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  • 1995-1999  (1,554)
  • 1995  (1,554)
  • Analytical Chemistry and Spectroscopy  (1,554)
  • Nuclear reactions
  • 1
    ISSN: 0269-3879
    Keywords: 4-fluoro-7-nitro-2,1,3-benzoxadiazole ; NBD-F ; 4-(N,N-dimethylaminosulphonyl)-7-fluoro-2,1,3-benzoxadiazole ; BDD-F ; enantimoeric separation ; D,L-amino acid ; biological sample ; Pirkle type stationary phase ; HPLC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The enantiomeric separations of D, L-amino acids derivatized with fluorogenic reagents, 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F), 4-(N,N-dimethylaminosulphonyl)-7-fluro-2,1-3,-benzoxadiazole (DBD-F) and 4-aminosulphonbly-7-fluoro-2,1,3- benzoxadiazole (ABD-F) by high-performance liquid chromatography (HPLC) ON various Pirkle type chiral stationary phases (CSPs, Sumichiral OA series) with citric acid in methanol as a mobile phase were studied. Since the least retention and no separation was observed for the derivatives of racemic phenylalanine methyl-ester,-amide and a drug without an α-carboxyl group, the carboxylic acid group of the amino acid derivatives seemed to contribute to the enantioselective fixation of the derivatives through hydrogen bonding on the N-acyl-amino acid amide moiety of the CSP. The enantioselective retention of the derivatives was attained through the (S) or (R) configuration of valine, phenylglycine, naphthylglycine, naphthylethylamine or the tert-leucine moiety in the CSP. The 2, 1, 3-benzoxadazole (benzofurazan) moiety in the derivatives helps the effective fixation of the derivatives through a π-πinteraction with an aromatic moiety such as a 3, 5-dinitrophenyl group in the Pirkle type chiral stationary phases.D-Amino acids in biological samples were easily determined utilizing the present derivatization with NBD-F, enantiomeric separation and fluorometric detection (530 nm em/470nm ex) following deproteinization of biological samples (serum or brain homogenate) with methanol and centrifugation. The applications of the method were clearly demonstrated by the following results; D-Ala was detected in sera of healthy volunteers at a level of 0.48-3.10μM. D-Lys was found in the serum of a patient with myeloma and requiring renal dialysis, and D-Ser was found in rat and bovine cerebrum. Peak identification was performed by use of different types of stationary phases especially those bearing the opposite configuration to that of the chiral centre.
    Additional Material: 7 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 28-31 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Hybrid isoelectic focusing of apolipoprotein A-I in polyacrylanide gels with immobilized pH-gradients under non-denaturing conditions resulted in the occurrence of additional bands which could prevent the specific and sensitive detection of genetic variants. Hybrid isoelectric focusing of tow chromatographically distinguishable apolipoprotien A-I isoforms that differ by sulphoxidaton of methionine residues, apo A-I(Met) and apo A-I(MetSO), revealed that the additional bands were caused by this post-translational modification. Several antioxidative additives and conditions were compared for their ability to prevent methionine sulphoxidation in apoliporotein A-I In the presence of 200 g/L mannitol in the gel, apolipoprotein A/I focused as a single band. Since methionine sulphoxidation in proteins is a general phenomenon either taking place in vivo or in vitro by isoelectric focusing, we conclude that isoelectric focusing in the presence of mannitol will improve the quality of resolution of many proteins in gels with immobilized pH-gradients.
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  • 3
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: We established a highly sensitive method to determine triazolam and its major metabolites, α-hydroxytriazolam and 4-hydroxytriazolam, in human plasma and urine with a liquid chromatography-mass spectrometry system which incorporates an atmospheric chemical ionization interface. A plasma sample and a urine sample after solvent extraction were injected into an ODS column of reversed phase with a mobile phase in a linear solvent gradient of initially 50 mM ammonium acetate (pH 4.0) 50%: methanol 50% and 15 min later methanol 100%; quantification limits of as low as 20 pg/mL at an SNR of 3 were obtained for each compound. With diazepam as an internal standard, recovery yields of 84, 81, and 77% were obtained for triazolam, α-hydroxytriazolam and 4-hydroxytriazolam, respectively.
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  • 4
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 52-55 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A high sensitive analytical method for salmon calcitonin (sCT) was established by means of derivatization with a fluorescence labelling agent, DBD-F, followed by HPLC separation and fluorescence detection at 558 nm with excitation at 430 nm.Under optimized conditions (DBD-F, 0.1 M borate buffer (pH 8.5): acetonitrile (70:30, v/v)), three molecules of DBD-F reacted with one sCT molecule in the presence of 1 mM sodium dodecyl sulphate (SDS) at 50 oC for 3 h. The detection limit for the sCT derivative was 20 fmol. A linear relationship was obtained between the amount of sCT on column and the peak heights in the range of 35-8000 fmol.
    Additional Material: 7 Ill.
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  • 5
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: This report describes the N-glycosylation mapping of recombinant tissue plasminogen activator (rt-PA) using micellar electrokinetic capillary chromatography. The carbohydrate structures were tentatively assigned by comparison with the anion-exchange fractionated oligosaccharides and by a comparison with previously reported data. The separation was shown to rely mainly on the degree of sialylation of the oligosaccharides, allowing a quantitative determination of the proportion of neutral and mono- to tetrasialylated structures. Significant differences in the oligosaccharide distribution of the two variants of rt-PA, which differ by the presence (type I) or the absence (type II) of oligosaccharides at the Asn-184 site, were observed. The distribution of the oligosaccharides at each of the rt-PA glycosylation sites was then determined. Glycopeptides were prepared by tryptic digestion of rt-PA and isolated using two consecutive chromatographic procedures. The glycopeptides were finally treated with N-glycanase, and the resulting oligosaccharides were analysed by capillary electrophoresis. Oligosaccharide mapping revealed that the Asn-448 and Asn-184 sites carry the same population of complex-type oligosaccharides but that the relative amounts of each oligosaccharide vary markedly. High-pH anion-exchange chromatography performed on the desialylated oligosaccharides at each glycosylation site showed that the degree of microheterogeneity was related not only to the degree of sialylation but also to structural differences in the oligosaccharide sequences. From the results as a whole, we concluded that the Asn-448 site contains a greater proportion of heavily sialylated structures and has a higher degree of microheterogeneity. The Asn-117 site was demonstrated to contain a significant number of monosialylated structures (18.4%) in addition to the high-mannose-type oligosaccharides.
