine samples is presented.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130030511
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  • 59
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    Identification by gas chromatography/mass spectrometry of long-chain fatty acids and alcohols from hamster meibomian glands using picolinyl and nicotinate derivatives (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 251-254 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Meibomian secretions from the hamster were hydrolysed with base and examined as TMS, [2H9]TMS, methyl ester/TMS, picolinyl ester/TMS and nicotinate/TMS derivatives by capillary GC/MS. Over 90 compounds, representing over 89% of the hydrolysed fraction, were identified. Fatty acids with chain lengths from 10 to 32 carbon atoms were found, the most common of these were in the C15 to C18 and in the C25 to C30 regions. Chain types were predominantly iso or anteiso branched, mono-unsaturated (C16 and C18) and straight. Fatty alcohols were mainly from the iso or anteiso series and tended to have longer chain lengths; the major alcohols had anteiso-25 and 27 and iso-26-chains. In these respects the secretions were similar to those reported earlier from other species, although fewer mono-unsaturated compounds with longer chains (C20 to C30 region) were found than in the rat and human. The steroid fraction was characterized by a larger number of compounds than normally present in secretions of this type. The major compound was cholesterol, in common with that in all other examined species except the rabbit.
    Additional Material: 3 Ill.
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  • 60
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    High resolution chromatography of ribonucleosides and its application to RNA analysisAbbreviations used. ψ, pseudouridine; D, 5,6-dihydrouridine; m3C, 3-methylcytidine; m1A, 1-methyladenosine; m5C, 5-methylcytidine; m7G, 7-methylguanosine; Cm, 2′-O-methylcytidine; I, inosine; rT, ribothymidine; Um, 2′-O-methyluridine; m1I, 1-methylinosine; m1G, 1-methylguanosine; m2G, 2-N-methylguanosine; m22G, 2-N,N-dimethylguanosine; m6A, 6-N-methyladenosine; Am, 2′-O-methyladenosine; Gm, 2′-O-methylguanosine; Y, a-amino-b-hydroxy-4,9-dihydro-4,6-dimethyl-9-oxo-1-H-imidazole-1,2-a-purine-7-butylic acid; pG, guanosine 5′-phosphate; Gp, guanosine 3′-phosphate; pGp, guanosine 3′,5′-diphosphate. In abbreviations for oligonucleotides, phosphates between nucleosides are excluded, e.g., AGCUp is ApGpCpUp. (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 246-250 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple and precise method was developed for the separation of nucleosides including modified nucleosides and oligonucleotides. Nineteen kinds of nucleosides were completely separated by HPLC using an ODS column (TSK-gel ODS 80TM) and aqueous mobile phases. The RNA molecule was digested by base restrictive RNase (RNase A, RNase T1) and the digests were separated chromatographically into each oligonucleotide. The nucleoside composition of an oligonucleotide was then determined by this analytical system. It is thus possible to fit the oligonucleotide in the original RNA molecule by using modified bases as markers. The reaction site of quinacrine mustard for tRNAPhe (from yeast) could be determined by this analytical system.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130030604
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    Simultaneous analysis of furosemide and bumetanide in horse plasma using high performance liquid chromatography (1989)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 3 (1989), S. 262-265 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A high performance liquid chromatographic method is described for the simultaneous determination of furosemide and bumetanide in horse plasma. The C8 (3 μm) reversed phase column (4.8 × 150 mm) provided clear separation of furosemide and bumetanide with other components present in the horse plasma. The detection limit for both the drugs was 10 ng/mL. Both drugs were stable in plasma (at natural or acidic pH) for up to 24 h. The method is sufficiently sensitive to detect furosemide levels in plasma obtained from horses receiving a therapeutic dose of furosemide.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130030607
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  • 62
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    Multicomponent determinations by a membrane-discriminated gas phase analyzer and successive regression in the fiduciary region (1989)
    New York, NY : Wiley-Blackwell
    Journal of Chemometrics 3 (1989), S. 601-608 
    Details
    ISSN: 0886-9383
    Keywords: Gas phase flow injection analysis ; Membrane-differentiated analysis ; Multicomponent determinations ; Successive linear regression ; Successive regression in fiduciary region ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A membrane-discriminated gas phase analyzer is proposed for multicomponent determinations. Nitrogen gas flows countercurrent through outer and inner channels in a tube-in-tube arrangement. The only communication between the two channels occurs through a 500 μm aperture covered by a porous PTFE membrane. A mixture of organic compounds (up to four components) is injected into the inner channel by a heated backflushed injector and the sample components diffusing into the outer channel are monitored by a flame ionization detector (FID). A calibration set, consisting of pure components, binary, ternary and quaternary mixtures (a total of 64 samples), provides the known data base: temporal profiles of the FID output as a function of sample composition. Although the overall response behavior is not a linearly additive function of individual analyte concentrations, the use of successive inverse multiple linear regression (while continually altering the choice of the calibration samples considered for the forward regression, on the basis of the most recent values of the predicted unknown sample composition) is shown to yield analytical results for unknown samples that are in good agreement with their true values.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cem.1180030408
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    Product news (1989)
    New York, NY : Wiley-Blackwell
    Journal of Chemometrics 3 (1989), S. 609-609 
    Details
    ISSN: 0886-9383
    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/cem.1180030409
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  • 64
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    Measurement of mevalonate in human plasma and urine by multiple selected ion monitoring (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 174-176 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Plasma levels and urinary excretion of mevalonate were reported to be correlated with cholesterol biosynthesis. Evaluation of mevalonate concentration in plasma and urine represents therefore a non-invasive method for studying the modifications of cholesterol synthesis. A method is described here by wich mevalonate in plasma and urine is determined by the selected ion monitoring technique after extraction as mevalonolactone and conversion into the trimethylsilyl ether. Linear responses were obtained in the evaluation of mevalonate added to plasma in the 10-100 ng/ml (r 〉 0.995) and to urine in the 50-1000 ng/ml concentration ranges, respectively. Identity of mevalonate in plasma and urine was confirmed by high-resolution mass spectrometry.
