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  • 101
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 300-302 
    ISSN: 0935-6304
    Keywords: Supercritical-fluid-extraction ; supercritical-fluid-chromatography ; vitamin E ; pharmaceuticals ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No abstract
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 102
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 315-321 
    ISSN: 0935-6304
    Keywords: Glycopeptide antibiotics ; chiral selectors ; Teicoplanin ; enantioseparations ; CZE ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Baseline separation of the enantiomers of a number of negatively charged amino and mandelic acid derivatives was achieved in less than 10 min by capillary electrophoresis in a polyacrylamide coated capillary, using the “partial filling method” (PFM) with submillimolar concentration of Teicoplanin (TE) as the chiral selector. The influence of the charge and concentration of TE, electrolyte solution composition and pH, on the enantioresolution was examined. Further proofs were brought to corroborate the hypothesis that the enantiorecognition takes place at the D-Ala-D-Ala binding site, whose blockade is responsible for the antibacterial activity of glycopeptide antibiotics. While the dependence of the chiral recognition capabilities of TE on electrolyte solution composition and pH could limit its applicability, improved sensitivity, reduction of TE wall adsorption, resulting in a good efficiency, and high cost reduction, due to the very small amount of chiral selector required, were shown as advantages of the PFM adopted in this study.
    Additional Material: 6 Ill.
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  • 103
    ISSN: 0935-6304
    Keywords: Large volume on-column injection ; partially concurrent solvent evaporation ; solvent trapping ; retaining precolumn ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---When 0.53 mm i.d. uncoated precolumns connected to a solvent vapor exit are used for sample introduction with partially concurrent solvent evaporation, substantial losses of volatile solutes are often observed. They were found to be the consequence of solute accumulation at the front end of the flooded zone, which in turn is the result of a strong pressure drop over the flooded zone owing to the formation of plugs of sample liquid. The pressure drop causes significant solvent evaporation at the front, which enriches the solute material there and causes its loss. The use of 0.32 mm i.d. restrictions between the uncoated precolumn and the vapor exit greatly reduced this problem.
    Additional Material: 10 Ill.
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  • 104
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 339-342 
    ISSN: 0935-6304
    Keywords: Chlorophyll ; SFC ; supercritical fluid chromatography ; vegetables ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Complex mixtures of chlorophyll degradation products may arise during processing and storage of vegetable oil and green plant materials like broccoli and spinach. Determination of these compounds is important in the area of food chemistry. Therefore a method using packed column supercritical fluid chromatography (SFC) has been developed. The method comprises chromatography using a simple gradient of methanol in carbon dioxide at constant column back pressure of 30 MPa and a column temperature of 40°C. Effects of pressure and mobile phase composition showed the importance of applying a modifier gradient for optimal separation of the chlorophyll products. The method permits separation of 15 chlorophyll derivatives including chlorophyll a and b, pheophytins, and pyropheophytins on a C18 column in about 20 minutes. Identifications of the individual peaks were based on reference compounds, the retention order of the compounds, and their absorption spectra.
    Additional Material: 5 Ill.
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  • 105
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; gas chromatography-mass spectrometry ; essential oil analysis ; Lepechinia schiedeana ; antioxidant activity ; lipid peroxidation ; Ledol; Ledol HMQC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Steam distillation (SD), simultaneous distillation-solvent extraction (SDE), microwave-assisted solvent extraction (MWE), and supercritical (CO2) extraction (SFE) were used to isolate secondary metabolites from Lepechinia schiedeana. The various extracts were analyzed by capillary gas-chromatography, on poly (dimethylsiloxane) (DB-1) and poly(ethyleneglycol) (INNOWAX), 60 m columns, using FID or MSD (EI, 70 eV). Kováts indexes, mass spectra, or standard compounds were employed for compound identification. 43, 61, 67, and 79 compounds at concentrations above 0.01% were detected in the SD, SDE, MWE, and SFE extracts, respectively. Ledol, C15H26O, was the major constituent (20.04-36.87%) in all extracts. Oxygenated sesquiterpenes (24.36-43.14%), C10H16, monoterpenes (27.70-39.87%), and C15H24, sesquiterpenes (10.04-22.22%) were the main groups of compounds present in SD, SDE, MWE, and SFE extracts. Heavy hydrocarbons (Cn 〉 15), diterpenoids, and phytosterols were found only in MWE and SFE extracts. The antioxidant activity of Lepechinia schiedeana was measured by the HRGC quantification of the volatile carbonyl compounds, final products of lipoxidation, released in a model lipid system (sunflower oil) by the effect of the Fenton reagent. The concentration of volatile carbonyl compounds decreased by 65% when lipid oxidation was induced in the presence of macerated Lepechinia plant. The protection of polyunsaturated acids in sunflower oil was also studied by measuring their concentrations after heating of the oil (180°C, 2 h) with and without macerated Lepechinia plant.