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  • 6
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 85-89 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A selective and sensitive method for the determination of glutathione (GSH) and related aminothiols such as cysteine (Cys), cysteinylglycine (CysGly) and γ-glutamylcysteine (γ-GluCys) by gas chromatography (GC) has been developed. GSH and related aminothiols were converted into their N, S-isopropoxycarbonyl methyl ester derivatives and measured by GC with flame photometric detection using a short capillary column (5 m × 0.53 mm i.d.) of cross-linked DB-1. The calibration curves were linear in the range 1-25 nmol for GSH and in the range 0.2-5 nmol for other aminothiols, and the detection limits of GSH, Cys, CysGly and γ-GluCys were approximately 5, 0.2, 0.3 and 0.5 pmol per injection respectively. This method was successfully applied to blood samples without prior clean-up, and GSH and related aminothiols in these samples could be analysed without any influence from coexisting substances. Overall recoveries of GSH and other aminothiols added to blood samples were 88-107%. The analytical results of free and total blood GSH and related aminothiols in normal subjects are presented.
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  • 7
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995) 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 8
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 130-134 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple HPLC assay for serum guanase based on the direct determination of enzymatically formed xanthine was applied to normal and pathological sera. The procedure is sensitive, precise (CV below 5%) and suitable for routine purposes, and the method requires only 50 μL of sample. Using this method the reference range as determined from the sera of 40 healthy adult controls is 0-1.1 U/L. In patients with various liver diseases serum guanase activities were found to be increased 5- to 50-fold compared with the normal mean value.
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  • 9
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 226-228 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A steroeselective method, involving a single liquid-liquid extraction step, was developed and validated for the analysis of nadolol in human plasma. The assay involved extraction of nadolol and desmethyl-nadolol as internal standard (IS) from alkalinized plasma into dichloromethane. The organic solvent was separated and evaporated under nitrogen at 40°C. A chiral derivatization scheme with (R)-(-)-napthylethylisocyanate (50 μL of 0.1% solution in dichloromethane for 60 min) was employed to convert the enantiomers of nadolol into the corresponding diastereomeric derivatives. The residue was reconstitutd in the mobile phase and injected onto a C-18 column. The mobile phase was a mixture of methanol: tetrahdrofuran: water (52:7:41 by vol) containing about 0.001% v/v of both phosphoric acid and tetramethylethylenediamine. Fluorimetric detection was performed at excitation 230 and emission 330 nm. The assay was specific for the enantiomers of nadolol and the lower limit of quantitation was 2 ng/mL for of the enantiomers. Analysis of quality control samples resulted in precision estimates of 7% RSD for inter-assay and 10.1% RSD for intra-assay and the predicted concentrations deviated less than 9.4% of the nominal values for the four enantiomers. The extraction recoveries of the individual enantiomer was about 70%. Stability of nadolol enantiomers were established for four freeze/thaw cycle periods and in the autosampler at 5°C for at least 116 h.
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  • 10
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    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. i 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 11
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 251-253 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 2 Ill.
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  • 12
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 1 Ill.
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  • 13
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    Biomedical Chromatography 9 (1995), S. 269-270 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 14
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    Biomedical Chromatography 9 (1995), S. 257-258 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 15
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: In certain pathophysiological conditions, such as rheumatoid arthritis, there are alterations in the glycosylation pattern of the acute phase protein, alpha-1-acid glycoprotein (AGP). These changes are likely to be functionally significant, however, verification of the latter role requires a system which reflectsin vivo glycosylation changes in AGP and also produces sufficient quantities of the protein for further study. The human hepatoma cell line HepG2 is documented as displaying a shift in the glycosylation pattern of glycoproteins from normal state to acute phase after stimulation with inflammatory mediators. We have isolated AGP from the culture medium of HepG2 cells both before and after stimulation with a cytokine preparation and analysed the glycosylation pattern of each preparation, after enzymatic release, by high pH anion-exchange chromatography. Before stimulation, the glycosylated population was similar to a profile which was of AGP isolated from normal plasma; however, cytokine stimulation resulted in a shift to a profile which was consistent with that of AGP from a rheumatoid arthritis sufferer. Thus a HepG2 cell culture system is capable of being a crude model of the changes in glycosylation of acute phase proteins although it has a tendency to produce oligosaccharide chains which are not fully sialylated.
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  • 16
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 17
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    Biomedical Chromatography 9 (1995), S. 291-291 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 18
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple and rapid procedure is described that permits the simultaneous determination of o- and p- cresol in urine of workers or other individuals exposed to toluene. The urine samples are enzymatically hydrolysed and analysed by high-performance liquid-chromatography with a detetion limit of 0.2 mg/L, one fifth of the biological threshold limit value for o-cresol (1 mg/g ), a specific marker of toluene exposure. A graphitized carbon column Hybercarb-S, that exhibits an excellent selectivity for aromatic positional isomers, was used with 1% phosphoric acid-acetonitrile (70:30, v/v) as mobile phase and a detection wavelength of 271 nm. The overall accuracy for o-cresol determination was 4.5% at 5 mg/L and 8% at 0.5 mg/L. The cresol isomers were sufficiently resolved from endogenous materials to avoid the need for any extraction step, and the method appears suitable for monitoring workers accurately under the permissible level of exposure for occupational medicine purpose.
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  • 19
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    Biomedical Chromatography 9 (1995), S. 267-268 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 20
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 21
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 22
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    Biomedical Chromatography 9 (1995), S. 305-308 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: An assay for the measurement of unbound L-tryptophan concentrations in plasma was developed using reverse-phase HPLC with fluorescence detection. Unbound L-tryptophan from plasma was obtained using the Amicon MPS-1 ultrafiltration device. L-tryptophan binding to the membrane in the ultrafiltration device was not significant. A linear relationship between the peak-area ratios (peak-area of L-tryptophan to internal standard) and concentrations of L-tryptophan was obtained in the range of 0.1 μg/mL to 2.5 μg/L. The intra-assay precision was less than 10% for each control (0.18 μg/mL, 0.75 μg/mL and 2.0 μg/mL). The inter-assay precision was less than 15% for each control; the accuracy for each control, expressed as percent difference from nominal (%DFN), was less than 12%. This method was used to determine unbound L-tryptophan concentrations in plasma from nine male subjects who participated in a clinical study.
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  • 23
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    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995) 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 24
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    Electronic Resource
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    Biomedical Chromatography 9 (1995), S. 23-27 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Using native fluorescence detection, 5-hydroxytryptamine (5-HT), 5-hydroxyindoleacetic acid (5-HIAA) and tryptophan were resoved from themselves and other naturally occurring compounds using reversed-Phase HPLC within 5 min. Deproteinated platelet-poor plasma (ppp) and crude diluted urine were injected directly into the chromatograph. Careful selection of the HPLC column is important and various octadecyl silica (ODS) and base deactivated silic (BDS) columns were evaluated. Pre-treatment of an ODS column with tetrabutylammonium ions gave good selectivity. Between pH5 and 6 the compounds were well resolved from each other. The limit of quantitatiave detection of 5-HT and 5-HIAA was 3.5 nmol/L. The overal chromatogram obtained using native fluorescence is cleaner than that obtained with the more commonly employed electrochemical (EC) systems although the chromatography is effectively the same. For analysis of 5-HT in plasma, collection in EDTA was more efficient than lithium heparin. Plasma 5-HT in healthy volunteers was mean 61 (SD=±73) nmol/L, n=20; urine 5-HIAA gave mean 28.95 (SD=±0.98)μmol/L, (n=12). Whole blood 5-HT analysis is unreliable in comparison with platelet-poor plasma.
