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  • 1985-1989  (943)
  • 1880-1889
  • 1986  (943)
  • Analytical Chemistry and Spectroscopy  (943)
  • 1
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 1-6 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A fluorescence high performance liquid chromatographic method using an immobilized 3α-hydroxysteroid dehydrogenase column as a post-column enzymatic reactor was developed for the determination of corticosteroid metabolites in the urine of subjects with congenital adrenal hyperplasia. 3α-Hydroxysteroids, such as pregnanetriol, pregnanediol and pregnanetriolone, in the eluate from μ-Bondapak phenyl column (300 × 3.9 mm I.D.) using 0.05% ammonium phosphate buffer (pH 7.1)-acetonitrile-methanol (100: 55: 15) as the mobile phase was mixed with NAD+ solution in the enzyme column at 30 °C to generate NADH, which was monitored by a fluorophotometric detector. Each steroid was measured at the 2.5 μg/dl at the highest sensitivity of the detector. The mean recoveries and reproducibilities were 91.5-108.2% with 0.9-6.5% (CV%).
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  • 2
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 21-26 
    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 with electrochemical detection (LC/EC) was developed to measure cystine and cysteinyl-penicillamine disulfide in the urine of patients screened or treated for cystinuria. Urine was acidified, centrifuged to remove urinary protein, diluted and injected. The disulfides were separated on a reversed-phase column, reduced at the upstream electrode of a dual electrochemical detector with gold-mercury amalgam (Au/Hg) electrodes and the resultant thiols measured at the downstream electrode. The sample preparation is simple, the analysis rapid, specimens can be easily batched and the specificity of the method is better than those of two other separative procedures with which it was compared. The coefficient of variation for cystine in cystinuric urine is 6.7%, 5.5% and 3.2% for levels of 0.09, 0.52 and 1.02 mmol/l respectively, and for cysteinyl-penicillamine disulfide 2.6% and 7.5% for levels of 0.45 and 0.98 mmol/l respectively. Urine for analysis of these disulfides should not be collected within 24 hours of administration of the radiopaque agent diatrizoate but no other interference to the assay has been noted. This method is suitable as a screen for cystinuria in patients with renal tract calculi, for ongoing monitoring of cystinuric patients and to check patient compliance with d-penicillamine therapy.
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  • 3
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 38-40 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The 190 nm high performance liquid chromatographic photodiode array profiling of the urinary carboxylic acids of the first urine of a newborn affected with isovaleric aciduria afforded an abnormal peak at 27.8 min. This peak was greatly increased in the carboxylic acid profiling of the 14 h urine sample from the same infant. Isolation of this peak by fraction collecting; solvent extraction of the eluent; trimethylsilyl derivatization of the residue and gas chromatographic/mass spectrometric analysis identified the compound as isovalerylglycine. Correlation of the 190 nm absorbance of isovalerylglycine (y) with concentration (x) afforded a least squares curve: y = 476.4x - 13.72 (r = 0.99) run-to-run variation 6.92%; day-to-day variation 8.88%; with a minimum detectable concentration of 25 μg/ml.
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  • 4
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The trypsin-sensitive glycopeptides from cell surfaces of a multipotential murine haemopoietic cell line (DE) have been studied using serial lectin affinity chromatography on columns of immobilized lentil lectin (LCA), concanavalin A (Con A), and wheat-germ agglutinin (WGA). WGA-binding material consisted of glycopeptides that failed to bind to LCA and Con A. Step elution from the WGA-column with 0.01-, 0.1-, 0.5- and 1.0 M N-acetyl-D-glucosamine yielded four affinity classes of glycopeptide (WGA-W, WGA-I, WGA-S and WGA-SS respectively). WGA-W, WGA-I and WGA-S contained both alkali-stable (N-linked) and alkali-labile (O-linked) carbohydrate on high molecular weight glycopeptides. The WGA-SS fraction contained only N-linked carbohydrate. N-linked glycopeptides isolated from each WGA-binding class differed in molecular size, relative N-acetylneuraminic acid content and affinity for Ricinus communis 120 agglutinin. endo-β-Galactosidase digestion showed that these glycopeptides contained polylactosamine-type glycans. Gel filtration profiles of the enzyme treated materials were different for each WGA-binding population suggesting variation in branching patterns and/or substitution with fucose residues. Affinity chromatography has shown that the WGA binding molecules are the major glycopeptide group at DE cell surfaces.
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  • 5
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 64-77 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 21 Ill.
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  • 6
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    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 93-94 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 7
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 95-100 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: In the clinical laboratory, paper chromatography is still the most useful, simple, inexpensive procedure for initial identification of abnormalities of amino acid excretion. The results of its use for more than 8000 paediatric and adult renal patients is surveyed. Nonspecific generalized aminoaciduria was the most frequent abnormality found, comprising some 70% of abnormal results, with cystine-lysinuria the next most common. The identification of the abnormal excretory pattern of amino acids as distinct from the normal was complicated by the effects of the New Zealand diet. In particular, valine, citrulline, hydroxyproline and glutamic acid are found in considerable amounts as part of the normal pattern. Their dietary origin is discussed. Varying mixtures of monosaccharides and disaccharides occurred in association with a range of amino acid patterns.
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  • 8
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 109-118 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Inherited purine and pyrimidine disorders may be associated with serious, sometimes life-threatening consequences. Early and accurate diagnosis is essential. Difficulties encountered when using existing high pressure liquid chromatographic (HPLC) methods led to the development of an improved method based on prior fractionation of urine. The advantages are as follows. 1. Production of fingerprints demonstrating altered urinary excretion patterns characteristic of any one of ten different disorders, in 30 minutes. 2. Positive identification and quantification by comparison with established methods (using conventional chromatography, electrophoresis and UV spectrophotometry) in addition to specific retention times and characteristic UV absorbance ratios at two separate wavelengths (245 and 280 nm) by HPLC. 3. Direct analysis of all the purines and pyrimidines normally found in human body fluids as well as identification of abnormal compounds. 4. Short time between successive analyses while maintaining excellent resolution between compounds of interest and column longevity. 5. Improved separation of the different adenine-based compounds encountered in some disorders, plus demonstration of potential interference by dietary or drug metabolites. 6. Applicability to the monitoring of therapy involving a variety of different purine and pyrimidine analogues.Particular attention should be paid to sample preparation. Plasma profiles will confirm the diagnosis in some, but not all, of these disorders.