    Additional Material: 4 Ill.
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  • 106
    ISSN: 0935-6304
    Keywords: Silver ion HPLC ; long chain polyunsaturated fatty acid ; isopropanol ; separation of positional isomers ; degree of unsaturation ; normal phase retention effect ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---A high resolution approach to silver ion HPLC was studied for the separation of positional isomers of triacylglycerols (TAGs) containing long chain polyunsaturated fatty acids (PUFA) such as eicosapentaenoic acid (EPA), docosahexaenoic acid (DHA), and docosapentaenoic acid (DPA) in enzymatically synthesized structured TAGs. Isopropanol was used as a novel modifier in a hexane-acetonitrile based mobile phase for silver ion HPLC. Peak identification was based on HPLC-mass spectroscopy and selectivities of lipases. Positional isomers of TAGs containing one molecule of EPA, DHA, or DPA with saturated fatty acids (FAs) such as caprylic acid and palmitic acid were separated within 13 min using a gradient of hexane-isopropanol-acetonitrile as mobile phase. TAGs containing two or more EPA, DHA, or DPA were also separated from each other within 25 min, but their positional isomers were unresolved. The retention characteristics of the TAG were found to be related to the number of carbon atoms in the FAs present in addition to the number of double bonds and their isomeric configuration. One isomer with an unsaturated FA in the sn-2 position eluted faster than the other with the unsaturated FA in the sn-1 or 3 position. Species with longer chain FAs attached to TAGs with the same degree of unsaturation eluted faster than those that have shorter chain FAs. For example, docosapentaenoylhexadecanoyloctanoin (DPA/C16/C8) was eluted faster than dioctanoyldocosapentaenoin (DPA/C8/C8).
    Additional Material: 2 Ill.
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  • 107
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 373-378 
    ISSN: 0935-6304
    Keywords: Electrophoresis ; electrophoretic mobilities ; CZE ; MEKC ; peptides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---A computer model is presented for the prediction of the electrophoretic mobilities of peptides from physical constants derived from their amino acid sequences. The model assumes that the electrophoretic mobility can be represented by a product of four functions according to the relation:  lcomp= l(L)w(W)q(Q)c(CC), where L (a length parameter) is represented by the number of amino acid residues of the peptide, W (a width parameter) is represented by the average residue mass, Q = the charge of the peptide, and CC = the position of the center of charge relative to the center of mass. The model was used to calculate the electrophoretic mobilities of peptides in a 50 mM phosphate buffer at pH 2.5. Sixty-four test peptides ranging in size from 2 to 39 amino acid residues were used for this study. The calculated mobilities show excellent correlation with experimental measurements with a correlation coefficient greater than 0.98.
    Additional Material: 5 Tab.
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  • 108
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 386-390 
    ISSN: 0935-6304
    Keywords: Sulfur chemiluminescence detection ; sulfur simulated distillation ; boiling point distribution ; simultaneous FID/SCD analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A gas chromatographic system for the simultaneous acquisition of hydrocarbon and sulfur chromatograms was developed. Detection of sulfur compounds is achieved using a sulfur chemiluminescence detector (SCD) mounted in series with a flame ionization detector (FID). A constant fraction of the effluent of the FID is transferred to the SCD by means of a fixed restrictor. Unlike previous versions of this approach, the FID is not used to generate the chemiluminescent sulfur species. Rather, the FID is operated under optimum conditions for hydrocarbon analysis and a furnace is used to generate the chemiluminescent sulfur species. The system permits dual acquisition of the hydrocarbon and sulfur signals in a single analysis with a single column, since the detectors are operated in a serial fashion. The application of sulfur simulated distillation using this approach was examined, since this requires simultaneous universal and sulfur selective detection. Precision of absolute response of both the FID and SCD was typically less than 2% RSD for a standard reference material.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 109
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 391-394 
    ISSN: 0935-6304
    Keywords: REMPI-TOFMS ; laser mass spectrometry ; supersonic jet ; GC-MS ; interface ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The laser-based methods Laser Induced Fluorescence (LIF) and Resonance-Enhanced Multi-Photon Ionization (REMPI) can be used as highly selective detection modes for gas chromatography (GC). One major prerequisite for successful application of these detection methods is the availability of appropriate and reliable interfaces between the GC effluent and the molecular beam inlet. When a pulsed supersonic molecular beam (jet) source is used, the analyte molecules are efficiently cooled, allowing maximum selectivity of the laser spectroscopic detection methods. However, several technical problems have to be solved for practical realization of a GC-supersonic jet valve hyphenation. The pulsed jet interface should not interfere with the GC properties and the supersonic molecular beam properties. Further a good working cycle for the conversion from the continuously flowing GC current to the pulsed jet gas flow should be attained. This paper presents a novel setup of a GC-pulsed jet interface. The construction allows temporal and spatial compression of the analyte molecules in jet gas pulse and thus an increase of the detection sensitivity. Moreover, the GC effluent comes into contact only with glass surfaces and not with valve parts like plungers and seals. This reduces memory effects and sample decomposition. The valve setup is tested with a REMPI-TOFMS instrument.