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  • 25
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    Biomedical Chromatography 9 (1995), S. 36-41 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple method for the measurement of clozapine and its N-desmethyl metabolite in human pläsma or serum by high performance liquid chromatography is described. An internal standard (aqueous nortriptyline, 4 mg/L) (50 μL) and Tris buffer (2 mol/L, pH 10.6) (100 μL) are added to plasma/serum (200 μL) and the analytes and internal standard extracted into methyl tert-butyl ether (200 μL). The extracts are analysed on a 150 mm column containing Spherisorb S5SCX using methanol containing ammonium perchlorate (35 mmol/L, pH 6.7) as eluent at a flow rate of 1.5 mL/min. Detection is by ultraviolet absorption (215 nm). The limit of detection is better than 0.05 mg/L for both analytes and the intra-assay precision (CV) for clozapine and norclozapine was 5.3 and 7.3% at 0.5 mg/L and 2.6 and 2.8% at 1.5 mg/L, respectively. The method can be applied to the measurement of these compounds in plasma after acute overdosage, for the assessment of compliance in patients apparently refractory to therapy and to identify interactions between clozapine and other neuroleptic and antidepressant drugs which may effect toxicity.
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  • 26
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 2 Ill.
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  • 27
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    Biomedical Chromatography 9 (1995), S. 295-301 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The chiral separation of several dipeptide enantiomers, derivatized by naphthalene-2,3-dialdehyde (NDA), was achieved by use of cyclodextrin-modified micellar electrokinetic chromatography (CD-MEKC). The dipeptides contained one or two chiral centers. In the case of several dipeptides containing two chiral centers, all four of the optical isomers could be separated and baseline resolved in less than 15 min with 20 mM γ-CD and 50 mM sodium dodecyl sulphate (SDS) in the background electrolyte. The order of elution of these derivatized dipeptides was explained by considering important chemical equlibria in the SDS, CD and peptide system. Additionally, the influence of geometric location of the chiral center, the structure of the side-chain and the effect of CD concentration on the resolution are discussed.
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  • 28
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    Biomedical Chromatography 9 (1995), S. 18-22 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Best conditions suited for the extraction and trace analysis of dimethoate, malathion, methyl-parathion, carbaryl, carbendazim and carbofuran in soils, using HPLC, were established, Theis was followed by studies related to persistence of residues in different soils, Half-life and take for 95% dissipation were determined in each case, Higher Ph, moderate mosture and hihg calcium carbonate content aided degradation while organic matter increased persistence.
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  • 29
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The introduction of chiral chromatographic methods has revolutionized the art of separationand quantitation of chiral drugs in biological fluids. A large number of chiral derivatization reagents for various funtional grups are available commercially. Therefore, Pre-column derivation methods have become attractive and simple for the gas chromatographic assays in biologcal fluids. The intent of this article is to review the pre-column chiral derivatization reagents employed in gas chromatographic separations and analyses of enantiomers. A discussion of numerous procedures necessary to develop a quantitative gas chromatographic assay method for drug enantiomers is presented. In this regard, quantitative gas chromatographic assays based on this approach have been applied to investigate the stereoselective pharmacokinetics of several chiral drug such as fenfluramine, norfenfluramine, methylphenidate, etodolac, propranol, suprofen and methoxyphenamine.
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  • 30
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    Biomedical Chromatography 9 (1995), S. 42-47 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Optimal purification of immunoglobulin M (IgM) grown as spent tissue culture supernatant can be achieved by a straightforward size-exclusion chromatography procedure. Preparative isolation of IgM was achieved by precipitation with saturated ammonium sulphate to achieve a 45% solution. IgM was then purified by gel filtration chromatography with a solution of 100 mM Tris+150 mM NaCl at pH 8. Denaturing electrophoresis and Western immunoblotting revealed two prominent bands at 80 and 25 kDa, indicative of the heavy and light chains of IgM respectively. The specific immunoreactivity of this IgM was assessed by a modified enzyme antigen capture assay. In contrast to affinity and ion-exchange chromatographies, gel filtration allows retention of IgM immunoreactivity.
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  • 31
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995) 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 32
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A rapid and sensitive HPLC-fluorescence assay was developed and validated for the determination of nadolol, a β-blocker, in human plasma. Nadolol and the internal standard (desmethyl nadolol) were extracted from alkalinized plasma into methyl-tert.-butyl ether. The organic solvent was evaporated under nitrogen at 40°C. The residue was reconstituted in the mobile phase and injected on to a C18 silica column (25 cm × 4.6 mm i.d.) at a flow rate of 1.4 mL/min. The mobile phase was 0.05 M monobasic ammonium phosphate (pH 4.2) and acetonitrile (84:16, v/v). Fluorimetric detection was performed at excitation 230 nm and emission 330 nm. The nominal retention times were 3.3 and 4.3 min for the internal standard and nadolol, respectively. The lower limit of quantitation was 5 ng/mL and linearity (R2 ≥ 0.994) of the standard curve was demonstrated between 5 and 500 ng/mL. The analysis of quality control (QC) samples at 60, 200 and 400 ng/mL resulted in precision estimates ≤7.0% relative standard deviation (RSD) for the inter-assay and ≤6.3% RSD for intra-assay. The predicted concentrations of the QC samples deviated 〈10% from the nominal values. The extraction recovery of nadolol from human plasma was 64%. Nadolol was stable in human plasma at -20°C for at least 5 months and for at least three freeze-thaw cycles. Nadolol and the internal standard were stable in the autosampler at 5°C for at least 40 h. Overall, the assay was accurate, precise, sensitive, specific and reproducible for the analysis of nadolol in plasma. The validated assay procedure was applied to study the pharmacokinetics of nadolol after administration of single and multiple doses to human subjects.
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  • 33
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A sensitive and specific high-performance liquid chromatographic assay for the non-peptide cholecystokinin subtype B receptor antagonist, CI-988, in human and cynomolgus monkey plasma has been developed and validated. The method involves isolation of CI-988 and internal standard by batch robotic solid phase extraction with a C18 cartridge, liquid chromatographic separation on a C18 column and quantitation by fluorescence detection. The human plasma assay is linear from 0.25 to 500 ng/mL for a 1.00-mL plasma aliquot. Assay precision for CI-988 based on human plasma quality control samples was within ±7.2% relative standard deviation with an accuracy of ±5.6% relative error. The monkey plasma assay is linear from 1.00 to 250 ng/mL for a 0.500-mL plasma aliquot. Assay precision based on monkey plasma quality control samples was within ±11.0% relative standard deviation with an accuracy of ±2.6% relative error.
    Additional Material: 3 Ill.