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  • 9
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 140-142 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple HPLC method for penbutolol and 4-hydroxypenbutolol assay has been developed. Plasma or serum (200 μl) is vortex-mixed (30 s) with Tris solution (2 M, pH 10.6) containing an internal standard (50 μl) and methyl t-butyl ether (200 μl). After centrifugation, the extract (100 μl) is analysed using an unmodified silica column (250 × 5 mm ID) and iso-octane-methanol-methyl t-butyl ether (55:25:20) containing ammonium perchlorate (10 mM, pH 5.7) as eluent and with fluorescence detection. No interference has been encountered and the limit of accurate measurement for both compounds is 5 μg/l.
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  • 10
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A combination of gradient reversed-phase high performance liquid chromatography (RP/HPLC) with a radioreceptor assay detector that uses two ligands is used to obtain effectively the metabolic profile of endogenous receptoractive opioid peptides in the canine pituitary and in seven selected brain regions including the hypothalamus, caudate nucleus, mid-brain, amygdala, thalamus, pons-medulla, and the hippocampus. Gradient RP/HPLC separates a mixture of endogenous peptides over a wide range of hydrophobicities. A novel opioid preparation from canine limbic system synaptosomes is utilized in a radioreceptorassay screen; tritiated etorphine (ET) or D-2ala, D-5leu-leucine enkephalin (DADL) is used as the competitively displaced ligand. This receptor-rich preparation contains several receptor types, and thus serves well as a screen with the required low level of specificity. Subsequent analysis with other detectors of high specificity (MS, RIA) will follow this screen in other studies. Etorphine interacts with several of the opioid peptide-preferring receptors, whereas DADL is more specific towards the delta receptor that preferentially binds the smaller pentapeptides of the enkephalin family. The highest amount of peptide receptor activity found in this study is in the pituitary tissue, a smaller amount in the hypothalamus and caudate nucleus, and still lower amounts in the other five brain tissue extracts. This variation in peptide concentration most probably reflects three separate factors that operate in this biologic system: differential tissue-specific processing patterns of the large peptide precursors; distribution of the three opioid peptide systems; and the receptor preparation and the radioligand used in the assay. The structures of the receptoractive compounds in each RP/HPLC peak await mass spectrometric confirmation.
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  • 11
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Rat pituitary homogenates were subjected to two phase countercurrent partition in a poly(ethylene glycol)-dextran mixture using a simple apparatus with enhanced gravity to facilitate the phase separations. Assay of the fractions for organelle marker enzymes and prolactin after 17 transfers showed similar distributions for endoplasmic reticulum, lysosomes, prolactin granules and plasma membrane at the lowest dextran concentrations. Increasing the dextran concentrations had a differential effect on the various organelles. Excellent resolution of endoplasmic reticulum from the other organelles was obtained and marked organelle heterogeneity was demonstrated. Two-phase countercurrent partition thus offers an alternative approach to the subcellular fractionation of pituitary homogenates and should prove useful in separating endoplasmic reticulum from plasma membrane and other cell components.
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  • 12
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The simultaneous determination of amino acid composition including cysteine of egg albumin, a model protein containing a/s cysteine residue, is reported. All the thiol groups of the cysteine residue(s) of egg albumin were labelled with 4-(aminosulfonyl)-7-fluoro-2,1,3-benzoxadiazole, a fluorogenic reagent for thiol groups. The labeled egg albumin was hydrolyzed in 6N HCl at 110°C for 24 h. The hydrolysate was lyophilized, derivatized with 4-fluoro-7-nitro-2,1,3-benzoxadiazole, a fluorogenic reagent for amines, and subjected to HPLC. 18 derivatized amino acids including double labelled cysteine were separated within 90 min on a Nucleosil ODS column (150 mm × 4.6 mm i.d.; 5 μm), and detected at 530 nm (ex. 470 nm) in a range from 90 fmol (aspartic acid) to 1.3 pmol (cysteine) (S/N = 3). Composition ratios of amino acids of egg albumin were similar to theoretical values except for methionine, which would be destroyed under the present acid hydrolysis condition. Analytical methods for cysteine residues are reviewed, and the availability of fluorogenic reagents having the benzofurazan structure is also discussed.
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  • 13
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The hypothesis tested was that a particular glycoconjugate(s) in the exposed cell-surface membrane of susceptible insect cells acts as a receptor and/or modulator for the specific interaction with the protoxin/activated toxin of the δ-endotoxin of Bacillus thuringiensis var. kurstaki. As candidates, the total neutral and acidic fraction glycolipids, and the isolated neutral glycosphingolipid components, were screened for binding activity by the thin layer chromatogram overlay technique. The main protoxin/activated toxin-binding glycolipid in the neutral fraction (5B) had the structure: Gal(α1-3)GalNAc(β1-4)GlcNAc(β1-3)Man(β1-4)Glc(β1-1)Cer. The main protoxin/activated toxin-binding glycolipid in the acidic fraction was designated band 1, the structure of which is at present unknown. The possibility that the component 5B carbohydrate sequence may also function as a toxin-binding site of relevant insect plasma membrane glycoproteins is discussed.