    Additional Material: 2 Ill.
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  • 110
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 414-416 
    ISSN: 0935-6304
    Keywords: Selenium ; water ; SPME ; GC/MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---A method for the selective determination of Se4+ and Se6+ using solid phase microextraction (SPME) and GC/MS analysis is presented. Se4+ is selectively derivatized by reaction with 4,5-dichloro-1,2-phenylenediamine to form the corresponding piazselenolo complex, extracted by the SPME fiber, and determined by GC/MS. The RSD at a 5 μg/L concentration was 9.88% and the theoretical detection limit 6 ng/L. The method was employed to test real matrices; tap and river water were analyzed before and after spiking giving a recovery rate of 102% in river water and 97% in tap water.
    Additional Material: 3 Ill.
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  • 111
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 565-588 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Kovats retention index ; vapor pressure ; boiling point ; Wilson activity coefficient ; binary phase diagrams ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Non-ideal mixing in a dimethylsilicone stationary phase is modeled according to the Wilson activity coefficient. Pure liquid vapor pressures of alkylated compound series are calculated from capillary GLC retention with the functional group heat of solution in a polymer solvent. The new method uses the Kovats index, molar mass, and functional group to determine the bubble line of a compound. Boiling points at reduced and normal pressure are compared to literature values of 194 gasoline components. An unlike molecular pair interaction parameter is derived, using only bubble line data of the pure liquids. Binary phase diagrams are constructed and compared to vapor liquid equilibrium data.
    Additional Material: 22 Ill.
    Type of Medium: Electronic Resource
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  • 112
    ISSN: 0935-6304
    Keywords: Computer modeling of GC ; computer simulation of GC ; computer-assisted GC analysis ; GC multicolumn analysis ; heart cutting GC analysis ; computer-assisted column design ; computer-assisted selectivity tuning ; retention index mapping ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The analysis of four components in a mixture containing many possible interferents is simplified by heart-cutting serially connected columns containing stationary phases of widely different polarities. The design of the proper lengths of the two columns and timing the heart-cuts is accomplished with the aid of a computer simulation of the problem. The computer program calculates the proper lengths of column to produce the shortest analysis time and also outputs the predicted chromatograms from both columns. The chromatogram from the first column is used to construct the timing gates for the heart-cuts and the chromatogram from the second or analytical column is used to set integration gates for the selected compounds of interest.
    Additional Material: 7 Ill.
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  • 113
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 609-612 
    ISSN: 0935-6304
    Keywords: Cyclodextrins ; 2-p-toluidinyl-6-naphthalenesulfonate ; indirect fluorimetric detection ; liquid chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Cyclodextrins (CD's) were visualized by postcolumn mixing with 2-p-toluidinylnaphthalene sulfonate (TNS) in liquid chromatography. The indirect detection is based on fluorescence enhancement due to the formation of an inclusion complex between TNS and CD's. β-CD gave larger signal intensity than α- and γ-CD. Different selectivities were observed for alkyl-bonded silica stationary phases with different chain length.
    Additional Material: 7 Ill.