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  • 34
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Fullerenes (C60 and C70) were separated on a reversed-phase high-performance liquid chromatography column with a mobile phase of tetrahydrofuran-water (70:30, v/v) and detected with ultraviolet or electrochemical detection. A baseline resolution of C60 and C70 was achieved with a capacity factor values of 7.6 and 10.8 respectively and a resolution of 3.7. The detection limit for C60 was 0.1 pmol on column and was nearly the same for both detection methods.
    Additional Material: 1 Ill.
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  • 35
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Porphyrin metabolisms in human porphyria cutanea tarda (PCT) and in rats treated with hexachlorobenzene (HCB) have been studied in detail by high performance thin layer chromatography (HPTLC), high performance liquid chromatography (HPLC) and liquid secondary ion mass spectrometry (LSIMS). The analyses of porphyrin metabolites in the urine, faeces and liver biopsies of patients with PCT have shown that apart from uroporphyrin I and III and their expected decarboxylation intermediates and products, a complex mixture of many other porphyrins are present. The new porphyrins identified are: meso-hydroxyuroporphyrin III, β-hydroxypropionic acid uroporphyrin III, hydroxyacetic acid uroporphyrin III, peroxyacetic acid uroporphyrin III, β-hydroxypropionic acid heptacarboxylic acid porphyrin III, hydroxyacetic acid heptacarboxylic porphyrin III and peroxyacetic acid pentacarboxylic porphyrin III.
    Additional Material: 13 Ill.
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  • 36
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 157-161 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Molecular interactions can be easily determined both by thin-layer and high performance liquid chromatography. The theory and practice of the determination of molecular interactions and the various methods for the calculation of complex stability are presented. Examples of the applications of liquid chromatographic methods for the measurements of molecular interactions are also discussed.
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  • 37
    ISSN: 0269-3879
    Keywords: Tagging reagent ; pre-column derivatization ; free fatty acid in rat serum and human plasma ; fluorescence detection ; high-performance liquid chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The free fatty acids in blood were determined by high-performance liquid chromatography (HPLC) after pre-column tagging with 4-(2-carbazoylpyrrolidin-1-yl)-7-(N,N-dimethylaminosulphonyl)-2, 1, 3-benzoxadiazole (DBD-ProCZ). The tagging conditions were optimized with palmitic acid (C16:0) and linoleic acid (C18:2) as representative free fatty acids, saturated and unsaturated, respectively. Under the mild reaction conditions of room temperature for 90 min in dimethylformamide (DMF) containing 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride (EDC, 0.2 M)/pyridine (2%), all the fatty acids tested were tagged with the DBD-ProCZ to produce highly fluorescent derivatives which emit light at 550 nm (excitation at 450 nm). The fluorescence wavelenghts were essentially the same for all fatty acids, whereas the intensities were different for individual fatty acids. The derivatives obtained from ten free fatty acids were completely separated by reversedphase chromatography with two isocratic elution conditions. The on-column detection limit (signal-to-noise ratio of 3) with proposed HPLC separation and fluorescence detection is in the range of 19 (palmitic acid) -176 fmol (palmitoleic acid). The free fatty acids in rat serum and human plasma were successfully determined using the present method.
    Additional Material: 9 Ill.
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  • 38
    ISSN: 0269-3879
    Keywords: Phenylisothiocyanate ; PITC ; D/L-amino acid sequence ; peptide containing D-amino acid ; HPLC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A potential use for phenylisothiocyanate (PITC), the most popular Edman reagent, is presented for analysis of the amino acid sequence and configuration in peptides containing D/L-amino acids. After derivatization with PITC of the N-terminal amino acid (L-Tyr) of an enkephalin analogue, [D-Ala2, D-Leu5]-enkephalin, followed by cleavage/cyclization with trifluoroacetic acid at 50°C for 5 min, the liberated 2-anilino-5-thiazolinone-L-Tyr (ATZ-L-Tyr) was further treated with 20% aqueous trifluoroacetic acid at 50°C for 10 min. The resultant phenylthiohydantoin (PTH)-L-Tyr was then separated on a chiral stationary phase (a penylcarbamoylated cyclodextrin column), retaining its configuration. The residual sequence and configurations of the peptide (D-Ala-Gly-L-Phe-D-Leu) were also determined by separating the corresponding PTH-D- or L-amino acids on chiral columns. This method may be applicable to an automatic Edman sequence analyzer for the configuration determination of peptides containing D/L-amino acids.
    Additional Material: 1 Ill.
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  • 39
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A sensitive high-performance liquid chromatography (HPLC) method with fluorescence detection has been developed and applied to the determination of ACTH4-9 analogue (ebiratide), 4-(N,N-Dimethylamino-sulphonyl)-7-fluoro-2,1,3-benzoxadiazole (DBD-F) was used as a fluorogenic labelling reagent.Ebiratide in 0.1 m borate buffer (pH 9.0) was reacted with DBD-F in acetonitrile solution at 50°C for 30 min. After cooling, the mixture was seperated by a reversed-phase HPLC. Then DBD-ebiratide was monitored at 580 nm with the excitation at 440 nm. The calibration curve was liner up to 10 pmol on column (r=0.999) with the detection limit of 0.25 pmol (signal-to-noise=3).
    Additional Material: 7 Ill.
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  • 40
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A high-performance liquid chromatographic assay is described for the separation and quantification of nadolol isomers in human plasma. The isomers were quantified using reverse-phase HPLC and fluorometric detection after derivatization with the chiral reagent R(-)-1-(naphthyl)ethylisocyanate [R(-)-NEI]. The N-isopropyl analogue (one isomer) of nadolol was used as the internal standard. The method was reproducible based on precision studies where the percent relative standard deviation was less than 15%. The lower limit of quantitation for each isomer was 2.5 ng/mL. This method was used to evaluate the pharmacokinetic profile of nadolol isomers in human subjects following both single and multiple oral dosing.
    Additional Material: 4 Ill.
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  • 41
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    Biomedical Chromatography 9 (1995), S. 155-156 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A gas Chromatogrphy method using steam as the carrier gas was established for the determination of salicylic acid in plasma. A 0.5 mL plasma sample was mixed with 0.5 mL of 6N HCl and then extracted with 2 mL of dichloromethane. The dichloromethane was evaporated to dryness and the residue was redissolved in 0.5 mL of water and then analysed by gas Chromatogrphy using steam as the carrying gas. The result was calculated by external standardization.
    Additional Material: 2 Ill.