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  • 14
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986) 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 15
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 53-57 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A rapid, specific and sensitive method using reversed phase HPLC for the simultaneous determination of clozapine and its two metabolites in serum and urine has been developed. The mobile phase was a mixture of 67% (v/v) methanol in water containing 0.4% tetramethylethylenediamine and 0.32% acetic acid (pH 5.5). The influence of methanol content, the pH of the mobile phase and the effect of adding alkylammonium ions as peak tailing reducer in the mobile phase have been investigated. The solvent for extracting clozapine from serum and urine was ether. 50 μ1 of 0.25 M H2SO4 solution was used to redissolve the dry residue to eliminate the endogenous compounds which could otherwise be eluted together with clozapine from the HPLC column. The analysis of a single sample was accomplished within half an hour. The identities of the chromatographic peaks of clozapine and its N-demethyl metabolite collected from the patient urine sample were confirmed by mass spectrometry. The method is sufficiently sensitive (5 ng/ml) and reproducible (CV 2.9%-6.7%) for clinical and pharmacokinetic studies, and preliminary results in these respects are presented.
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  • 16
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986) 
    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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  • 17
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Metabolites of 2,4,6-trinitrotoluene (TNT) were found in the urine of a group of TNT munition workers. The urine extracts were analysed by micro liquid chromatography/mass spectrometry. The metabolites found included 2-amino-4,6-dinitrotoluene, 4-amino-2,6-dinitrotoluene, 2,4-diamino-6-nitrotoluene, 2,6-diamino-4-nitrotoluene and untransformed TNT. The detection limit of the metabolites in urine was 0.1 ng/ml for 20 ml urine samples.
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  • 18
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986) 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 19
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    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 143-146 
    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 monitoring forphenicinol, a possible therapeutic drug for cancer and muscular dystrophy, in human plasma and erythrocytes. Forphenicinol in the deproteinized samples was separated from interfering biogenic substances on an aminopropyl-bonded silica (Unicil NH2) column within 10 minutes with isocratic elution, and determined with fluorescence detection. The detection limits for forphenicinol in plasma and erythrocytes are 65 pmol (12.8 ng)/ml and 160 pmol (31.5 ng)/ml, respectively, corresponding to 2 pmol each in a 100 μl injection volume. The method is very simple, and sensitive enough to permit the quantification of forphenicinol in the blood samples from man dosed with forphenicinol.
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  • 20
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    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 159-162 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A method for determining urine porphyrins by HPLC is described. In the preliminary step, porphyrins are purified in high yields and concentrated by low pressure reverse-phase chromatography on C18 (octadecylsilane bonded silica) cartridge. Porphyrins are stable for 10 days after adsorption on C18 cartridge. The separation of porphyrin esters is performed on an aminopropyl-bonded silica column with an eluting system containing n-heptane and ethyl acetate. The system enables rapid isocratic separation of porphyrin methyl esters with high selectivity. The simplicity and reproducibility of the whole procedure allows its application to the routine analysis of urinary porphyrins in the clinical laboratory.
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  • 21
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    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 155-158 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Endogenous opioid receptoractive peptides in the cerebrospinal fluid (CSF) of human controls and in those patients diagnosed as having senile dementia of the Alzheimer's type (SDAT) are measured with a radioreceptorassay following HPLC separation. [3H]Etorphine is the ligand used to detect in the HPLC fractions the presence of those endogenous peptides that preferentially interact with several opioid receptors. The RRA uses a receptor-rich P2 fraction extracted from a canine limbic system. The total opioid peptide content found in the HPLC fractions 6-20 (to avoid salts in fractions 1-5) of SDAT CSF (383 ± 187 pmol ME-equivalents per ml CSF) is significantly higher than the corresponding total from patients with no known neurological disorders (89.1 ± 46.3 pmol ME-equivalents per ml).
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  • 22
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    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 169-172 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple and accurate HPLC method for the determination of Orthophosphate in the presence of large amounts of organophosphates is described. The method is based on the formation and separation of the molybdenum Orthophosphate complex. In order to prevent the hydrolysis of organophosphates, the sample was deproteinized with silicotungstate in acetate buffer (pH 4.0) under ice-cooling and then treated with ammonium molybdate in maleate buffer (pH 7.0). The sample was injected onto Styragel 60 Å column (5 mm ID × 100 mm) with 38% (v/v) acetonitrile containing 0.3 M sulfuric acid as eluent. Detection was at 310 nm. The method was applied to the determination of Orthophosphate in liver, kidney, spleen and mouse blood.
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  • 23
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    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 177-179 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Trazodone, an anti-depressant medication, is found in serum in the 500-1000 ng/mL range in patients taking therapeutic doses. Because of this relatively high concentration, it has been possible to devise an HPLC assay system using the rapid, convenient microscale procedure described previously by Lam et al. (Clin. Chem. 26, 963 1980) to prepare the sample for chromatography. To 0.1 mL serum were added 0.1 mL acetonitrile and 10 μL of 10% zinc sulfate in water. The mixture was centrifuged and 50 μL of the clear supernatant was injected into a reversed-phase column which was eluted with 65% 0.05 M potassium phosphate-35% acetonitrile, with detection by ultraviolet absorbance at 210 nm. The trazodone elutes in 6 min, clearly resolved from endogenous interferences. The recovery of trazodone added to serum was better than 90%. Peak height was proportional to concentrations in the serum sample from 125 ng/mL to 3000 ng/mL.
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  • 24
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986) 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 25
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A sensitive HPLC method for the assay of UDP-GlcNAc:β-galactoside β1 → 3-N-acetylglucosaminyltransferase activity was developed. Using lactose as an acceptor, the formation of the product GlcNAcβ1 → 3Galβ1 → 4Glc can be determined without interference by substrates resulting from enzymatic and chemical breakdown of the donor substrate UDP-GlcNAc. The method is very specific since products of other transferase reactions, which potentially may be formed in the incubations in vitro, elute at positions different from that of GlcNAcβ1 → 3Galβ1 → 4Glc.By use of this assay method it could be demonstrated that normal and malignant hematopoietic cells and cell-lines, with the exception of erythrocytes and reticulocytes, contain β1 → 3-N-acetylglucosaminyltransferase activity.
