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Summary A method to determine free amino acids by pre-column derivatization with phenylisothiocyanate is discussed. The method has been applied to determine free amino acids in wine samples, and the results have been compared with those obtained by means of an automatic orthophthal-aldehyde-9-fluorenylmethyloroformate (OPA-FMOC) method. 相似文献
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G. Liu 《Chromatographia》1995,40(1-2):99-101
Summary Acetophnone, a substance stable at room temperature, is readily oxidizes in a high temperature open tubular liquid chromatographic system by the residual oxygen in the mobile phase. The oxidation product is less UV absorptive and detection sensitivity decreases greatly. To prevent the oxidation, through degassing of the mobile phase is necessary. 相似文献
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High performance liquid chromatography of disaccharides on a porous graphitic carbon column applying post-column derivatization with benzamidine 总被引:1,自引:0,他引:1
Summary A sensitive post-column fluoresence method based on the reaction of reducing sugars with a fluorigenic reagent (benzamidine) under alkaline conditions and elevated temperature is described. Optimum reaction conditions suitable for the detection of fluorescent reaction products have been investigated. A porous graphitized carbon column (shandon Hypercarb) was employed as the chromatographic solid phase and elution was isocratic by an aqueous acetonitrile mixture.A special problem in sugar analysis is the tendendy of anomer formation giving doublet peaks. This tendency varies largely among the different sugars, and systematic studies on conditions that eliminate this problem were performed. Efficient and selective separations of a series of disaccharides were obtained using high temperatures and a low concentration of acetonitrile in the mobile phase. The detection limits (S/N=3) with an injection volume of 20 L ranged from 10–60 picomoles. Linear calibration graphs were obtained in the 2–20 M concentration range (r
2>0.99). A relative standard deviation between 1–3% (n=6) demonstrated good precision of the developed system.Deceased July 21, 1996 相似文献
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Summary A novel method is described for the determination of paracetamol (acetaminophen;N-acetyl-4-aminophenol) in urine. After reversed-phase HPLC separation, paracetamol is oxidized by H2O2 with horseradish peroxidase catalysis. Detection is performed fluorimetrically at an excitation wavelength of 329 nm and
an emission wavelength of 435 nm. Urine samples were spiked with paracetamol, diluted, and injected directly without further
pretreatment. Under these conditions, the limit of detection was 2×10−8 molL−1, and the limit of quantification was 7×10−8 molL−1. The method was validated by two different approaches based on HPLC with UV-Vis detection. 相似文献
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Summary An improved method for the quantitative determination of amino acids using HPLC, after preliminary derivatisation with o-phthalaldehyde, is described. Separation was carried out on a LiChrospher RP-18 column, using gradient elution and a fluorescence detector. Hydrolysis was performed with 6M HCl or with 3M p-toluenesulphonic acid depending on the amount of carbohydrates in the sample. In addition, the time required for total hydrolysis was shortened from 24 hours to 15 minutes by the use of a microwave oven. The results with these two hydrolytic methods are compared with regard to the extent of peptide bond cleavage and the percentage of decomposition of amino acids in a test mixture. 相似文献
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Summary L-N-(3,5-dimethoxyoxybenzoyl)isoleucine, ionically bonded to γ-aminopropyl silica, has been tested as a chiral stationary
phase for the separation of racemates by HPLC. The phase shows good selectivity towards different types of racemates and in
particular for those having an electron-poor aromatic group in their molecule. The separation of benzoin racemate can be achieved
on the developed chiral phase with an α value of 1.10. 相似文献
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A. Péter G. Török G. Tóth W. Van Den Nest G. Laus D. Tourwé D. W. Armstrong 《Chromatographia》1998,48(1-2):53-58
Summary High-performance liquid chromatographic and gas chromatographic methods were developed for the separation of unusual secondary
aromatic amino acids. Amino acids containing 1,2,3,4-tetrahydroisoquinoline, 1,2,3,4-tetrahydronorharmane-1-carboxylic acid
and 1,2,3,4-tetrahydro-3-carboxy-2-carboline moieties were synthetized in racemic or chiral forms. The high-performance liquid
chromatography was carried out either on a teicoplanin-containing chiral stationary phase or on an achiral C18 column. In the latter case the diastereomers of the amino acids formed by precolumn derivatization with the chiral reagents
2,3,4,6-tetra-O-acetyl-β-D-glucopyranosyl isothiocyanate or 1-fluoro-2,4-dinitrophenyl-5-L-alanine amide were separated. The gas chromatographic
analyses were based on separation on a Chirasil-L-Val column.