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  • 42
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The thin-layer chromatographic (TLC) behaviour of liposomes containig inositol phosphates (IPs) was studied. The liposomes contained different concentrations of D-myo-inositol 1, 4, 5-trisphosphate (IP3), D-myo-inositol 1, 2, 6-trisphosphate (α-trinositol, PP 56, a novel Perstorp Pharma derivative), D-myo-inositol 1, 3, 4, 5-tetrakisphosphate (IP4), D-myo-inositol 1, 3, 4, 5, 6-pentakisphosphate (IP5) and D-myo-inositol 1, 2, 3, 4, 5, 6-hexakisphosphate (IP6). Migration of all liposome batches was compared to that of control liposomes (containing only triple-distilled water), and to that of free phosphatidylcholine (PC); the same amount of lipid was used in all situations.Thin-layer chromatography was performed on silica gel as adsorbent. As solvent we used an n-buthanol: ethanol: water mixture in a 4:3:3 volume ratio. Significant differences were found between PC and all liposome batches, as well as between control liposomes and the ones containing IP3, α-trinositol, IP4, or IP5, in various concentrations. Liposomes containing IP6 migrate completely differently compared not only to phosphatidylcholine and control liposomes, but also to the ones containing other IPs (〈10-3 M). Unlike the other IPs studied, liposome-entrapped IP6 elicits dose-independent contractions of the isolated rat aorta. This suggests that liposomes loaded with IP6 undergo, during or after their preparation, physico-chemical alterations that eventually change their drug-delivery capacity.
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  • 43
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. i 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 44
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 45
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 273-275 
    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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  • 46
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple high-performance liquid chromatographic (HPLC) method was developed for determination of dimetridazole and metronidazole residues in poultry muscle, liver, serum and eggs. The drug residues were extracted from tissues and egg samples with acetonitrile followed by solid-phase extraction clean-up and HPLC analysis with photodiode array detector. Serum samples were treated with trichloroacetic acid, centrifuged and analysed without further clean-up. The detection limits were 2 ng/g and 5 ng/mL of analysed tissue (egg) and serum samples, respectively. Average recoveries for spike levels of 10 and 20 ng/g ranged from 82 to 94%, and coefficients of variation were below 10%.
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  • 47
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    Biomedical Chromatography 9 (1995), S. 249-249 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 48
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 2 Tab.
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  • 49
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. i 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 50
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The direct chiral separation of ofloxacin by capillary affinity zone electrophoresis using serum albumins from different animal sources as chiral selector in the supporting electrolyte is described. In addition, the effects of displacers on the mobility and enantioselectivity of ofloxacin were studied. Firstly, the separation behaviour of the enantiomers of the ofloxacin (OFLX) and tryptophan (Trp) was compared. The influence of albumin types, including chemically modified bovine serum albumins (BSAs), and buffer types on the migration behaviour of enantiomers was investigated. The results showed that stereoselectivity of Trp is independent of the type of albumin used. However, chiral separation of OFLX depends on the biological species of albumin. Use of chemically modified BSA led to poorer resolution of enantiomers. Only with acetylated BSA could chiral separation of Trp be achieved. Using Good's buffer solutions (DIPSO and HEPES) as a supporting electrolyte affected the migration times of OFLX enantiomers. Finally, a variety of displacers were added to the buffer along with the protein, and the effects on separation behaviour were observed. The displacers included warfarin, ketoproten, diazepam, propranolol, benzoinphenylbutazone, digitoxin and octanoic acid. From the results obtained, it is concluded that capillary affinity zone electrophoresis using albumin as a chiral selector may allow screening of OFLX-displacer interactions.
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  • 51
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A sensitive liquid chromatographic analysis for myo-inositol was developed using glycocyamine as the postlabelling reagent. The sensitivty was 500 pmol/injection. The system was applied to analyse myo-inositol in sera from eight patients with chronic renal failure. The average concentration of serum myo-inositol was 498.6 ± 257.0 μmol/L before haemodialysis, and 244.0 ± 131.1 μmol/L after haemodialysis. These results indicated that the kidney is the main site of myo-inositol metabolism.
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  • 52
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995) 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
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  • 53
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 2 Ill.
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  • 54
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 55
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    Biomedical Chromatography 9 (1995), S. 271-272 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 1 Ill.
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  • 56
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 57
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    Biomedical Chromatography 9 (1995), S. 32-35 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A capillary gas chromatographic method with mass-selective detection was developed for the determination of oxeladin in human plasma. Plasma samples (1 mL) were alkalinized and extracted using 5 mL of hexane: isoamyl alcohol (99:1). The method was demonstrated to be sensitive (limit of quantitation at 1 ng/mL), linear between 1 and 150 mg/mL, accurate and precise enough (mean error and mean coefficient of variation at the limit of quantitation were 2.3 and 13.3%, respectively) to support pharmacokinetic evaluation of the drug at doses down to 30 mg.
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  • 58
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The endogeneous ligand for the cannabinoid receptor, arachidonylethanolamide (anandamide) and its analogues, oleinylethanolamide, palmitylethanolamide and eicosapentaenoylethanolamide, were derivatized with a fluorogenic reagent, 4-(N-chloroformylmethyl-N-methyl)amino-7-N, N-dimethylaminosulphony 1-2,1,3-benzoxadiazole (DBD—COCl). They were separated on a reversed phse HPLC with a mobile phase of acetonitrile: water. The fluorometric detection of the derivatives was made at 560 nm with excitation at 450 nm and the detection limits for anandamide was 20 fmol on column. The structures of DBD—CO-ethanolamides were confirmed by liquid chromatography-atmospheric pressure chemical ionization - mass spectrometry (LC—APCI—MS).
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  • 59
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    Biomedical Chromatography 9 (1995), S. 80-84 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Continuous beds derivatized with three triazine dyes (Cibacron Blue 3G-A, Pricon Red HE-3B and Pricon Red H-3B) were used for chromatographic purification of dehydrogenases from yeast enzyme concentrate. All three columns, which were prepared by a very simple and cost-effective method, provided strong binding of glucose-6-phosphate dehydrogenase and lactate dehydrogenase. The Cibacron Blue 3G-A column showed high affinity for alcohol dehydrogenase. Under the same conditions, the Pricon Red HE-3B column showed a lower affinity and the Pricon Red H-3B column showed none. The adsorbed dehydrogenases were eluted specifically from the columns in high yields (71-113% by desorption with the coenzymes NADP, NADH and NAD respectively). Non-specific binding of human serum albumin and transferrin to these columns was also investigated. Enzyme assays and analyses by capillary electrophoresis showed that the continuous beds derivatized with triazine dyes gave a high degree of purification.
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  • 60
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: An isocratic and simple high-performance liquid chromatographic method is developed for the diirect resolution of the tranylcypromine (TCP) enatiomers. The method involves the use of an S-18-crown-6-ether chiral stationary phase known as the Crownpak CR (+) column. The stereochemical separation factor (α) obtained was 1.30 and the stereochemical resolution factor (Rs) was 0.69 when using a mobile phase consisting of 0.1 N perchloric acid containing 12% methanol at 23°C. The method has been used to monitor and identify, qualitatively, the profile of enantiomers of TCP in urine of an atypical depressive patient. It was found that the (-)-S-TCP concentration is significantly higher than the (+)-R-enantiomer.