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  • 26
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    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 151-154 
    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 with ultraviolet detection was developed for the determination of nivacortol (WIN 27914) in biological samples. The drug was isolated from human plasma by using a solid-phase extraction and eluted with ethanol. The solvent was evaporated and the residue dissolved in the chromatographic eluent. The sample was subjected to chromatography on a C8 silica column and eluted with a gradient of acetonitrile in 0.1 M sodium acetate buffer, pH 6.5. A single concentration of a structural analogue (WIN 31338) was used as internal standard for the quantitative determination of the analyte. The plasma concentrations were below that needed to suppress ACTH secretion by pituitary cells in culture and did not suppress plasma ACTH in Nelson's syndrome.
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  • 27
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 39-43 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Parallel triple detection ; Diesel fuels ; Polyaromatic hydrocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Diesel fuels from different parts of the UK have been analyzed for polycyclic aromatic hydrocarbons (PAH), nitrogen-containing PAH, and sulfur-containing PAH using capillary column GC with simultaneous parallel triple detection. The concentrations of polyaromatic compounds (PAC) were high and showed considerable variability amongst the fuels. The PAH are mainly naphthalene, fluorene, and phenanthrene and their alkylated homologs; the PANH are mainly carbazole and its methyl derivatives; the PASH are mainly dibenzothiophene and its methyl derivatives.
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  • 28
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 240-241 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Glass capillary columns ; Stationary phase immobilization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 29
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 236-239 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, LC ; Reversed phase ; Chemically bonded phases ; Mixed eluents ; Partition effects ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A simple linear relationship which enables the effect of the composition of a binary mobile phase on the retention of a solute to be assessed in reverse phase liquid chromatography using a bonded stationary phase has been derived. The equations have been tested using published experimental data.
    Additional Material: 3 Ill.
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  • 30
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography, SFC ; Chiral stationary phase, CSP ; Optical resolution ; α-Amino acid derivatives ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 31
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 32
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    Journal of High Resolution Chromatography 9 (1986), S. 213-217 
    ISSN: 0935-6304
    Keywords: Capillary supercritical fluid chromatography ; Injection system ; Polycyclic aromatic compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A sample introduction system for capillary supercritical fluid chromatography, which allows the dissolution of the sample in the supercritical mobile phase before being introduced into the column, was constructed and evaluated. Supercritical n-pentane was shown to solvate high-molecular-weight polycyclic aromatic compounds that could not be solvated using typical liquid solvents. In addition, split injection of a supercritical fluid solution was found to be more reproducible than split injections of a liquid solution. The potential of such an injection system was demonstrated, although further developments are needed in order to make the technique of practically utility.
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  • 33
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    Journal of High Resolution Chromatography 9 (1986), S. 224-235 
    ISSN: 0935-6304
    Keywords: Thin-layer chromatography, HPTLC ; Biological matrices ; Fluorimetric detection ; Selenium ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The present determination of selenium in biological matrices by HPTLC with in situ fluorimetric detection is an accurate alternative method, comparable to other established methods such as photometry, polarography, neutron activation, or X-ray fluorescence analysis, gas chromatography, and atomic absorption spectrometry.The excellent sensitivity of this procedure is proved by the detection limit of 250 fg of selenium per spot (using purified 2,3,1-naphthoselenodiazole). The oxidation of organic matrices, applying a novel digestion procedure, may be carried out with little instrumental expenditure.Sample preparation steps, such as the oxidation of selenium to Se (VI) and subsequent reduction to Se (IV) do not lead to significant random or systematic errors, nor does the digestion step, if an optimized procedure is used.A recovery rate of 103% and nearly parallel calibration curves for digested selenocysteine standards compared with spiked human serum samples demonstrate the accurate quantitative preparation of a biological matrix. Any interfering metal ions can be masked by addition of chelate-forming reagents.
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  • 34
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    Journal of High Resolution Chromatography 9 (1986), S. 252-254 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Post-column derivatization reaction ; Fluorogenic reaction ; Haloperidol ; N1-Methylnicotinamide chloride ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 5 Ill.
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  • 35
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    Journal of High Resolution Chromatography 9 (1986), S. 260-260 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 36
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    Journal of High Resolution Chromatography 9 (1986) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 37
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    Journal of High Resolution Chromatography 9 (1986), S. 289-290 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 38
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    Journal of High Resolution Chromatography 9 (1986), S. 295-297 
    ISSN: 0935-6304
    Keywords: Gas-liquid chromatography, GC ; Fused silica tubing ; Connector ; Coupling ; Press-fit ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
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  • 39
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    Journal of High Resolution Chromatography 9 (1986), S. 304-305 
    ISSN: 0935-6304
    Keywords: HPLC ; Non-porous supports ; Tetra-ortho silicates ; Commercial supports ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 40
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    Journal of High Resolution Chromatography 9 (1986), S. 314-316 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 41
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    Journal of High Resolution Chromatography 9 (1986), S. 312-313 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Fused silica capillary micro-packed columns ; Open tubular columns ; Sample capacity ; Trace analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 42
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    Journal of High Resolution Chromatography 9 (1986), S. 320-327 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Electron capture detector, ECD ; Electron capture sensitization ; Polynuclear aromatic hydrocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The electron capture detector (ECD) response to numerous aromatic hydrocarbons of low electron affinity (EA) is shown to be detrimentally affected by two processes which compete with and typically overwhelm the electron capture reactions of these molecules. It is shown that the effects of these two undesired reactions can be eliminated by the permanent addition of trimethylamine and one of several alkyl monochlorides to the detector make-up gas. These modifications of the detector gas result in greatly increased sensitivity, increased linearity, and increased reproducibility of response. A kinetic model for the ECD responses of low EA resonance capture molecules is developed which appears to explain these improvements.