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    URL: http://dx.doi.org/10.1002/bms.1200180305
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    Fast atom bombardment of metal-pyochelin complexes: Metastable analysis at constant B/E of zinc-pyochelinMention of a trade name, proprietary product, or specific equipment does not constitute a guarantee or warranty by the US Department of Agriculture and does not imply its approval to the exclusion of other products that may be suitable. (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 185-191 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fast atom bombardment (FAB) mass spectrometry was used to characterize the pyochelin complexes of iron and zinc. Ferripyochelin readily forms the [M + H]+ and [2M + H]+ ions in a glycerol matrix. The molecular ion was 2.5 fold more abundant when acetic acid was present. Iron was shown to be present in the iron-pyochelin complex as the ferric ion by wet chemical methods. Differentiation between ferric and ferrous ions by FAB was not successful owing to the FAB reducing environment. Ferric ions were reduced by FAB to ferrous ions in the following model salts - ferric chloride, ferric nitrate and ferric sulfate - when dissolved in either glycerol, thioglycerol or the magic bullet matrix. Ferric and ferrous chloride salts gave virtually identical spectra with a glycerol/acetic acid matrix. Zinc-pyochelin readily forms the [M + H]+ and [2M + H]+ ions, but only when acetic acid was present in the glycerol matrix. The FAB mass spectrum of zinc-pyochelin exhibited various fragmentations which can be used in structural analysis. Linked-scan at constant B/E and accurate mass data were used to characterize the fragmentations of the zinc-pyochelin complex. Metastable analysis allowed the fragmentation pathway of zinc-pyochelin to be determined.
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    URL: http://dx.doi.org/10.1002/bms.1200180307
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    Electron impact mass spectrometry of BHT and its alteration products (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 207-217 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The electron impact (EI) mass spectra of 2,6-di-tert-butyl-4-methylphenol (BHT) and certain of its alteration products are described in detail. Accurate mass measurements confirm the elemental compositions of important fragment ions in the EI spectra. Collisionally activated mass spectra are also used to study fragmentation and suggest common ion structures. The reference spectra provide the basis for identifying various alteration products of BHT by capillary gas chromatography/mass spectrometry (GC/MS) without the necessity of isolating individual components. Application of GC/MS is made to three studies: (i) pyrolysis of hydroperoxy-BHT as a potential pathway to alteration products in food; (ii) GC/MS pyrolysis of hydroperoxy-BHT as a model study; and (iii) alteration of BHT in ethanol/water as a food-simulating solvent.
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    URL: http://dx.doi.org/10.1002/bms.1200180310
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    Fast atom bombardment mass spectrometry of the D-aldohexoses and some deoxyaldohexoses (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 363-372 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The MI and CA spectra of selected positive and negative ions generated by fast atom bombardment (FAB) of the stereoisomeric aldohexoses can be used to differentiate among these isomers, without prior derivatization or addition of other substances. The main fragmentation routes were traced and compared to those of some 2- and 6-deoxyaldohexoses, which appeared to be suitable model compounds. In both positive and negative ion FAB mass spectrometry, the OH group at the C-2 position plays an important role in the fragmentation reactions of the pseudomolecular [M + glycerol + H]+ and [M - H]- ions.
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    Rapid identification of calbindin-D28k cyanogen bromide peptide fragments by plasma desorption mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 387-393 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Chicken intestinal calbindin-D28k is an intracellular protein which is believed to have a fundamental role in vitamin D-mediated transport of calcium. A mapping approach based on 252Cf plasma desorption mass spectrometry (PD mapping) was used to screen the DNA-deduced sequence of calbindin-D28k for sequence changes and posttranslational modifications. In the PD mapping experiment, purified calbindin-D28k was cleaved with cyanogen bromide and the resulting peptides were subjected to PD mass spectrometric analysis either as a mixture or as high-performance liquid chromatography isolated fractions. The DNA-derived primary structure of calbindin-D28k was confirmed by rapid PD mass spectral identification of the CNBr peptide fragments, and the nature of the N-terminal blocking group was readily determined to be an acetyl group. The relatively non-destructive nature of the PD mass spectrometric analysis allowed the mapping of the N-terminal peptide through an additional in situ V8 protease enzymatic reaction.