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  • 114
    ISSN: 0935-6304
    Keywords: Enantioselective multidimensional gas chromatography-mass spectrometry (enantio-MDGC-MS) ; methylcitric acid (MCA) ; inherited metabolic disease ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Methylcitric acid (2-hydroxybutane-1,2,3-tricarboxylic acid-MCA) is a structural analogue of citric acid, but due to an additional methyl group it is a chiral molecule with two stereogenic centers and thus four stereoisomers are conceivable. MCA occurs naturally as prominent metabolite in body fluids of patients with inherited metabolic diseases such as propionic acidemia, methylmalonic aciduria, or holocarboxylase synthetase deficiency. Therefore methylcitric acid is considered to be an important diagnostic marker for these diseases. MCA is most likely produced from accumulated propionyl-CoA in these diseases by the enzyme si-citrate synthase from the citric acid cycle; however, there are other enzymes known which could catalyze the same reaction with different stereoselectivity, such as re-citrate synthase or the more specific enzyme methylcitrate synthase, found in microorganisms. Almost all methods dealing with MCA in the literature are non-enantioselective. For that reason there is no information about occurrence of MCA enantiomers in healthy people, patients with propionic acidemia, methylmalonic aciduria, or holocarboxylase synthetase deficiency and about value of enantiomeric distribution for diagnosis and long-term treatment. The enantioselective analysis of MCA as corresponding trimethyl ester was achieved by enantioselective multidimensional gas chromatography coupled with mass spectrometry using heptakis-(2,3-di-O-methyl-6-O-tert-butyl-dimethylsilyl)-β-cyclodextrin as chiral stationary phase. The described method allows a reliable screening of MCA in complex matrices like urine without time consuming sample preparation and with mass selective detection. During this investigation urine samples from various patients and healthy controls were analyzed. As concluded, MCA is a good diagnostic marker and can be easily measured by the method presented. Only the two stereoisomers (2S,3R) and (2S,3S) were detectable in patients and healthy controls. The varying ratios of these stereoisomers cannot presently be correlated with the health status of patients, although there are some indications that this might be possible. However, the quantitative levels of MCA, determined as the ratio of MCA absolute peak area divided by 1,000 to the creatinine contents of urine samples in this investigation, showed a dependence on the state of health and MCA would thus also be a possible marker for long-term treatment. Such a substance is of major interest nowadays since there are different studies searching for such a long-term marker in propionic acidemia or methylmalonic aciduria.
    Additional Material: 4 Ill.
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  • 115
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 623-627 
    ISSN: 0935-6304
    Keywords: Supercritical fluid extraction ; hydrocarbons ; high temperature ; thermal desorption ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The extraction of n-alkanes, polyaromatic hydrocarbons (naphthalene, methylated naphthalenes, phenanthrene, methylated phenanthrenes, anthracene, and methylated anthracenes) and biomarkers (hopanes) from Posidonia shale by high temperature supercritical fluid (HT-SFE) carbon dioxide extraction has been evaluated, including the relative contributions from thermal desorption and relative comparisons to conventional Soxhlet extraction. These current results confirm those of previous studies indicating a widely differing extractability of strongly and weakly associated hydrocarbons in ancient sediments and the significantly higher recoveries possible using HT-SFE compared to conventional Soxhlet extraction. The present study also demonstrates that these high HT-SFE recoveries are due to true extraction rather than simple thermal desorption and that this procedure is a useful tool to study speciation as well as total extractable hydrocarbons from sediments.
    Additional Material: 2 Ill.
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  • 116
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 631-634 
    ISSN: 0935-6304
    Keywords: Dill ether ; stereoselective synthesis ; dill ether stereoisomers ; enantioselective multidimensional gas chromatography-mass spectrometry (enantio-MDGC/MS) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 2 Ill.
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  • 117
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 639-643 
    ISSN: 0935-6304
    Keywords: Cyclodextrin ; Halowax ; hexachloronaphthalene ; PCN ; polychlorinated naphthalenes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 3 Ill.
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  • 118
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 501-508 
    ISSN: 0935-6304
    Keywords: Fast GC ; film inefficiency factor ; high pressure drop ; thick film columns ; thin film columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The negative effect of the liquid stationary phase film thickness on the column efficiency is strongest for peaks with retention factors, k, in the vicinity of k = 0.3-0.4 and rapidly diminishes with the departure of k from that region. Additionally, at the high pressure drop required for fast analysis of complex mixtures, the negative effect of the same film thickness diminishes with the increase in column length, regardless of the k values. In practice, it is recommended to ignore the film thickness and optimize the columns as thin film ones regardless of their actual film thickness. Accounting for the film thickness results only in a modest improvement in the resolution for a few affected peaks - those with k = 0.3-0.4. However, this improvement comes at the cost of a substantial increase in analysis time, and should be used only as the action of the last resort.
    Additional Material: 4 Ill.
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  • 119
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 514-520 
    ISSN: 0935-6304
    Keywords: Solid-phase extraction ; high temperature - gas chromatography ; gas chromatography - mass spectrometry ; wax esters fennel seed oil ; caraway seed oil ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---A rapid method for the isolation and quantitative determination of wax esters in vegetable oils was developed. For the first time wax esters in oils were separated from the triglyceride matrix by means of solid-phase extraction, which allows rapid sample preparation in parallel and therefore a high sample throughput. The thus obtained wax ester fractions of fennel and caraway seed oils were analyzed by high temperature gas chromatography. GC-MS analyses were carried out using electron impact ionization in order to characterize the wax ester fraction. With respect to the results of the GC-MS analyses different isomers of saturated wax esters with the same carbon number were observed. Additional monounsaturated wax esters with an unsaturated fatty acid moiety were identified.