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  • 43
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    Journal of High Resolution Chromatography 9 (1986), S. 328-334 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; GC/MS ; Fused silica (capillary) columns ; Retention index data ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Retention indices of standard organic compounds of environmental interest were determined by gas chromatography/mass spectrometry, using a DB-5 fused-silica capillary column. Retention indices are useful references for tentative compound identification by gas chromatography, or confirmation by gas chromatography/mass spectrometry. They provide elution order for isomers that might be indistinguishable based on mass spectra. Modified Kovats and Lee retention indices are given for polycyclic aromatic hydrocarbons; sulfur heterocycles; nitrogen heterocycles; aromatic amines; oxygen heterocycles; phenols; alcohols; ketones; alkanes; nitriles; and methylesters of fatty, dicarboxylic, and aromatic acids for comparison and reference. Retention index values for heterocycles by gas chromatography/mass spectrometry are comparable with gas chromatography values previously reported.
    Additional Material: 1 Tab.
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  • 44
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns, glass ; OV-240-H, 33% cyanopropyl ; Immobilization by condensation ; Crosslinker, dimethyltetramethoxysiloxane ; in situ methylation, diazomethane ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Coating intensely leached glass capillaries with OV-240-OH, the most polar commercially available OH-terminated polysiloxane phase at the present time, is described. Beside chemical bonding of the phase via condensation with silanol groups of the support, additional immobilization using dimethyltetramethoxysiloxane as a crosslinker is carried out. After in situ methylation of the immobilized coating, and transformation of acidic impurities of the cyanopropyl substituted phase into the respective methyl esters, increased inertness of the column was observed. Working instructions are given, and processes involved are discussed.
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  • 45
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    Journal of High Resolution Chromatography 9 (1986), S. 366-372 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 46
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    Journal of High Resolution Chromatography 9 (1986), S. 383-387 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Dual capillary gas chromatography ; Alcohols ; MTBE ; Gasolines ; Additives ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A gas chromatographic method has been developed for the identification and direct determination of alcohols and methyl tert-butyl ether (MTBE) in gasolines. The technique involves simultaneous injection of the gasoline without any sample preparation onto two fused silica capillary columns of differing polarities. The method permits simultaneous determinations of methanol, ethanol, 2-propanol, tert-butanol, 1-propanol, sec-butanol, 1-butanol, and MTBE. By using an automatic sampler in combination with electronic pressure programming and BASIC programming, the determinations were performed automatically and reproducibly with a relatively short analysis time.
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  • 47
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    Journal of High Resolution Chromatography 9 (1986), S. 409-410 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Reversed phase ; MAPS phase ; Explosives ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 48
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    Journal of High Resolution Chromatography 9 (1986), S. 417-419 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Normal phase ; Bonded phases ; Mercaptopropyl silica gels ; Donor-acceptor complexes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 49
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    Journal of High Resolution Chromatography 9 (1986), S. 561-565 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Pharmacokinetics ; Quantification in human plasma ; Bronchosecretolyticum ; Separation from metabolites ; Ambroxol ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The bronchosecretolytic drug ambroxol can be reliably quantified in human plasma by high performance liquid chromatography. Plasma is buffered alkaline, extracted with ether, and the organic solvent back-extracted with diluted acid. An automatically sampled aliquot is separated by reversed phase HPLC; the analyte is well separated from two metabolites that interfered strongly in earlier methods. UV detection at 230 nm enables a lower limit of quantitation of 5 ng/ml. Internal standardization with propranolol allows accurate and precise quantification. Evaluation of the optimized combination of mobile and stationary phase is described, and application of the method to experimental and clinical pharmacokinetic studies is illustrated.
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  • 50
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    Journal of High Resolution Chromatography 9 (1986), S. 122-124 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Nonsuppressed ion exchange ; Conductivity ; Detectability ; Inorganic anions ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 51
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    Journal of High Resolution Chromatography 9 (1986), S. 127-128 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Reversed-phase HPLC ; Metal chelates ; 8-Hydroxyquinolinates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 52
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    Journal of High Resolution Chromatography 9 (1986), S. 595-595 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Connection device ; Micro packed columns ; Macrobore capillaries ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 53
    ISSN: 0935-6304
    Keywords: Preparative planar chromatography, PPC ; Centrifugal planar-column chromatography, CPCC ; Circular development ; On-line observation and detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 54
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    Journal of High Resolution Chromatography 9 (1986), S. 613-617 
    ISSN: 0935-6304
    Keywords: Fused silica capillary tube isotachophoresis ; Multichannel photodiode array detector ; Cationic dye analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Isotachophoresis carried out in a 0.25 mm i.d. fused-silica capillary tube yielded high resolution, compared with that in a fluorinated ethylene-propylene polymer tube. The use of an ultraviolet-visible multichannel spectrophotometer with photodiode array as detector together with a cross flow cell (volume 0.01 μl) was investigated. The system was successfully applied to the analysis of cationic dyes such as neutral red, bismarck brown, and basic fuchsine.
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  • 55
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    Journal of High Resolution Chromatography 9 (1986), S. 535-537 
    ISSN: 0935-6304
    Keywords: Liquid chromatography ; Fused silica capillary columns ; Reverse-phase ; Nanoliter flow cell ; Column packing ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 56
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    Journal of High Resolution Chromatography 9 (1986) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 57
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    Journal of High Resolution Chromatography 9 (1986), S. 306-307 
    ISSN: 0935-6304
    Keywords: Liquid chromatography ; Fluorometric determination ; Postcolumn reaction ; o-Phthaldehyde ; Saliva bradykinin ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 58
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    Journal of High Resolution Chromatography 9 (1986), S. 335-340 
    ISSN: 0935-6304
    Keywords: Capillary gas-liquid chromatography ; Stationary-phase focusing ; Swelling ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Sample introduction using the solvent effect can lead to significant swelling of the stationary phase. The phenomenon has been studied theoretically and experimentally. The longitudinal profile of the swollen phase has been established. Swelling can affect the retention time of solutes, the shape of solute bands emerging from the inlet, and the maximum permissible sample size.