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  • 61
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    Biomedical Chromatography 9 (1995), S. 106-109 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: We found a high concentration (1030 pmol per pineal gland) of D-aspartic acid (D-Asp) in the pineal gland of 6-week-old Sprague-Dawley (SD) rats. The content of D-Asp decreased with age, being 210 and 33 pmol per pineal gland in 28- and 45-week-old rats respectively. The proportion of D-Asp [(D-Asp/total Asp) × 100] also decreased with age, declining from 66% to 10% between 6 and 45 weeks after birth. The proportion of D-Asp did not differ between the sexes. The concentration of D-Asp was higher at night (at 2.00 a.m. 2830±485 pmol per pineal gland) than during the day (at 10.00 a.m. 1030±200 and at 3:00 p.m. 682±194 pmol per pineal gland), suggesting that biosynthesis of D-Asp in the pineal gland occurs at night. D-Asp was found to be distributed in the cytosol of pinealocytes, but its biological role remains unclear.
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  • 62
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    Journal of Chemometrics 9 (1995), S. 1-2 
    ISSN: 0886-9383
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 63
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    Journal of Chemometrics 9 (1995), S. 3-20 
    ISSN: 0886-9383
    Keywords: Deconvolution algorithms ; Instrumental analysis ; Spectrometry ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Deconvolution algorithms for measurand reconstruction are considered. Their metrological and numerical properties are briefly characterized. Six algorithms most frequently used for instrumental applications are selected for closer analysis. Their comparative study is based on the use of spectrometric-type synthetic data, calorimetric-type synthetic data and spectrometric real-world data. Conclusions concerning computational complexity and accuracy of the compared algorithms as well as their metrological applicability are drawn.
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  • 64
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    Journal of Chemometrics 9 (1995), S. 67-68 
    ISSN: 0886-9383
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 65
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    Journal of Chemometrics 9 (1995) 
    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
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  • 66
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    Journal of Chemometrics 9 (1995) 
    ISSN: 0886-9383
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 67
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    Journal of Chemometrics 9 (1995), S. 125-135 
    ISSN: 0886-9383
    Keywords: Procrustean analysis ; FT-IR spectroscopy ; NIR spectroscopy ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Procrustean methods allow the fitting of a given matrix to another given matrix observed on the same objects. In the traditional approach orthogonal constraints are imposed upon the transformation matrix, whereas in the alternative approach Procrustean analysis may be performed without such constraints. The two methods (with and without constraints) were compared on data dealing with mid- and near-infrared spectra of oil. The aim was to reconstruct the mid-infrared spectral information using data from the near-infrared spectra. Unconstrained Procrustean analysis proved to be the more efficient for both the calibration and verification sets. Furthermore, the analysis of the transformation matrix between the two infrared ranges made it possible to indicate wavelengths and wave numbers corresponding to the same chemical groups.
    Additional Material: 7 Ill.
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  • 68
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    Journal of Chemometrics 9 (1995), S. 91-123 
    ISSN: 0886-9383
    Keywords: H-principle ; PCA ; PLS regression ; latent variable models ; quadratic models ; sensitivity analysis ; outlier tests ; prediction variances ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: We present here an algorithmic approach to modelling data that includes principal component analysis (PCA) and partial least squares (PLS). In fact, the numerical algorithm presented can carry out PCA or PLS. The algorithm for linear analysis and extensions to non-linear analysis applies to both PCA and PLS. The algorithm allows for combination of PCA and PLS types of models and therefore extends modelling to new types of models that involve combination of regression models and ‘selection of variation’ models, which is the idea of PCA-type models. The fact that the algorithm carries out both PCA and PLS shows that PCA and PLS are based on the same theory. This theory is based on the H-principle of mathematical modelling. The algorithm allows tests for outliers, sensitivity analysis and tests of submodels. These aspects of the algorithm are treated in detail. We compute various measures of sizes, e.g. of components, of the covariance matrix, of its inverse, etc. that show how much the algorithm has selected at each step. The analysis is illustrated by data from practice.
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  • 69
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    Journal of Chemometrics 9 (1995), S. 169-178 
    ISSN: 0886-9383
    Keywords: minimum volume ellipsoid (MVE) estimators ; robust distance method ; pattern recognition ; Hotelling's T2 statistics ; near-infrared spectra ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method for pattern recognition analysis of near-infrared spectra has been developed using robust distances determined by minimum volume ellipsoid (MVE) estimators of multivariate location and scatter. Classical methods such as the Mahalanobis distance method often fail in the presence of a moderate number of outliers in a training data set, while robust distance methods can tolerate a considerably larger proportion of outliers in a training data set Outliers can be detected by their relatively large robust distances and can be excluded from a training set without a priori knowledge of the nature of the data set. In this paper the properties of a robust distance method are examined using near-infrared spectra of sulfamethoxazole and mixtures with its major degradation products, sulfanilic acid and sulfanilamide. The robust distance method successfully detected unacceptable samples (71.4%-89.3% (α = 0.05) or 78.6%-92.9% (α = 0.10)) even when they were inadvertently included in the training data set.
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  • 70
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    Journal of Chemometrics 9 (1995), S. 226-228 
    ISSN: 0886-9383
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 71
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    Journal of Chemometrics 9 (1995), S. 197-209 
    ISSN: 0886-9383
    Keywords: proficiency test ; true value ; homogeneity robust statistic ; standard ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Profficiency tests raise two types of problems: (i) the homogeneity of a sample must be carefully checked before using it as a reference material; (ii) it is necessary to define a conventional reference value (RV) in order to rank participants. Since these topics are poorly addressed in the literature, a reference material was specially prepared in order to propose a procedure for verifying homogeneity and to establish whether the algorithms classically used to compute the conventional true value have an influence on the conclusion of the test.The homogeneity of the sample was not perfect and univariate and multivariate techniques were used to demonstrate some analytes can be suspected as heterogeneous. However, this was considered adequate for introducing the sample in a large proficiency test organized between four laboratory associations which regularly perform such tests. Altogether more than 3000 measurements were collected and eight algorithms were applied to compute the RV on 14 analytes. Thus is was possible to demonstrate that some of these algorithms are better adapted than others. It is also obvious that some analytes are better suited to proficiency testing.It can be concluded from this work that some effort towards standardization would be profitable to check homogeneity or to compute the RV, especially since the economic weight of proficiency testing is becoming even more important with the development of certification accreditation.
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  • 72
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    Journal of Chemometrics 9 (1995), S. 331-342 
    ISSN: 0886-9383
    Keywords: partial least squares (PLS) ; variable selection ; IVS-PLS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: With the aim of developing PLS models with improved predictive properties, an interactive variable selection (IVS) approach for PLS regression was introduced in Part I of this series. IVS-PLS is based on a dimension-wise selective removal of single elements in the PLS weight vector w. IVS uses cross-validation (CV) as a guiding tool. The present paper illustrates the use of IVS-PLS on both simulated data and real examples from chemistry. In the first example, spectrophotometric data were simulated according to an experimental design. The objective was to see how IVS-PLS was influenced by different levels of noise in X and Y and by the number of predictor variables (K). The results of the modelling are shown as response surfaces. In addition, four real examples were modelled by the IVS-PLS technique. The real data sets were chosen to reflect different types of data from chemistry. For each example a comparison of ‘prediction error sum of squares’ (PRESS) between IVS-PLS and classical PLS is madeFor most of the examples containing many predictor variables IVS-PLS shows an improvement in predictive properties over classical PLS. Also, improvements for IVS-PLS2 (modelling of more than one y-variable) models were found. For data sets with a moderate number of variables the influence of the IVS method becomes less pronounced.