    Additional Material: 4 Ill.
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  • 120
    ISSN: 0935-6304
    Keywords: Clusia criuva Cambess ; counter-current chromatography ; flavonoids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The family Guttiferae belongs to the superorder Theiflorae, order Theales and according to Dahlgren's system of classification, it is equivalent to Hypericaceae (=Clusiaceae) [1]. This family consists of 49 genera encompassing over 1000 species of wide distribution in the tropics as shrubs and trees [2]. Plants of the genus Clusia have been used in folk medicine for the treatment of different kind of illness such as: febrifuge, anti rheumatic, purgative, for stomach problems and, in Brazil, they are very commonly used to heal wounds [3]. The key of any study of material from natural sources is the availability of suitable separation methods for the isolation of pure products [4-6]. Tentatives for separations using chomatography on solid support phases were not very efficients in the fractionation of Clusia criuva Cambess methanolic/ethyl acetate extracts. However, the use of counter-current chromatography, an all liquid technique, showed advantages in comparison with the more traditional liquid-solid separation methods and even with HPLC. In this sense it was possible to isolate flavonoid glycosides from ethyl acetate extract of Clusia criuva, in a very short operation time.
    Additional Material: 3 Ill.
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  • 121
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 541-546 
    ISSN: 0935-6304
    Keywords: Solvating gas chromatography ; gas chromatography ; fast separation ; pesticides ; herbicides ; aldehydes ; packed capillary columns ; polymer-encapsulated silica ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Rapid separations of selected environmentally important polar compounds using polymer-encapsulated silica stationary phases and a carbon dioxide mobile phase under solvating gas chromatography (SGC) conditions are reported. Ten underivatized short chain aldehydes and ten nitrogen-containing herbicides were separated within 1 min and 5 min, respectively, using a 30 cm×250 μm i. d. column packed with diol-bonded, polyethylenimine (PEI)-coated, and hexamethyldisilazane (HMDS)-end-capped silica particles (5 μm, 120 Å). Seven organophosphorus pesticides were resolved in less than 5 min using a 30 cm×250 μm i. d. column packed with polymethylhydrosiloxane-deactivated and SE-54 encapsulated silica particles. Separation numbers per unit time increased with pressure and temperature ramps. Both rapid pressure and temperature programming can be used to increase the speed of SGC. The effects of pressure and temperature on apparent retention factors of solutes with various polarities were investigated using diol-PEI-HMDS silica particles in SGC.
    Additional Material: 9 Ill.
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  • 122
    ISSN: 0935-6304
    Keywords: Liquid chromatography ; dead time ; multiparametric least-squares adjustment ; homologous series ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---In reversed phase liquid chromatography (RP-HPLC), the validity of a multiparametric non-linear least-squares regression iterative method for the determination of the column dead time tM and the regression parameter (slope b), based on the use of alkan-2-ones, alkyl aryl ketones, and 1-nitroalkanes has been evaluated. The determination of tM and b has been extensively studied for two mobile phase systems acetonitrile-water and methanol-water on seven octadecyl-C18 and one octyl C8 analytical columns. The calculated tM and b values were compared with those obtained by Guardino's and Grobler's methods. The influence exerted thereon by the nature of the homologous series, the mobile phase composition, and the packing materials were investigated.
    Additional Material: 5 Tab.
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  • 123
    ISSN: 0935-6304
    Keywords: SFE ; experimental design ; additives ; recycling ; polyolefins ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The performance and feasibility of supercritical fluid extraction (SFE) applied to the extraction of some antioxidants (Irganox 1076, Irgafos 168) and one UV-stabilizer (Chimassorb 81) from both virgin and recycled low density polyethylene (LDPE), and virgin high density polyethylene (HDPE) are studied. Due to the high number of variables a full-factorial design has been applied to minimize the number of experiments required to reach the optimum extraction conditions. Further analysis has been carried out off-line by reversed-phase HPLC. Modification of the physical properties of the polymeric matrix and increased number of recycling cycles as well as the influence of physical properties on the efficiency of SFE are also discussed.
    Additional Material: 1 Ill.
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  • 124
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 595-598 
    ISSN: 0935-6304
    Keywords: Xylitol ; samarium ; weak association ; equilibrium constant ; capillary electrophoresis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 1 Ill.