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  • 59
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    Journal of High Resolution Chromatography 9 (1986), S. 345-349 
    ISSN: 0935-6304
    Keywords: Isothermal vs programmed indices ; Coefficient of index increase ; Equivalent isothermal temperature ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A systematic approach was utilized to deduce the relation between the programmed and isothermal retention indices in chromatography. The relation was given in the form of a chart from which the equivalent isothermal temperature Te is plotted vs ΔT′ with IP as the parameter. ΔT′ is a function of both the inlet and outlet temperatures during the temperature programmed run and Te is the temperature at which the isothermal index is equal to the programmed index IP.
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  • 60
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    Journal of High Resolution Chromatography 9 (1986), S. 362-363 
    ISSN: 0935-6304
    Keywords: Back fat of pigs ; Skatole ; Indole ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 61
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    Journal of High Resolution Chromatography 9 (1986), S. 388-391 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Cryogenic GC ; Capillary, fused silica ; Sulfur gases ; Water alterations of phase polarity ; Reverse solvent effect ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Data are presented to illustrate putative water effects on the retention times and peak shapes for seven sulfur-containing compounds when determined by sub-ambient FSOT capillary GC/FPD. The observations are consistent with explanations based upon reported “phase soaking” and “reverse solvent effect” phenomena.
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  • 62
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    Journal of High Resolution Chromatography 9 (1986), S. 405-407 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Solvent effects ; Solvent trapping ; Phase soaking ; Large sample volumes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 63
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    Journal of High Resolution Chromatography 9 (1986), S. 397-399 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Capillary columns ; Nifedipine ; Determination in human plasma ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A rapid, sensitive, and reliable method for the determination of nifedipine in human plasma is described. Using a single-step solvent extraction and capillary gas chromatography combined with electron capture detection, an assay sensitivity of 2 ng/ml is achieved routinely using 0.5 ml of plasma. Intact nifedipine is quantitated and separated from its nitroso- and nitropyridine-derivatives. The suitability of the assay for pharmacokinetic studies is illustrated.
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  • 64
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    Journal of High Resolution Chromatography 9 (1986), S. 30-34 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Nickel capillary columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Electroformed nickel tubing was deactivated by chemical vapor deposition of silicon from silane gas and subsequent treatment with cyclooctamethyltetrasiloxane (D4). Standard activity tests performed on the uncoated tube and also on columns coated with crosslinked and uncrosslinked, nonpolar stationary phase, show that good quality flexible columns can be prepared from nickel tubing. The inner surface of the silicon coated tube was characterized by Auger depth profile analysis.
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  • 65
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    Journal of High Resolution Chromatography 9 (1986), S. 102-105 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Pharmacokinetics ; Quantitation in human serum ; Antidiabeticum ; Glibenclamide ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The antidiabetic drug glibenclamide can be reliably quantitated in human serum with high performance liquid chromatography. The serum is buffered and extracted with toluene. The organic solvent is evaporated, the residue dissolved in the mobile phase and an aliquot sampled automatically and chromatographed. UV-detection at 229 m allows a lower limit of quantitation of 5 ng/ml. Precise handling of exact volumes facilitates external calibration. Statistical data for imprecision and inaccuracy are given and illustrate reliable quantification. Application of the method to experimental and clinical pharmacokinetic studies with specific problems is illustrated.
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  • 66
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    Journal of High Resolution Chromatography 9 (1986), S. 115-115 
    ISSN: 0935-6304
    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 High Resolution Chromatography 9 (1986), S. 129-130 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 68
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    Journal of High Resolution Chromatography 9 (1986), S. 136-136 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 69
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    Journal of High Resolution Chromatography 9 (1986), S. 154-160 
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography ; Ion mobility detection ; Tunable, selective detection ; Fourier transform-ion mobility spectrometry ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Using a unidirectional flow ion mobility detector, non-selective detection, tunable selective detection, and complete Fourier transformed ion mobility spectra were successfully obtained after supercritical fluid chromatography on compounds with higher molecular weights than have been previously investigated. In the most selective mode, single oligomers from polymeric material could be independently detected. Using the Fourier transform capabilities of this instrument, complete ion mobility spectra for each oligomer could be obtained in a single chromatographic separation. The collection of individual ion mobility spectra of the components of polymeric material has not been possible prior to the technique described in this paper. Only complex ion mobility spectra of polymeric mixtures are available in the literature. The spectra obtained in this study are all simple, uncomplicated spectra consisting of only one or two product ion peaks. Ko values reported in this work range from 0.633 to 1.61, which are some of the lowest values ever reported in ion mobility spectrometry.With the unidirectional flow design of the detector, the supercritical fluid mobile phase, carbon dioxide, was efficiently eliminated from the detector so that the ion mobility spectrometer could be operated in its normal manner. The fact that CO2 did not interfere with normal ion mobility operation indicates that other supercritical fluids may also be compatible with this sensitive and versatile detection method.