    Additional Material: 6 Ill.
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    Rapid determination of sequence variations in actinidin isolated from Actinidia chinensis (var. Hayward) using fast atom bombardment mapping mass spectrometry and gas phase microsequencing (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 424-428 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A current limitation in the use of fast atom bombardment (FAB) mass spectrometric mapping of peptide mixtures, derived from enzymic digestion of proteins, is that most of the hydrophilic peptides are not observed. However, it has been demonstrated from previous work that esterification of the peptide mixture results in the detection of almost all peptides in FAB mass spectrometry. This strategy of FAB mapping was applied to the protein actinidin, isolated from an Italian variety of Actinidia chinensis. Two of the 12 tryptic peptides in FAB mass spectrometry did not exhibit molecular ions predicted from the known sequence of actinidin isolated from the New Zealand variety of A. chinensis. The two peptides were isolated by high-performance liquid chromatography, subjected to Staphylococcus aureus V8 protease digestion and sequenced by gas-phase microsequencing. Nine changes in amino acid composition were detected using the rapid and powerful combination of FAB mass spectrometric mapping and gas-phase microsequencing.
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    URL: http://dx.doi.org/10.1002/bms.1200180611
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    Studies on anabolic steroids II - gas chromatographic/mass spectrometric characterization of oxandrolone urinary metabolites in manFor Part I see Ref. 1. (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 429-438 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The metabolism of 17α-methyl-17β-hydroxy-2-oxa-5α-androstan-3-one (oxandrolone) in man has been investigated by gas chromatography/mass spectrometry. After oral administration of a 10 mg dose to man, five metabolites were detected in the free fraction of the urinary samples. Oxandrolone, the major compound excreted in urine, was detected within 72 h after administration. During this period 35.8 and 8.4% of the administered dose was excreted as unchanged oxandrolone and 17-epioxandrolone, respectively. In addition, minute amounts of 16α- and 16β- hydroxyoxandrolone and a δ-hydroxy acid resulting from the hydrolysis of the lactone group of oxandrolone were detected in the urine samples 8-60 h after administration. Furthermore, the susceptibility of oxandrolone to hydrolysis was investigated under several pH conditions. Extraction and fractionation of steroidal metabolites was achieved by using C18 and silica Sep Pak™ chromatography. The mass spectra of the metabolites are presented and major fragmentation pathways discussed.
    Additional Material: 10 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180612
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    Gas chromatographic and gas chromatographic/tandem mass spectrometric characterization of precursors on the sesterterpene pathway for steroid biosynthesis (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 572-575 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An increasing amount of evidence is accumulating to support the proposal that steroidogenesis can occur by a sesterterpene pathway as well as the cholesterol pathway. Key intermediates on the sesterterpene pathway are 23,24-dinor-5-cholen-3β-ol (guneribol) and some of its metabolites, e.g. 23,24-dinor-4-cholen-3-one (guneribone). It has been reported that these intermediates are biosynthesized and converted to steroid hormones by a range of endocrine tissues in vitro. Monitoring the pentafluorobenzyloxime derivatives by negative ion chemical ionization mass spectrometry in the electron capture mode provided evidence for the presence of guneribone in extracts of bovine testicular and human adrenal tumour tissue. Complementary evidence was obtained from gas chromatographic/tandem mass spectrometric data generated on a triple-quadrupole instrument by monitoring daughter ions (in the multiple ion detection, MID mode) of the molecular anion of derivatized guneribone in both standards and tissue extracts. The present findings that sesterterpene pathway intermediates are present as endogenous compounds in tissue extracts, together with the previously reported radiochemical data, give further support to the sesterterpene pathway hypothesis.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180811
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    Determination of cyclic butylboronate esters of some 1,2- and 2,3-diols in plasma by high-resolution gas chromatography/mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 592-597 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A gas chromatographic/mass spectrometric analytical procedure is described to determine glycols in plasma as cyclic butyl boronate esters. The method, involving a pre-deproteinization step, required only 0.25 ml of plasma and a short time (20 min) to react with the derivatizing agent (butyl boronic acid). The gas chromatographic separation on a CP Sil 8 CB silica capillary column coupled to a mass detector assured a complete identification of the compounds. The analytical recoveries (〉95%) with low coefficient of variation (4-11%) assured the feasibility of the method over a concentration range from 5 to 1000 μg ml-1 for each glycol. The lower detection limits, namely 1-5 μg ml-1, confirmed the sensitivity of the method.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180814
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    Isotope labelling of lipids using the Favorsky rearrangement (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 603-612 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis of tetradeuterated 10-methylundecanoic acid, dideuterated tetracos-2-enoic acid, (1-14C)pristanic acid and (1-14C)tetracos-2-enoic acid using the Favorsky rearrangement are described. They will be used for studies of long-chain fatty acid metabolism in patients. The positions of isotope labelling were determined by mass spectrometry.