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  • 125
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    Journal of High Resolution Chromatography 22 (1999), S. 599-603 
    ISSN: 0935-6304
    Keywords: Capillary electrochromatography ; retention ; mixed stationary phases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Most commercially available instruments for capillary electrochromatography (CEC) have a fixed configuration and lack the flexibility to use shorter columns. Applying a blended stationary phase (a phase consisting of a given ratio of bare silica and reversed phase material) can simulate columns of different length in CEC. The goal of this work was to examine the effect of the degree of blending of reversed-phase columns (with bare silica) on the speed of the separation of neutral compounds in CEC. Optimum column packing mixture was determined from the variation of the solute retention factors as a function of the ratios of blending of reversed-phase and bare silica. By adjusting the column composition, solute retention factors and the analysis run time were halved when compared to a pure reversed-phase column of the same length. Stationary phase blending can be considered as an additional parameter to mobile phase variation, column temperature and applied electric field for the optimization of selectivity and analysis time. By adjusting the stationary phase composition, mobile phase composition, column temperature and applied electric field, the analysis run time of neutral components was decreased more than 75% when compared to a separation obtained on neat reversed-phase column of the same dimensions. The linear dependence of the retention factors as a function of the blend ratio (reversed phase/bare silica) offers a framework for designing a “blended” packed capillary column for CEC separations.
    Additional Material: 5 Ill.
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  • 126
    ISSN: 0935-6304
    Keywords: Liquid chromatography ; retention index ; multiparametric least-squares adjustment ; homologous series ; nitramines ; nitroaromatics ; aminoaromatics and nitrophenols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---In reversed phase liquid chromatography, the retention indices of some neutral and acidic explosives and related compounds (nitramines, nitroaromatics, aminoaromatics, and nitrophenols) based on the alkan-2-one, alkyl aryl ketone, and 1-nitroalkane retention index standards have been determined by the application of a new mathematical adaptation method, viz. a multiparametric least-squares regression iterative method. This method was applied to two types of columns. The first group includes six octadecyl-C18 columns with different packing materials and obtained from different manufacturers, while the second group comprises one octyl-C8 column. The retention indices have been extensively studied using either methanol-water or methanol-phosphate buffer mobile phase systems. The calculated multiparametric retention indices values were compared with those obtained by Guardino's, Grobler's, and Kovàts' methods. The influences of the concentration of the organic modifier in the mobile phase, aqueous mobile phase pH, and the column packing material on the retention indices of the explosives were also investigated. Good agreement was observed between the retention indices calculated by the use of the four mathematical methods for both neutral and acidic explosives.
    Additional Material: 4 Tab.
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  • 127
    ISSN: 0935-6304
    Keywords: Organochlorine compounds ; pesticides ; food analysis ; tomatoes ; GLC-ECD ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---A method is described for the simultaneous extraction and determination of twenty organochlorine pesticides residues [hexachlorocyclohexane (HCH) isomers (α, β, γ, δ), aldrin, dieldrin, endrin, heptachlor and its epoxide (HE), hexachlorobenzene (HCB), α-endosulfan, o,p′-DDD, p,p′-DDD, o,p′-DDE, p,p′-DDE, o,p′-DDT, p,p′-DDT, dicofol, methoxychlor, and mirex] that were spiked in tomatoes. Samples were extracted with ethyl acetate, and the extract was subjected to a rapid clean-up using a Florisil column. The residues were determined by GLC-ECD using two columns of different polarity. The calibration graph correlation coefficient ranged from 0.9903 to 0.9990. The recoveries ranged from 95 to 99% with relative standard deviation ranging from 0.5 to 14.7% in the concentration range 0.005 to 0.2 μg/g. The limits of detection ranged from 0.004 to 0.05 μg/g and the limits of quantification ranged from 0.005 to 0.174 μg/g.
    Additional Material: 1 Ill.
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  • 128
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    Journal of High Resolution Chromatography 22 (1999), S. 628-630 
    ISSN: 0935-6304
    Keywords: p-Nitrophenol ; urine ; SPME ; GC/MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 2 Ill.
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  • 129
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    Journal of High Resolution Chromatography 22 (1999), S. 635-638 
    ISSN: 0935-6304
    Keywords: High resolution gas chromatography ; thermal desorption ; archeological cosmetic powders ; PTV injector ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
    Additional Material: 5 Ill.