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    Journal of High Resolution Chromatography 9 (1986), S. 186-187 
    ISSN: 0935-6304
    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 High Resolution Chromatography 9 (1986), S. 193-194 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 72
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    Journal of High Resolution Chromatography 9 (1986) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 73
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    Journal of High Resolution Chromatography 9 (1986), S. 357-358 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column, glass ; Large on-column injection ; Retention gap ; Diethyl-dithiocarbamate-metal chelate analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 74
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    Journal of High Resolution Chromatography 9 (1986), S. 361-361 
    ISSN: 0935-6304
    Keywords: Preparative gel-chromatography ; Quantitative analysis of polycarbonates ; Hydrolysis of polycarbonates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 75
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986) 
    ISSN: 0935-6304
    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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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 419-420 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Ligand exchange ; Uracil derivatives ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 77
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 78
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 452-455 
    ISSN: 0935-6304
    Keywords: Liquid adsorption chromatography ; Mixed mobile phases ; Surface activity coefficients ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: General equations describing adsorption from solutions on solids and liquid adsorption chromatography with mixed mobile phases are formulated in terms of the bulk and surface activity coefficeints. Definition of the surface activity coefficients is extended; they describe nonideality of surface solution due to difference in molecular interactions of the components as well as nonideality of this solution generated by the adsorbent heterogeneity. It is shown that the above general equations predict simpler expressions known already in the literature.
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  • 79
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    Journal of High Resolution Chromatography 9 (1986), S. 515-517 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary column ; Electron impact mass spectrometry ; Linear retention indices ; Dinitrofluoranthenes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This paper reports the retention indices of eighteen of the possible twenty-five dinitrofluoranthene isomers.
    Additional Material: 1 Ill.
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  • 80
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    Journal of High Resolution Chromatography 9 (1986), S. 64-64 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 81
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    Journal of High Resolution Chromatography 9 (1986), S. 73-77 
    ISSN: 0935-6304
    Keywords: Capillary supercritical fluid chromatography ; Fast analysis ; Nonvolatile analytes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Capillary supercritical fluid chromatography (SFC) is proving to be a viable and useful separation method for thermally labile and nonvolatile materials. As with other capillary chromatographic techniques, very fast separations can be accomplished by sacrificing total efficiency and optimizing the conditions for rapid analysis. This is achieved using short, small-bore capillary columns, increased mobile phase linear velocities and very fast pressure programming rates. These principles are demonstrated for the rapid separation of selected component systems.
    Additional Material: 4 Ill.
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  • 82
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    Journal of High Resolution Chromatography 9 (1986), S. 84-88 
    ISSN: 0935-6304
    Keywords: Liquid chromatography ; Fused silica capillaries ; Micro-HPLC ; Gradient elution ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fused-silica microparticulate packed columns are demonstrated to have equal or better separation efficiency and resolving power than conventional 4.6 mm i.d. packed columns. While neither separation efficiency nor resolving power is an inherent consequence of capillary column use, there re potential advantages of using fused-silica capillary columns, particularly when microparticulate particles of 1 to 5 üm are used in the gradient elution mode. Gradient elution techniques compatible with flow rates below 30 μL/min are discussed. Spli-flow gradient elution of twenty PTH amino acids using 10 and 40 cm × 0.54 mm i.d. columns packed with 4 μm Micro-Pak PTH-AA particles is demonstrated. Detection limits of 0.1-0.3 picomoles are meaured for PTH amino acids and 0.01-0.02 picomoles for tricyclic antidepressant drugs.
    Additional Material: 7 Ill.
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  • 83
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    Journal of High Resolution Chromatography 9 (1986), S. 434-434 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 84
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    Journal of High Resolution Chromatography 9 (1986), S. 446-451 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns, fused silica ; Retention index library ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: During the development of a GC retention index library very rigorous standard parameters were used in the SADTLER laboratories. Because most chromatographers presumably have their “favourite” and well-proven columns a study has been carried out on how to make use of them for standard index generation. Variables such as column geometry, split ratio, and film thickness were examined and the calculated indices were compared to some “basic” values. Splitless and cool on-column injection techniques were also investigated and comparable temperature programming indices have been obtained. Finally, standard index values of 53 volatile halogenated hydrocarbons measured on very thick-film bonded fused silica capillary columns are tabulated.
    Additional Material: 6 Tab.
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  • 85
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    Journal of High Resolution Chromatography 9 (1986), S. 474-476 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Dead volume FPD ; Peak shape ; Sulfur gases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 86
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    Journal of High Resolution Chromatography 9 (1986), S. 485-488 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 87
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    Journal of High Resolution Chromatography 9 (1986), S. 572-576 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, LC ; Chromophore mobile phase ; Indirect UV detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An indirect UV photometric detection technique is described in which a low concentration of a UV-absorbing compound (UVAC) is added to the mobile phase in reversed phase liquid chromatography, thereby making it possible for non UV-absorbing compounds such as the lower alcohols to be detected by the UV detector. This happens because the injected analyte may extract a portion of the UV absorbing compound from the mobile and/or stationary phase and the complex is co-eluted as a positive peak at the retention time of the analyte. Alternatively, the injected analyte may appear as a negative peak if the UV-absorbing compound is transferred to the mobile and stationary phases. In any case, the injected compound appears either as a positive or negative peak depending on the relative polarities and concentrations of all the compounds in the system. In addition, the resulting excess or deficiency of detection agent in the stationary phase is eluted separately as a positive or negative peak, indicating that the system has returned to equilibrium. In the work described herein, the chromatographic conditions and variables of the indirect photometric technique were studied to develop a quantitative HPLC method for UV-transparent compounds. It was found that under optimal conditions it is possible to determine some analytes quantitatively at concentrations as low as 0.05%.
    Additional Material: 3 Ill.
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  • 88
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    Journal of High Resolution Chromatography 9 (1986), S. 596-597 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Gas chromatography-mass spectrometry, GCMS ; Curie-point pyrolysis ; Biomaterials ; Biomass ; Foodstuffs ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 89
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    Journal of High Resolution Chromatography 9 (1986), S. 602-604 
    ISSN: 0935-6304
    Keywords: HPLC ; Amino acids ; Dansyl chloride derivatization ; Infusion solution ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 90
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    Journal of High Resolution Chromatography 9 (1986), S. 285-288 
    ISSN: 0935-6304
    Keywords: Thin-layer chromatography ; Continuous development ; ΔRf ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Equations for predicting analysis time in thin-layer chromatography as a function of spot separation, solvent velocity constant, ΔRf and Rf, are presented and discussed.