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  • 73
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    Journal of Chemometrics 9 (1995), S. 389-409 
    ISSN: 0886-9383
    Keywords: multivariate image analysis ; principal component analysis ; exploratory data analysis ; projection in multivariate space ; graphical visualization ; noise ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Multivariate image analysis (MIA) is a powerful tool for many image segmentation and classification problems, but the interpretation and understanding of the original and resulting multidimensional (multivariate) data are not always easy. A strategy for MIA has been proposed which describes its usage on multivariate images for segmentation tasks. MIA starts with principal component analysis (PCA) and then continues with interactive analysis of the output from PCA. In this paper a number of extensions to MIA are proposed. The extensions are the suggestion to incorporate preprocessing of the multivariate image in MIA, the suggestion to use synthetic multivariate image models which create a clear-cut situation, and new visualization tools which improve the interactivity and understanding of the results. Extended MIA is applied on synthetic multivariate image data simulating a possible application with large noise, positron emission tomography (PET). As a result of the interactive analysis, suggestions for preprocessing emerge. The developed methodology for handling the noise is then applied on real PET image data with good results.
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  • 74
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    Journal of Chemometrics 9 (1995), S. 21-29 
    ISSN: 0886-9383
    Keywords: Near-infrared absorbance ; Partial least squares ; Principal component regression ; Root-mean-square error of prediction ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The use of principal component regression (PCR) as a multivariate calibration method has been discussed by a number of authors. In most situations principal components are included in the regression model in sequence based on the variances of the components, and the principal components with small variances are rarely used in regression. As pointed out by some authors, a low variance for a component does not necessarily imply that the corresponding component is unimportant, especially when prediction is of primary interest. In this paper we investigate a different version of PCR, correlation principal component regression (CPCR). In CPCR the importance of principal components in terms of predicting the response variable is used as a basis for the inclusion of principal components in the regression model. Two typical examples arising from calibrating near-infrared (NIR) instruments are discussed for the comparison of the two different versions of PCR along with partial least squares (PLS), a commonly used regression approach in NIR analysis. In both examples the three methods show similar optimal prediction ability, but CPCR performs better than standard PCR and PLS in terms of the number of components needed to achieve the optimal prediction ability. Similar results are also seen in other NIR examples.
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  • 75
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    Journal of Chemometrics 9 (1995), S. i 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 76
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    Journal of Chemometrics 9 (1995), S. 137-138 
    ISSN: 0886-9383
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 77
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    Keywords: pattern recognition ; infrared spectra ; factor analysis ; maximum likelihood method ; entropy of information ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The spectral region from 700 to 3600 cm-1 is subdivided into several wave number intervals. The peaks in each interval are summarized by means of three encoding algorithms. Using a factor model of kcommon factors, the total extractable variacnce (com) of a given set of intervals is calculated and correlated with the redundancy of information in all these intervals. The value of com is verified by analysis of the factor loadings aik (factor pattern). Finally, the information content of some chosen sets of intervals coded by the three selected feature algorithms will be correlated to the probability of information flow through a serial-parallel network. The encoding using only wave numbers was found to be the most effective.
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  • 78
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    Journal of Chemometrics 9 (1995), S. 211-221 
    ISSN: 0886-9383
    Keywords: diagnostics statistics ; QSAR ; MASCA ; principal component regression ; non-least squares regression ; types of multicollincarity ; flagged observations ; influential points ; high-leverage points ; outliers ; extra-carrier points ; random perturbation ; cluster correalation ; resampling ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The formal application of a Hansch analysis to a series of 3-quinuclidinyl benzylates (QNBs) led to a ‘statistically significant’ QSAR equation. In contrast, the application of the MASCA model has shown that the design matrix is unsuitable for each QSAR analysis: one sample member is an outlier but not a high-leverage or influential point; another one is an influential point, a high-leverage point and an extra-carrier point. The regressors of the design matrix are multicollinear without predictive model power. The result of such flagged observation and this type of multicollinearity is a multiple cluster correlation. The QNB series is a good example for ‘sampling artifacts’ where no practically important but artificial QSARs can be found.
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  • 79
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    Journal of Chemometrics 9 (1995), S. 230-231 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 80
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    Journal of Chemometrics 9 (1995), S. 239-262 
    ISSN: 0886-9383
    Keywords: industrial experimentation ; parameter design ; quality by design ; robust design ; Taguchi method ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The aim of this paper is to present a simple structured review of the different approaches to robust process design to clarify their similarities and dissimilarities. It is primarily written for practitioners who wish to understand and compare the main ideas of each approach and to apply them to their work. Two examples are used to illustrate the different approaches and their corresponding data analysis strategies: the first one is a constructed example on a pigment kneading process and the second one is real example dealing with the validation of an HPLC method. A comparison of the different approaches is provided and some practical recommendations are formulated.
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  • 81
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    Journal of Chemometrics 9 (1995), S. 323-326 
    ISSN: 0886-9383
    Keywords: partial least squares ; biased regression ; ordinary least squares ; minimum length least squares ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An algebraic proof is given that in partial least squares (PLS) regression the Euclidean length of the estimator is shrunk in comparison with the ordinary least squares estimator or with PLS estimators based on a larger number of dimensions.
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  • 82
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    Journal of Chemometrics 9 (1995) 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 83
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    Journal of Chemometrics 9 (1995), S. 363-372 
    ISSN: 0886-9383
    Keywords: PLS regression ; orthogonal expansion ; optimization ; Lagrange multipliers ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A simple iteration algorithm that is faster and less memory-intensive than the NIPALS iteration algorithm for PLS regression is presented. The iteration algorithm is obtained by treating the orthogonal expansion or decomposition of a matrix X as an extremum problem subject to normalization and orthogonality constraint conditions and then solving the problem by use of the method of Lagrange multipliers. The main idea in this method is to find the transformation vector r. The latent variable t is expressed exactly as the linear combination of X-variables with the vector r so that the final regression coefficients can be conveniently provided. In the algorithm the recursion of the orthogonal projection is needed, which is derived by use of a matrix inverse formula. Algorithms are established from the equation for calculating the vector r that are suitable for dealing with three cases of large data sets. The first case is when the number of objects is very large, the number of variables is relatively small and the number of Y-variables is equal to or greater than the number of X-variables. The second case is when the number of objects is very large, the number of variables is relatively small and the number of X-variables is greater than the number of Y-variables. The last case is when the number of variables, either X- or Y-variables, or both, is very large and the number of objects is small.