    Additional Material: 12 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180816
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  • 74
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    Structure analysis of modified oligodeoxyribonucleotides by negative ion fast atom bombardment mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 617-619 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Negative ion fast atom bombardment mass spectrometry is used to verify the sequence of oligodeoxyribonucleotides containing a single modified nucleotide. Both the position in the sequence and the molecular weight of the modified nucleotide can be determined from the 3′ and 5′-phosphate sequence ions which are prominent in the mass spectrum.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180818
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    A comparison of positive ion and negative ion fast atom bombardment mass spectral data for some sulphonyl hydrazones and derivatives (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 620-623 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A number of sulphonyl hydrazones and derivatives have been synthesized and tested for biological activity as pesticides during the crop protection research programme at the Hatfield Polytechnic. A recent comparative ionization study of some of these compounds using electron impact (EI), fast atom bombardment (FAB) and various chemical ionization methods showed FAB mass spectrometry to be the optimum technique to use in terms of molecular weight information obtained. This study compares the FAB mass spectral data in positive and negative ion mode using an alternating positive and negative ion detection system.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180819
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    Rapid structural analysis of the in vitro and in vivo metabolism of SK&F 95448 by the combined use of thermospray liquid chromatography/mass spectrometry and liquid chromatography/tandem mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 637-644 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The thermospray liquid chromatography/mass spectrometry (LC/MS) interface has had a major impact on the direct analysis of the metabolic fate of xenobiotics in complex biological media. This paper outlines the rapidity and power of the LC/MS approach, and shows how detailed structural information can be obtained without recourse to individual compound isolation. This provides a great saving in time and effort. The additional specificity of liquid chromatography/tandem mass spectrometry is highlighted in identifying the sites of metabolic transformation. The ability to handle biological samples with little or no clean-up using wide high-performance liquid chromatographic gradients is a key feature of the success of this methodology.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180822
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    Phytochemical studies on the essential oils of species belonging to the Achillea genus by gas chromatography/mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 629-636 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Several populations of Achillea species were collected from Hungarian localities. The characteristic composition cf the essential oils of almost 220 populations were determined by gas chromatography/mass spectrometry. The main component of Achillea asplenifolia, A. setacea and A. collina oils is chamazulene, with a molecular mass of 184. The composition of some A. setacea is different: instead of chamazulene it contains a significant amount of farnesene. Oils of A. distans, A. crithmifolia, A. nobilis, A. pannonica and A. ochroleuca contain some different and specific compounds instead of chamazulene. During the analysis of many essential oils, we found some very interesting differences within species originating from another geographical area.
    Additional Material: 13 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180821
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    Quantification of urinary 3-hydroxyisovaleric acid using deuterated 3-hydroxyisovaleric acid as internal standard (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 652-656 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Deficiency of biotin at the tissue level can be assessed indirectly by measuring the urinary excretion of 3-hydroxyisovaleric acid. This paper describes the application of an improved method of quantifying urinary 3-hydroxyisovaleric acid using unlabeled and uniformly deuterated 3-hydroxyisovaleric acid. These compounds were synthesized by a modification of the lithioacetic acid method for generation of beta-hydroxy acids. Elemental analysis, nuclear magnetic resonance, gas chromatographic and gas chromatographic/mass spectrometric data demonstrated that the compounds are greater than 95% pure. Mass spectrometry confirmed the identity of the unlabeled compound, demonstrated that the deuterated compound is uniformly labeled, and offered insight into the pattern of mass fragmentation. The method for determination of the concentration of 3-hydroxyisovaleric acid in rat urine uses gas chromatographic/mass spectrometric quantification of the di-trimethylsilyl derivative with the deuterated compound as the internal standard. Results provide evidence that this method is more accurate than a previously published method that did not utilize the unlabeled and deuterated standards.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180903