Presented at: Balaton Symposium on High-Performance Separation Methods, Siófok, Hungary, September 3–5, 1997 相似文献
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Summary The chromogenic reagent 4-phenylazobenzyloxycarbonyl chloride (PAZ-Cl) was used for the automated pre-column derivatization of amino acids (AAs) at ambient temperature followed by liquid chromatographic separation of the derivatives formed.Since in previous investigations it was realised that the selectivity of a C-18 stationary phase decreased after 40 injections of PAZ-AAs the suitability of 12 reversedphases distinguished by silica modification, carbon content, and particle characteristics was tested. Among these columns only a polymer-coated C-18 stationary phase furnished satisfactory repeatability of retention times for 250 analyses. 相似文献
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柱前衍生高效液相色谱法测定减肥药中的芬氟拉明 总被引:3,自引:0,他引:3
建立了柱前衍生反相高效液相色谱—紫外检测方法用于测定减肥药中的芬氟拉明。样品用三氯甲烷萃取,异丙醇转溶,再在四氢呋喃中和60℃下,用苯异氰酸酯衍生35min,然后用甲醇/水(72/28,V/V)为流动相和Kromasil C18分离柱,在240nm检测衍生物。方法的线性范围在2.52—126mg/L(r=0.9994),检出限和定量限分别为0.36ng(S/N=3)和1.2ng(S/N=10),平均回收率为98.4%,相对标准偏差(RSD)小于3.00%。 相似文献
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Summary The use of 2-bromoacetyl-6-methoxynaphthalene as a fluorogenic labelling reagent in pre-column derivatization for the HPLC separation of biologically active carboxylic acids (fatty acids and bile acids) has been investigated. The compound reacts (30 min. at 70°C) with carboxylic acids to give fluorescent esters that can be separated by reversedphase HPLC and detected at ex. 300 nm, em. 460 nm. The experimental conditions for the derivatization and chromatographic separation are discussed. Applications to the determination of valproic acid and chenodeoxycholic acid in pharmaceutical formulations are described. 相似文献
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Summary A method is presented that enables the fully automated precolumn derivatization of mixtures of DL-amino acids (DL-AA) witho-phthaldialdehyde together withN-isobutyryl-L(orD)-cysteine. HPLC on a 250 mm×4 mm i.d. column packed with Shandon Hypersil ODS, 5 μm, and a linear gradient
formed from 23 mM sodium acetate (pH 6.0) and methanol/acetonitrile (600 ml+50 ml) separates completely an AA standard composed
of 17 pairs of DL-AA (including Asn and Gln), Gly and the internal standard L-homo-Arg, within 75 min at a flow rate at 1 ml/min. Applications are shown of the determination of free D-AA isolated from an
orange juice concentrate and from soy sauce, and the detection of D-AA in a gelatine total hydrolysate. In the case of these
foodstuffs fluorescence detection (excitation at 230 nm, emission at 445 nm) allows the routine detection of 5–10 pmol per
AA; and approx. 0.2–1% D-AA, in an excess of L-AA, are quantifiable.
Presented in part at the “International Symposium on Separation of Peptides, Proteins and Polynucleotides”, October 29–31,
1990, Wiesbaden (abstract 620), ANAKON '91, April 22–24, Baden-Baden (abstract C 5), and at the “15th International Symposium
on Column Liquid Chromatography”, June 3–7, 1991, Basel (abstract P26/2). 相似文献
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A microwave-assisted extraction procedure using water as extractant has been performed for the extraction of acid herbicides
(namely, bentazone, 2,4-D, trichlopyr, 2,4,5-T and 2,4,5-Tp) from different types of soil. Two experimental designs were used
for the optimization of the leaching step. The selection of water as extractant provided a clean approach by avoiding the
use of organic solvents. The use of water also enhanced the extraction efficiency due to the high interaction of the microwave
irradiation with polar solvents. The time required for total removal of the target compounds was 35 min. The recoveries yield
were from 87.64 to 106.14% with a repeatability (expressed as relative standard deviation) ranging between 1.34 and 9.24%.