    Additional Material: 5 Ill.
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  • 91
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    Journal of High Resolution Chromatography 9 (1986), S. 298-300 
    ISSN: 0935-6304
    Keywords: Capillary gas-liquid chromatography ; Stationary phase focusing ; Thermal focusing ; Joule-Thomson effect ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
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  • 92
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    Journal of High Resolution Chromatography 9 (1986), S. 679-682 
    ISSN: 0935-6304
    Keywords: Fused silica capillaries ; Deactivation ; Silylation ; Aerobic conditions ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new, simple procedure to deactivate fused silica capillaries without hydrothermal treatment is proposed. Based on high temperature reactions of octamethylcyclotetrasiloxane (D4) in the presence of oxygen, this procedure results, upon coating with dimethylsilicone (SE-30), in columns which give almost symmetric peaks for as little as 150 pg of critical compounds, such as decylamine, thereby demonstrating very high inertness. A mechanism of the deactivation procedure, which, in contrast to previously developed procedures, is based on thermal reactions under aerobic conditions, is proposed.
    Additional Material: 2 Ill.
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  • 93
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    Journal of High Resolution Chromatography 9 (1986), S. 698-702 
    ISSN: 0935-6304
    Keywords: Capillary column gas chromatography ; Microwave-induced plasma emission spectrophotometric detector ; Photodiode array spectrophotometer ; Element-specific detector ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A microwave-induced plasma emission spectrophotometric detector (MIPD) was used as an element-specific detector for capillary column gas chromatography. The atmospheric pressure microwave helium plasma generated with an original device called a SURFATRON was used as an atomization and excitation source. Combining a photodiode array spectrophotometer with the above system made the emission spectrophotometric detector very powerful. A wide range of spectra could be instantly monitored without any mechanical device.However, the spectrum of atmospheric helium emission plasma was complicated by the presence of air around the plasma discharge. An on-line background correction scheme was developed to handle such complicated spectra.
    Additional Material: 5 Ill.
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  • 94
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    Journal of High Resolution Chromatography 9 (1986), S. 59-60 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Discrimination ; Moving needle injector ; Splitless injector ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 95
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986) 
    ISSN: 0935-6304
    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 High Resolution Chromatography 9 (1986), S. 78-83 
    ISSN: 0935-6304
    Keywords: Gas chromatography Chemometrics ; Capillary columns ; Orange oils ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Orange essence oils of the Navel and Valencia variety were analyzed by GC and GC/MS using two parallel capillary columns of different selectivity. Data were normalized, converted into a computer compatible format, and transferred via an asynchronous communications interface to a mainframe computer for statistical treatment, using the chemometrics software package ARTHUR. After suitable preprocessing of the raw data, reliable classification was possible. It appears that four substances which are present in both varieties can be used for that purpose.
    Additional Material: 6 Ill.
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  • 97
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    Journal of High Resolution Chromatography 9 (1986) 
    ISSN: 0935-6304
    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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    Journal of High Resolution Chromatography 9 (1986), S. 18-29 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Mass spectrometry ; Purge and trap ; Purgeable compound analysis ; Trace organic analysis ; Priority pollutants ; Cryotrapping of organic compounds ; Cryofocusing of organic compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The effects of trapping temperature and column film thickness were investigated with respect to their ability to promote effective cryofocusing on fused silica capillary columns. The study was a further development of the purge and trap with whole column cryotrapping (P&T/WCC) method. The rates at which compounds could be thermally desorbed from a P&T unit and transferred to a column (with zero split) were first examined. A near quantitative transfer of the desorbable analytes was obtained with a 4 min, 180°C, 20 mL/min desorption. The compounds tested included naphthalene. Columns with film thicknesses from 0.12 to 3.0 μm were then investigated in P&T/WCC analyses with WCC temperatures ranging from -80 to 0°C. The trapping took place from a transfer line gas stream initially at 175°C. The volatilities of the compounds examined varied from that of 1,1-dichloroethene to 1,1,2,2-tetrachloroethane. A higher film thickness was found to ease the WCC temperature requirements. Within each column type, the warmest WCC temperatures which allowed good cryotrapping with no significant increases in peak width were: 0.25 μm, -70°C; 1.0 μm, -50°C; 3.0 μm, -20°C. In addition to being quantitative, the trapping provided good chromatography.
    Additional Material: 12 Ill.
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  • 99
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    Journal of High Resolution Chromatography 9 (1986), S. 44-48 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Fourier Transform Ion Mobility Spectrometry ; Ion mobility detector ; Barbiturates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This paper demonstrates a novel operating mode of an ion mobility detector (IMD) for obtaining both qualitative and quantitative data after capillary gas chromatographic separation of 5,5′-disubstituted barbiturates. Using a recently developed time dispersive Fourier transform method for ion mobility spectrometry, complete ion mobility spectra could be obtained for each component in the chromatogram. This type of spectra can be used for providing qualitative information on unknown compounds or for selecting the proper detector conditions needed when operating in the continuous mobility monitoring mode.In this study each of the five barbiturates investigated produced a Fourier transformed ion mobility spectrum containing one major product ion. When drift times corresponding to those of the product ions measured in the FT mode were monitored continuously, selective chromatographic detection of the barbiturates was achieved. In one case even isomers could be differentiated based on mobility characteristics.
    Additional Material: 6 Ill.
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  • 100
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    Journal of High Resolution Chromatography 9 (1986), S. 68-68 
    ISSN: 0935-6304
    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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