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    Metabolic dissimilarity between (9,12,12-2H)cortisol and natural cortisol in vivo. Can deuterated cortisol be used for the measurement of the urinary cortisol production rate? (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 662-667 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The metabolism of deutrated cortisol (9,12,12,-2H)cortisol, (2H3-F) was compared to that of radioactive cortisol (3H2-F) and natural cortisol, when these three compounds were administered simultaneously to an adrenalectomized piglet. The relative isotope dilution of tritium was determined from the specific activities of the main urinary neutral cortisol metabolites, tetrahydrocortisone (THE) and tetrahydrocortisol (THF), normalized to that of the cortisol mixture administered. To obtain a comparison of the isotope dilution of deuterium in the metabolites THE and THF to that in the cortisol mixture, the three steroids were converted to the common oxidation product 11-oxo-aetiocholanolone, and deivatized to the methoxime-tert-butyl-dimethylsilyl ether. The relative 2H-isotope dilution then was measured by gas chromatography/mass spectrometry. It was found that the specific activity of THE in the cumulative urine collections was similar to that of the cortisol mixture administered; the two-day value was, however, less. The specific activity of THF was slightly but significantly smaller than 1 (∼0.9) at all times. The relative 2H-isotope dilution in THE was slightly but significantly larger than one (∼1.1) at all times, whereas that in the THF was larger than 1.0 at 9 and 32 h or equal to 1.0 at 20 and 47 h of urine collection. When comparing the metabolism of the two tracer cortisol species the quotient of the 3H- and the 2H-isotope dilutions in THE and THF was smaller than 1.0. It can be concluded that (2H3)cortisol may be used for the determination of the cortisol production rate.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180905
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    Direct analysis of different classes of surfactants in raw materials and in finished detergent formulations by fast atom bombardment mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 673-689 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The characterization of the components of a surfactant mixture is a challenge, since we are dealing with substances inherently difficult to purify or separate by any available chromatographic methods. The results of the present work provide evidence that with fast atom bombardment mass spectrometry it is possible to identify the single constituents of the different clases of tensides - non-ionic, anionic, cationic and amphoteric - directly in the mixture and in detergent formulations (shampoos). The method, which is based on unambiguous molecular weight determination of the single components, allows the definition of the exact distribution of oligomers in the surfactant mixture, and distinction of subtle variations in the detergent composition in finished formulations. The results obtained indicate that this technique is a powerful analytical tool which can be used as a rapid screen test for quality control.
    Additional Material: 12 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180907
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    Biotransformation of aliphatic formamides: Metabolites of (±)-N-methyl-N-(1-methyl-3,3-diphenylpropyl) formamide in ratsPresented in part at the 35th ASMS Meeting, Denver, Colorado, May 1987. (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 690-701 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The in vivo biliary and urinary metabolites of (±)-N-methyl-N-(1-methyl-3,3-diphenylpropyl) formamide (1) from male Wistar rats have been characterized by gas chromatography/mass spectrometry. In urine, non-conjugated metabolites included 1,1-diphenyl-3-butanone (4) and 3-methylamino-1,1, diphenylbutane (7). β-Glucuronidase liberated 4, 1,1-diphenyl-3-butanol (5), 1,1-diphenyl-3-butanone oxime (6), N-hydroxymethyl-N-(1-methyl-3, 3-diphenylpropyl) formamide (3), 1-(4-hydroxyphenyl)-1-phenyl-3-butanone (11), 1-(4-hydroxyphenyl)-1-phenyl-3-butanone oxime (12), N-methyl-N-(1-methyl-3-(4-hydroxyphenyl)-3-phenylpropyl) formamide (8), 1-(4-hydroxy-3-methoxyphenyl)-1-phenyl-3-butanone (16), 1-(4-hydroxy-3-methoxyphenyl)-1-phenyl-3-butanol (17), 1-(4-hydroxy-3-methoxyphenyl)-1-phenyl-3-butanone oxime (18), N-(1-methyl-3-(4-hydroxy-3-methoxyphenyl)-3-phenylpropyl) formamide (14) and N-methyl-N-(1-methyl-3-(4-hydroxy-3-methoxyphenyl)-3-phenylpropyl) formamide (13). Most of the carbinolamide (3) decomposed in the gas chromatograph inlet to N-(1-methyl-3,3-diphenylpropyl) formamide (2) unless stabilized as a trimethylsilyl (TMS) derivative. In bile, compounds 1, 2, 3, 5, 6, 11, 12 and 16 were present as non-conjugated metabolites. β-Glucuronidase also liberated N-(1-methyl-3-(4-hydroxyphenyl)-3-phenylpropyl) formamide (9), and all of the previously listed compounds except 7. Trimethylsilylation of the conjugated bile fraction revealed the presence of an additional two compunds: N-hydroxymethyl-N-(1-methyl-3-(4-hydroxyphenyl)-3-phenylpropyl) formamide (10) and N-hydroxymethyl-N-(1-methyl-3-(4-hydroxy-3-methoxyphenyl)-3-phenylpropyl) formamide (15). A stable carbinolamide metabolite standard was synthesized and the mass spectral fragmentations of its TMS derivative studied by tandem mass spectroscopy. This is the first report on stable carbinolamide metabolites of high-molecular-weight formamides.