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  • 130
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    Journal of High Resolution Chromatography 22 (1999), S. 666-670 
    ISSN: 0935-6304
    Keywords: Capillary electrochromatography ; mixed packing technique ; electroosmotic flow ; retention mechanism ; fast analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mixed packing capillary electrochromatography (MP CEC) with the stationary phase comprising a physical mixture of strong cation exchange (SCX) phase and octadecysilyl (ODS) phase was developed. With the existence of a sulfonic acid group on the surface of SCX, not only could the electroosmotic flow (EOF) remain high at low pH, but also the hydrophilicity of the stationary phase was increased greatly, leading to broad adaptable ranges of both pH and organic modifier concentration in the mobile phase. At the same time, with the coexistence of C18 on the surface of ODS, both the retention and the resolution of samples were improved. Accordingly, MP CEC combined the advantages of both SCX and ODS columns. Effects of operation parameters on EOF and the capacity factors of solutes as well as the retention mechanism of such a column were studied systematically. In addition, MP CEC columns were used in the analysis of strong polar solutes as well as for the high speed separation of acidic, basic, and neutral compounds in a single run.
    Additional Material: 7 Ill.
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  • 131
    ISSN: 0935-6304
    Keywords: Enantioselective capillary gas chromatography ; chiral stationary phase ; chiral recognition mechanism ; cholic acid ; cyclocholates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The suitability of cyclocholates as chiral selectors in gas chromatography has been evaluated. We present the synthesis and characterization of two cyclocholates, viz. 3α,7α-diacetoxycyclo[3]cholate and 3α,7α-diacetoxycylo[4]cholate. Mixtures of these new selectors with polysiloxanes were tested as chiral stationary phases in capillary gas chromatography. Several enantiomer separations of common racemates were achieved with the 3α,7α-diacetoxycyclo[3]cholate at 10% in OV-1701 (w/w). It was shown that column efficiency was strongly dependent on temperature and that enantioselectivity was very sensitive to column conditioning. This chromatographic behavior suggested that cyclocholates were only dispersed in polysiloxane. Thus, it was assumed that chiral discrimination occurred via enantioselective adsorption interactions of enantiomers at the surface of the solid chiral selector dispersed in the polysiloxane matrix OV-1701.
    Additional Material: 11 Ill.
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  • 132
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    Journal of High Resolution Chromatography 22 (1999), S. 683-686 
    ISSN: 0935-6304
    Keywords: Vacuum gas oils ; packed column chromatography ; n-paraffins ; carbon number distribution ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Gas chromatographic methods are of widespread use in the petroleum industry for assessing petroleum and derivatives quality. The feedstocks for catcracking processes are very sensitive to the n-paraffin contents, which can be accurately determined using capillary column chromatography. Nevertheless, packed column chromatography does have potential advantages, viz. sometimes shorter analysis times, lower costs, higher column capacity, for vacuum gas oil analysis. This paper presents a method for such a determination using a Dexsil-300 packed column. The results obtained (n-alkane contents, carbon number distribution) agree fairly well with those obtained on a 30 m × 0.25 mm DB-1 fused silica capillary column.
    Additional Material: 3 Ill.
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  • 133
    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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  • 134
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    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.
    Additional Material: 3 Ill.
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  • 135
    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.
    Additional Material: 3 Ill.
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  • 136
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    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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  • 137
    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.
    Additional Material: 7 Ill.
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  • 138
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    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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  • 139
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    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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  • 140
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    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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  • 141
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    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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  • 142
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    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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  • 143
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    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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  • 144
    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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  • 145
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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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  • 146
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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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  • 147
    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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  • 148
    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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  • 149
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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
    Additional Material: 1 Tab.
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  • 150
    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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  • 151
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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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  • 152
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 153
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 154
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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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  • 155
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    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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  • 156
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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.
    Additional Material: 6 Ill.
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  • 157
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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.
    Additional Material: 3 Ill.
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  • 158
    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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  • 159
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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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  • 160
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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.
    Additional Material: 3 Ill.
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  • 161
    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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  • 162
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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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  • 163
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    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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  • 164
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    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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  • 165
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    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.
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  • 166
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    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.
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  • 167
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    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.
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  • 168
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    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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  • 169
    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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  • 170
    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.
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  • 171
    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).
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  • 172
    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.
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  • 173
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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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  • 174
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    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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  • 175
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    Biomedical Chromatography 9 (1995), S. i 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 176
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 177
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    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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  • 178
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    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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  • 179
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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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  • 180
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 2 Tab.
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  • 181
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    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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  • 182
    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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  • 183
    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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  • 184
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    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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  • 185
    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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  • 186
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
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  • 187
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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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  • 188
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
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  • 189
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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.
    Additional Material: 1 Ill.
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  • 190
    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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  • 191
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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.
    Additional Material: 3 Ill.