A within-laboratory reproducibility, also expressed as relative standard deviation, varied from 3.97 to 10.41%. A flow-injection
manifold allowed automation of the whole process by hyphenating the steps subsequent to extraction (namely, filtration, preconcentration,
chromatographic separation and UV detection) for the determination of the analytes. 相似文献
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Simultaneous separation and identification of hashish constituents by coupled liquid chromatography-mass spectrometry (HPLC-MS) 总被引:1,自引:0,他引:1
C. Rustichelli V. Ferioli F. Vezzalini M. C. Rossi G. Gamberini 《Chromatographia》1996,43(3-4):129-134
Summary This paper reports the use of liquid chromatography for the separation and determination of the major cannabinoids extracted from hashish samples. The direct coupling to the mass spectrometer enables the selective identification both of neutral and acidic cannabinoids. The developed method does not require any preliminary derivatization and should, therefore, be of interest in forensic analysis for simple and unequivocal determination of hashish constituents.Part of this work was presented at the 2nd Italian-Spanish Joint Meeting of Medicinal Chemistry, 30 August–3 September 1995, Ferrara, Italy. 相似文献
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Summary One possible method of characterizing chemicall-modified stationary phases is to describe their chromatographic properties. In this study we investigated several chemically-modifiedpolystyrene-divinylbenzene packings for the separation of nitroarenes, polycyclic aromatic hydrocarbons and aminosubstituted aromatic hydrocarbons. Chromatography was carried out on commercially available polymer stationary phases, for example C-18 or vinylpyridine modified polystyrene. In addition, a chemically-immobilized polymer packing was prepared by introducing nitrogroups, which were established by elemental analysis and infrared spectroscopy. 相似文献
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C. Brenier-Maurel C. Delaurent G. Pages M. -C. Guilhem A. M. Siouffi 《Chromatographia》2002,56(5-6):277-282
Summary An optimization procedure for the separation of flavonoids from St John's Wort by reversed-phase high-performance liquid chromatography
on monolithic stationary phase is described. Three-component mobile phase systems are studied using experimental design methodology.
The starting experimental domain is a triangle, each vertex of which is a pure component. From preliminary isocratic experiments,
truncations in the domain are performed leading to a quadrilateral shape working domain with no symmetry. To cope with both
separation and analysis time, desirability functions are used. Optimal conditions are finally given by binary systems and
the four flavonoids are separated in less than seven minutes. 相似文献
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Summary A rapid and simple liquid-chromatographic method has been developed for on-line quantification of amphetamine in biological
fluids. Untreated samples (20 μL) are injected directly into the chromatographic system and purified on a 20 mm×2.1 mm i.d.
pre-column packed with 30 μm Hypersil C18 stationary phase. After clean-up the analyte is transferred to the analytical column (125 mm×4 mm i.d., 5 μm LiChrospher
100 RP18) for derivatization and separation using a mixture of acetonitrile and the derivatization reagent (o-phthaldialdehyde andN-acetyl-L-cysteine) as the mobile phase. The experimental conditions for on-line derivatization and resolution of the amphetamine
have been optimized, and the results have been compared with those obtained by derivatizing the analyte in pre-column mode.
The method described has been applied to the determination of amphetamine in plasma and urine. Good linearity and reproducibility
were obtained in the 0.1–10.0 μg mL−1 concentration range, and limits of detection were 25 ng mL−1 and 10 ng mL−1 with UV and fluorescence detection, respectively. The procedure described is very simple and rapid, because no off-line manipulation
of the sample is required; the total analysis time is approximately 8 min. 相似文献
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Summary A number of 11 triazine herbicides and 7 of their corresponding metabolites were separated in a single HPLC run. The separation
was achieved on a reversed-phase column using gradient elution with acetonitrile/buffer. Detection was by UV absorption at
a wave-length of 220 nm. 相似文献