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    URL: http://dx.doi.org/10.1002/bms.1200180908
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    Parent ion spectroscopy in the identification of advanced glycation products (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 713-718 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Advanced glycation products have been investigated by parent ion spectroscopy, employing B2/E = constant linked scans of furoyl ions obtained from hydrolysed glycated albumin and polylysine mixtures, without any extraction procedures. Using such an instrumental approach, together with exact mass measurements and collision spectroscopy, the identification of 2-(2-furoyl)-4-hydroxyl-1H-imidazole and 2-(2-furoyl)-4-carboxy-1H-imidazole among the advanced glycation products has been achieved.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180911
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    Identification of long-chain fatty acids and alcohols from human cerumen by the use of picolinyl and nicotinate esters (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 719-723 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Human cerumen was hydrolysed with base and the constituents were examined as trimethylsilyl (TMS), methyl ester/TMS, picolinyl/TMS and nicotinate/TMS derivatives by gas chromatography and gas chromatography/mass spectrometry. A sample was also reacted with osmium tetroxide for double bond location. The major constituents were cholesterol, squalene and several series of long-chain fatty acids and alcohols. These latter compounds had chain lengths of 12-26 carbon atoms and were predominantly either straight-chain saturated or straight-chain unsaturated compounds. Saturated branched-chain acids with methyl groups predominantly on even-numbered carbon atoms were present but were less abundant. Unsaturated, branched-chain acids were also present. The major unsaturated acids contained unsaturation at the delta-6-position or were derived from these acids by chain elongation. The compounds were similar to those found in vernix caseosa. The mass spectra of picolinyl esters were, for the first time, shown to be capable of determining both the position of unsaturation and methyl branching in the same molecule.
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    URL: http://dx.doi.org/10.1002/bms.1200180912
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    Tandem mass spectrometry of leucine enkephalin and physalaemin using a hybrid instrument (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 727-732 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Daughter ion mass spectral data of [M + H]+ ions of leucine enkephalin and physalaemin, which were formed by fast atom bombardment, were obtained using an instrument of EBQQ configuration. In the case of leucine enkephalin, experiments were carried out in which the collision energy was varied and the collision gas pressure kept constant and vice versa. The results show that conditions can be established under which seuqence-relevant ions above m/z 200 are formed, as well as under which mainly immonium and acylium type ions are generated. Of possible interest for characterization of unknown peptides, when using hybrid instruments, are the mid-chain cleavage ions, which, at a constant argon gas pressure of 5 × 10-6 mbat, were found to maximize at around 30 eV collision energy. Daughter ion mass spectral data are also presented for [M + H]+ ions of physalaemin (mol. wt 1264). Compared to data obtained for physalaemin on multisector instruments, our results indicate that the formation of mid-chain cleavage ions is clearly enhanced.
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    URL: http://dx.doi.org/10.1002/bms.1200180914
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    Characterization of virus infected cell cultures by pyrolysis/direct chemical ionization mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 757-760 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The supernatants of Vero cell cultures after infection with a herpes simplex virus or a poliomyelitis virus as well as a blank were analysed by pyrolysis/direct chemical ionization mass spectrometry (Py/DCI MS). Informative pyrogrammes were obtained and used for characterization of viral proteins by applying pattern recognition methods. Differentiation of viral proteins was evaluated by analysing ‘blind’ samples. Herpes viruses could be classified correctly but the observed differences between the blank and the polio virus supernatants were too small for reliable classification of the polio viruses. Purification of the samples seems to be a prerequisite for further studies. The potential value of Py/DCI MS as a rapid non-invasive diagnostic method for viral meningoencephalitis is stressed.
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    URL: http://dx.doi.org/10.1002/bms.1200180919
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    Fast atom bombardment combined with tandem mass spectrometry for analysis of a complex mixture of lipo-oligopeptides from Nocardia rubra cell wallskeletonPart of the results in this paper have been presented at the 36th ASMS Conference on Mass Spectrometry and Allied Topics, San Francisco, USA, p. 1285 (1988). (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 761-766 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Experimental variables in fast atom bombardment combined with tandem mass spectrometry based on low-energy collision-induced dissociation have been systematically invetigated in order to optimize parameters for analysis of synthetic lipo-oligopeptides. The parameters studied were matrix, ion polarity, collision gas, collision gas pressure and collision energy. The optimal parameters recommended in this study have been applied to the N-terminal amino acid seuquence determination of lipopeptide obtained from Nocardia rubra cell wall skeleton. Daughter and parent ion experiments with negative ion fast atom bombardment combined with tandem mass spectrometry have proven to be very useful for structure elucidation of a complex mixture of lipo-oligopeptides.
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    URL: http://dx.doi.org/10.1002/bms.1200180920
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    The determination of atmospheric bis (chloromethyl) ether by gas chromatography/tandem mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 775-779 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The technique of gas chromatography/tandem mass spectrometry is applied to the analysis of bis(chloromethyl) ether in laboratory and production environments. A selected reaction monitoring method is shown to yield superior sensitivity and selectivity to previous methods. A detection limit of ∼1 ppt is established even for chemically complex atmospheres which have proved intractable by previous techniques.