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  • 192
    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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  • 193
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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.
    Additional Material: 3 Ill.
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  • 194
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    Biotechnology and Bioengineering 48 (1995), S. 631-638 
    ISSN: 0006-3592
    Keywords: Saccharomyces cerevisiae ; fermentation ; on-line simulation ; state estimation ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: In order to study and control fermentation processes, indirect on-tine measurements and mathematical models can be used. In this article we present a mathematical on-line model for fermentation processes. The model is based on atom and partial mass balances as well as on equations describing the acid-base system. The model is brought into an adaptive form by including transport equations for mass transfer and unstructured expressions for the fermentation kinetics. The state of the process, i.e., the concentrations of biomass, substrate, and products, can be estimated on-line using the balance part of the model completed with measurement equations for the input and output flows of the process. Adaptivity is realized by means of on-line estimation of parameters in the transport and kinetic expressions using recursive regression analysis. These expressions can thus be used in the model as valid equations enabling prediction of the process. This makes model-based automation of the process and testing of the validity of the measurement variables possible. The model and the on-line principles are applied to a 3.5-L laboratory tormentor in which Saccharomyces cerevisiae is cultivated. The experimental results show that the model-based estimation of the state and the predictions of the process correlate closely with high-performance liquid chromatography (HPLC) analyses. © 1995 John Wiley & Sons, Inc.
    Additional Material: 7 Ill.
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  • 195
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    Biotechnology and Bioengineering 48 (1995), S. 659-666 
    ISSN: 0006-3592
    Keywords: methanogenic activity ; ethylene ; dechlorination ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Kinetics were determined for methanogenic activity and chlorinated ethylene dehalogenation by a methanol-enriched, anaerobic sediment consortium. The culture reductively dechlorinated perchloroethylene (PCE) to trichloroethylene (TCE), 1,1-dichloroethylene (1,1-DCE), vinylchloride (VC), and ethylene and ethane. The absence : of methanol or the addition of 2-bromoethanesulfonic. acid in the presence of methanol suppressed both methanogenic activity and dechlorination. In contrast, acetate production continued in the presence of 2-bromoethanesulfonic acid. These results suggest that dechlorination was strongly linked to methane formation and not to acetate production. A kinetic model, developed to describe both methanogenesis and dechlorination, successfully predicted experimentally measured concentrations of biomass, methane, substrate, and chlorinated ethylenes. The average maximum specific dehalogenation rates for PCE, TCE, 1,1-DCE, and VC were 0.9 ± 0.6, 0.4 ± 0.1, 12 ± 0.1, and 2.5 ± 1.7 μmol contaminant/ g. DW/day, respectively. This pattern for dechlorination rates is distinctly different than that reported for transition metal cofactors, where rates drop by approximately one order of magnitude as each successive chlorine is removed. The experimental results and kinetic analysis suggest that it will be impractical to targeting methanol consuming methanogenic organisms for in situ ground-water restoration. © 1995 John Wiley & Sons, Inc.
    Additional Material: 4 Ill.
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  • 196
    ISSN: 0006-3592
    Keywords: bovine serum albumin ; growth factor ; hollow-fiber culture ; perfusion culture ; antibody production rate ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The effects of the high-molecular-weight growth factors, transferrin and bovine serum albumin (BSA), on antibody production were analyzed quantitatively in continuous hollow-fiber cultivation over a period of 60 days. Transferrin enhanced cell growth but had no significant effect on the specific antibody production rate, whereas BSA significantly enhanced antibody production. The antibody production rate was increased 4- and 14-fold respectively by feeding BSA at 2 and 5 g L-1 into the EC side of the system (the side connected to the cell-containing outer part of the hollow-fiber unit) compared with the production achieved without BSA. Addition of 5 g L1 BSA into the IC side of the system (the side connected to the inner part of the hollow-fiber unit) resulted in a 2.5-fold increase in the antibody production rate. The effect of BSA was also analyzed using the perfusion culture system with a separation unit. When fresh medium containing either 2 or 5 g L-1 BSA was fed into the reactor, both the specific growth rate and specific death rate increased, while the specific antibody production rate was increased 2- and 25-fold, respectively, by feeding BSA at these two concentrations compared with no addition. Comparing the two systems, the increase in the antibody production rate achieved with the hollow-fiber system was threefold greater than that in the perfusion culture system with the same concentration of BSA feeding. © 1995 John Wiley & Sons, Inc.
    Additional Material: 9 Ill.
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  • 197
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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
    Type of Medium: Electronic Resource
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  • 198
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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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  • 199
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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
    Type of Medium: Electronic Resource
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  • 200
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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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