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  • 84
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    Journal of Chemometrics 9 (1995), S. 423-430 
    ISSN: 0886-9383
    Keywords: PLS ; neural network ; training ; interpretable ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This communication describes the combination of a feedforward neural network (NN) with one hidden neuron and partial least squares (PLS) regression. Through training of the neural network with an algorithm that is a combination of a modified simplex, PLS and certain numerical restrictions, one gains an NN solution that has several feasible properties: (i) as in PLS the solution is qualitatively interpretable; (ii) it works faster than or comparably with ordinary training algorithms for neural networks; (iii) it contains the linear solution as a limiting case. Another very important aspect of this training algorithm is the fact that outlier detection as in ordinary PLS is possible through loadings, scores and residuals. The algorithm is used on a simple non-linear problem concerning fluorescence spectra of white sugar solutions.
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  • 85
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    Journal of Chemometrics 9 (1995), S. 439-439 
    ISSN: 0886-9383
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 86
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    Keywords: PLS ; kernel algorithm ; multivariate calibration ; EM algorithm ; cross-validation ; missing data ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This is Part II of a series concerning the PLS kernel algorithm for data sets with many variables and few objects. Here the issues of cross-validation and missing data are investigated. Both partial and full crossvalidation are evaluated in terms of predictive residuals and speed and are illustrated on real examples. Two related approaches to the solution of the missing data problem are presented. One is a full EM algorithm and the second a reduced EM algorithm which applies when the number of missing values is small. The two examples are multivariate calibration data sets. The first set consists of UV-visible data measured on mixtures of four metal ions. The second example consists of FT-IR measurements on mixtures consisting of four different organic substances.
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  • 87
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    Journal of Chemometrics 9 (1995), S. 509-520 
    ISSN: 0886-9383
    Keywords: canonical variates ; discriminant analysis ; partial least squares ; principal components ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new set of derived variables is proposed for exhibiting group separation in multivariate data on for preprocessing such data prior to discriminant analysis. The technique combines optimal features of canonical variate analysis and principal component analysis: the derived variables are linear combinations of the original variables that optimize the canonical variate criterion (ratio of between-group to within-group variance) but subject to the orthogonality constraints of principal components. In this formulation the canonical variates can be derived even when the within-group matrix is singular (i.e. when there are more variables than objects in the data matrix). A simple computational algorithm for extraction of these variables is proposed. The methods are illustrated on several data sets and compared with alternative techniques such as principal component analysis and partial least squares.
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  • 88
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 89
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    Journal of Chemometrics 9 (1995), S. 59-66 
    ISSN: 0886-9383
    Keywords: Mathematical approximation ; Sigmoid curve ; Sensitometric curve ; Photographic material ; Non-linear regression ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This paper studies the application possibilities of various mathematical analytical functions to models of approximation of sigmoid sensitometric curves of photographic materials. The newly developed functions have been tested along with approximation functions taken from the literature: the former fulfil the statistical criteria of fitting the regression and experimental curve in the best way. The model functions can be used not only for objective determination of sensitometric quantities but also for determination of the general sensitivity (speed) of photographic materials.
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  • 90
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    Journal of Chemometrics 9 (1995), S. 69-89 
    ISSN: 0886-9383
    Keywords: chemometrics ; pattern recognition ; class modeling ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Different estimators of the Mahalanobis distance (such as that based on the Defrise - Gussenhoven correction) are studied and compared with respect to the bias on the distance and the characteristics (sensitivity and specificity) of the class model.Results obtained using estimators with critical values from χ2-statistics are compared with those obtained using estimators with critical values from β-statistics (training set) and Hotelling statistics (evaluation set).Tables are reported for D-statistics (useful for simulating populations of two categories with selectable theoretical sensitivity and specificity) and for critical values of the Mahalanobis distance obtained from β-statistics.For objects of the training set the estimator of the Mahalanobis distance based on the estimate of the covariance matrix produces models with the optimum sensitivity. The same model has too low a sensitivity for objects of the model category in the evaluation set, but good specificity for objects of outer categories.The estimator with the Defrise-Gussenhoven correction produces enlarged models with too high a sensitivity for objects in the training set, good sensitivity for objects of the model category in the evaluation set and low specificity for objects of outer categories.
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  • 91
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    Journal of Chemometrics 9 (1995), S. 139-141 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 92
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    Journal of Chemometrics 9 (1995), S. 229-229 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 93
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
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  • 94
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    Journal of Chemometrics 9 (1995), S. 309-322 
    ISSN: 0886-9383
    Keywords: simulated annealing ; messy genetic algorithms ; optimization of multimodal objective functions ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The method of simulated annealing is modified so that the concept of messy chromosomes is applied. Constituent genes of messy chromosomes are specified by their respective names (indices) and values (alleles) simultaneously. Unlike simple chromosomes (binary vectors), messy chromosomes may be either under- or overspecified with respect to the problem being solved. The messy simulated annealing algorithm is a very robust and efficient stochastic optimization method which is able to find correct minima of deceptive or highly multimodal objective functions. This is shown by way of a number of simulations.
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  • 95
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    Journal of Chemometrics 9 (1995), S. ii 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 96
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    Journal of Chemometrics 9 (1995), S. 373-387 
    ISSN: 0886-9383
    Keywords: robust regression ; outliers ; spectroscopy ; calibration ; MASBR (maximum sum of binary coded residuals) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In this paper, a novel robust regression method, the maximum sum of binary coded residuals (MASBR), is proposed. Instead of the sum of squared residuals used in least squares regression as the minimization criterion, MASBR regression maximizes the sum of binary coded residuals. MASBR regression is designed for cases where the conventional robust regression methods with breakdown points less than 50% fail. To circumvent the problem of being trapped in local optima, a stepwise-varying acceptable error limit (SVAEL) algorithm is proposed. Both numerical simulation and treatment of real analytical data demonstrate the feasibility of MASBR regression in conjunction with the SVAEL algorithm.
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  • 97
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    Journal of Chemometrics 9 (1995), S. 431-432 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 98
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 99
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    Journal of Chemometrics 9 (1995), S. 489-507 
    ISSN: 0886-9383
    Keywords: QSAR ; partial least squares ; robust regression ; CoMFA ; weighted regression ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A robust implementation of partial least squares (PLS) is developed in which the method of iteratively reweighted least squares is adapted for use with PLS. The result is a PLS algorithm which is robust to outliers and is easy to implement. Examples and case studies are presented, followed by two Monte Carlo studies designed to explore the behavior of the method.The paper begins with the motivation and intended applications for the procedure. A discussion is given of the method of interatively reweighted least squares (IRLS) for outlier detection. The procedure, given the name IRPLS, is then presented. Three case studies illustrate how the procedure works on various types of data and how it should be used. The first Monte Carlo study is designed to determine whether the IRPLS procedure correctly identifies multiple outliers in a wide variety of configurations. The second Monte Carlo study is designed to estimate the breakdown bound of the procedure.
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  • 100
    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
    Library Location Call Number Volume/Issue/Year Availability
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