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    URL: http://dx.doi.org/10.1002/bms.1200180922
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    Fast atom bombardment mass spectra of peptides. Dimer ion studies. Part VIPart V: see Ref. 1; Part IV: see ref. 2. (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 281-286 
    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 spectra of the opioid pentapeptides leucine enkephalin (1) (H-Tyr-Gly-Gly-Phe-Leu-OH or YGGFL), methionine enkephalin (2) (H-Tyr-Gly-Gly-Phe-Met-OH or YGGFM) and leucine enkephalin-2H2 (3) (H-Tyr-2Gly-2H2-Gly-Phe-Leu-OH or YGGFL-2H2) have been recorded in glycerol. The following experiments have been carried out: (i) dimer studies [2M + 1]+; (ii) decompositions of dimers: daughter ions from (YGGFL)2, (YGGFL-YGGFL-2H2) and (YGGFL-2H2)2 as well as (YGGFM-YGGFL) and (YGGFM)2 dimers; (iii) solvation site and pyridine collision-activated dissociation studies for dimer ions; (iv) mechanism of formation of [(2M + 1) - Gly4]+ ions.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180502
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    Practical considerations in the use of stable isotope labelled compounds as tracers in clinical studies (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 321-327 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Increasingly widespread usage of stable isotope tracers to aid clinical diagnosis and support basic research has stemmed from both advances in mass spectrometry and the availability of competitively priced labelled compounds. Stable isotopes have been used generally to investigate normal and abnormal metabolic pathways, to estimate energy expenditure and body composition and to quantitate substrate flux and oxidation rates. Despite the fact that the underlying principles relating to the use of stable isotopes for in vivo studies are straightforward, careful consideration must be given to all aspects of human studies. This review highlights some of these, including choice of label and tracer molecule, mode of tracer administration and sampling site, analytical instrumentation, interpretation of data and ethical constraints.
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    URL: http://dx.doi.org/10.1002/bms.1200180507
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  • 90
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    Masthead (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989) 
    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.1200180601
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  • 91
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    Forthcoming events (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 358-358 
    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.1200180512
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  • 92
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    Direct liquid inlet liquid chromatographic/mass spectrometric identification and high-performance liquid chromatographic analysis of a benzodiazepine glucuronide (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 359-362 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The glucuronide of N-1-hydroxy-ethyl flurazepam has been analysed by a direct liquid inlet liquid chromatographic/mass spectrometric system using MeOH/H2O (70:30 v/v) as mobile phase, at a flow rate of 0.7 ml min-1. Urine samples were purified by amberlite XAD-2 chromatography; the glucuronide was quantified by highperformance liquid chromatography using a counterion (tetrabutyl ammonium nitrate in methanol). Chromatographic results were validated by an enzymatic method: treatment of the samples with β-glucuronidase and extraction of the parent drug with ethyl ether at pH 9. The biological application of this method was demonstrated by determination of this glucuronide in the urine of healthy human volunteers following a single intravenous administration of 50 mg of N-1-hydroxy-ethyl flurazepam.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180602
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  • 93
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    Mass spectrometry of domoic acid, a marine neurotoxinNRCC No. 29369. (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 373-386 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Domoic acid is a naturally occurring amino acid, formerly available in limited amounts as a natural product of some algae of the family Rhodomelaceae. As the result of a recent incidence of toxicity in cultured blue mussels (Mytilus edulis) from a highly localized region of Atlantic Canada, useful amounts of this substance are likely to become available in the near future. Domoic acid is an important substance for fundamental studies in neurobiology as it possesses the highest affinity amongst known substances for the kainate receptors of the central nervous system. The present work describes fast atom bombardment (FAB) mass spectra of domoic acid, and of some of its isomers present in minor quantities in contaminated mussel extracts. These FAB spectra are subject to interferences from beam-inducced reduction reactions associated with matrices such as glycerol, but not with others such as 3-nitrobenzyl alcohol. Tandem mass spectrometry of the MH+ ions from these compounds is also reported. As a more feasible approach to quantitative analysis at trace levels, formation of the volatile tert-butyldimethylsilyl derivatives has been investigated and shown to be highly promising.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180604
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  • 94
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    Collisional activation mass spectra of M-. ions of azo dyes containing 2-naphthol (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 394-400 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Collisionally activated decomposition mass spectra of M-. ions of azo dyes are presented. The compounds are of general structure Ar(1)—N=N—Ar(2), where Ar(1) is substituted phenyl and Ar(2) is 2-naphthol. Characteristic fragment ions observed include m/z 157, which corresponds to the 2-naphthol substituent with cleavage of the —N=N— bond represented as [Ar(2) - N]-.. Ion of general structure [Ar(1)- NH]- are also observed. Parent ion scans of m/z 157 provide a potential screening technique for 2-naphthol-containing axo dyes. Specific results are reported for the chloroform extract of FD&C Red #8, and capillary gas chromatographic introduction is compared with direct exposure probe introduction for the identification of dyes.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180606
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  • 95
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    Studies on the biotransformation of ketamine. II - quantitative significance of the N-demethylation pathway in rats in vivo determined by a novel stable isotope technique (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 401-404 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In order to determine the fraction of an intravenous bolus dose of ketamine which is metabolized in vivo to the corresponding N-desmethyl compound, norketamine, a novel stable isotope technique was developed and applied to a study in rats. Co-injection of equimoiar amounts of deuterium-labeled ketamine and unlabeled norketamine to four animals, followed by gas chromatographic/mass spectrometric analysis of both the administered compounds and deuterium-labeled norketamine in plasma yielded pharmacokinetic data from which the fraction of the parent drug subjected to N-demethylation (fm) was calculated from AUC data to be 36.8 ± 2.4%. It is concluded that this stable isotope co-administration technique represents a powerful approach to the determination of fm, in that the pharmacokinetics of the metabolite of interest, given as the preformed compound and generated in vivo, are determined simultaneously. This experimental design thus obviates the influence of time-dependent changes in metabolite clearance which may complicate the interpretation of studies performed using the classical cross-over design.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180607
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  • 96
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    Profiles in altered metabolism. IV - induction of acute dicarboxylic aciduria following 2-octynoic acid administration to the ratPrevious paper in this series: ‘Profiles in Altered Metabolism III - (Ω-1)-Hydroxyacid Excretion in a Case of Episodic Hypoglycemia’, O. A. Mamer, J. A. Montgomery and E. Colle, Biomed. Mass Spectrom., 7, 53 (1980). (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 416-423 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Rats given 2-octynoic acid by intraperitoneal injection excrete elevated amounts of medium-chain dicarboxylic acids and other acidic metabolites usually associated with human medium-chain acyl-CoA dehydrogenase deficiency. Onset of this organic acid profile is immediate and lasts for approximately 24 h. The induced acidosis in this animal model closely, acutely and transiently resembles the human disorder. The 2-octynoate load is also extensively Ω- and Ψ-oxidized, and evidence is presented for the enzymic hydration of 2-octynoate to 3-ketooctanoic acid.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180610
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  • 97
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    High-sensitivity thermospray ionization mass spectrometry of dyes (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 445-449 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of dyes belonging to different chemical classes have been analyzed by thermospray (TSP) ionization mass spectrometry using a modified source containing a wire-repeller. Detection limits were determined and found to be in the range 0.05-20 ng, which are lower by a factor of 10-400 than previously published results. Positive-ion TSP mass spectra of some sulfonated dyes could be recorded for the first time owing to the increased sensitivity. Losses of SO3Na and 2SO3Na as well as losses of Na and 2Na were observed. The losses of each one of these groups involved replacement by a hydrogen atom.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180614
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  • 98
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    Determination of the new aromatase inhibitor CGS 16 949 in biological fluids by capillary gas chromatography/mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 558-562 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A specific and sensitive gas chromatographic/mass spectrometric method was developed and validated for the quantitative determination of the aromatase inhibitor CGS 16 949 in plasma and urine. A deuterium-labelled analogue of CGS 16 949 was used as internal standard. The analysis of spiked samples demonstrated the good accuracy and precision of the method. For both plasma and urine, the limit of quantification (LOQ: coefficient of variation (CV) = 10%) and the limit of detection (LOD: CV = 100%) were estimated to be 5 and 1 nmol l-1, respectively. The method was applied to the determination of unchanged CGS 16 949 in plasma and urine of a healthy volunteer orally dosed with 1 mg of CGS 16 949 A.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180808
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  • 99
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    Electronic Resource
    Determination of pipecolic acid in serum or plasma by solid-phase extraction and isotope dilution mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 566-571 
    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 pipecolic acid in serum or plasma by positive chemical ionization gas chromatography/mass spectrometry is assessed. This quantitative method involves stable isotope dilution and cation-exchange solid-phase extraction. Several derivatives of pipecolic acid and its octadeuterated analogue were investigated for their mass spectrometric characteristics. The beptafluorobutyric methyl ester derivatives afford optimal resolution on gas chromatography of biological extracts. Moreover, the derivatizing reagent (methanolic HCl) allows a combined elution and derivatization. Selected ion monitoring is performed on the [M + H]+ ions of both analyte and internal standard, at m/z 340 and 348, respectively. Serum or plasma samples from healthy subjects and patients suspected of peroxisomal diseases have been examined.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180810
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  • 100
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    On the use of laser microprobe mass spectrometry for the analysis of organic biomolecules (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 581-591 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Laser microprobe mass spectrometry has been applied to a variety of organic polyfunctional molecules, covering a wide range of polarity and mass spectrometric behaviour. The technique apparently combines desorption under relatively soft conditions with extensive fragmentation and hence allows much structural information from intactly released thermolabiles to be obtained. The mass spectra appear unfamiliar in comparison to conventional techniques. Interpretation is attempted in a purely empirical way by means of the evidence from our database and tentative hypotheses to rationalize the desorption and ionization by laser microbeam irradiation of organic solids. Selected examples are presented to illustrate the potential and limitations of the method in the field of biomolecules, such as pyridoxine and pyridoxal phosphate, nucleosides, nucleotides and related analogues, drugs and the corresponding N-oxides.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180813
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