药物分析(Ⅱ)

对国内(不含港、澳、台地区)药物分析在2008至2009年的主要进展进行综述。内容包括高效液相色谱法、气相色谱法、毛细管电泳法、薄层色谱法、分光光度法和其它分析方法等。另外,对高效液相色谱法和气相色谱法的不同联用技术进行分别评述。共引用文献3392篇。     

药物分析（Ⅰ）

对国内药物分析在2005~2006年的主要进展进行评述。内容包括高效液相色谱法、气相色谱法、毛细管电泳法、薄层色谱法、分光光度法和其它分析方法等。另外,对高效液相色谱法和气相色谱法的不同联用技术进行分别评述。共引用文献3294篇。     

药物分析 (Ⅱ)

对国内药物分析在2005~2006年的主要进展进行评述。内容包括高效液相色谱法、气相色谱法、毛细管电泳法、薄层色谱法、分光光度法和其它分析方法等。另外,对高效液相色谱法和气相色谱法的不同联用技术进行分别评述。共引用文献3294篇。     

色谱在天然产物活性物质筛选中的应用

高效的活性筛选方法是新活性物质发现的关键。从筛选活性物质的角度,综述了近年来薄层色谱、高效液相色谱在天然产物活性物质筛选方面应用中的最新研究进展及其发展前景。共引用文献30篇。     

Separation of Bufotalin and Cinobufotalin by Preparative Liquid Chromatography

Abstract

Complete resolution of bufadienolides by traditional column chromatography, or by thin-layer chromatography (TLC), is quite difficult. Separation of various bufadienolide conjugates by high performance liquid chromatography (HPLC) has been described, but not for resolution of the corresponding genins. A preparative HPLC procedure has been developed for resolving the difficultly separable bufotalin (1) and cinobufotalin (2). A Lobar B column packed with LiChromprep Si-60 was used to separate these bufadienolides employing a recycling procedure.     

Correlation of TLC,HPTLIC and PMD Results and Their Transfer to HPLC Systems

Abstract

The correlation of the results of five thin-layer chromatographic techniques and their transfer to high performance liquid chromatography are reported. The data obtained indicate that high performance thin-layer chromatographic results are faithfully reproduced by high performance liquid chromatography. Although plates were not activated, and mixed solvents were used, no major differences were observed between thin layer and high performance liquid chromatography.     

Chromatographic analysis and purification of multiply tritium-labelled eicosanoids

This is a comparative study of different chromatographic techniques [gas-liquid (GLC), thin-layer (TLC), liquid (LC), high-pressure liquid (HPLC) chromatography] as applied to the analysis and preparative purification of tritium-labelled eicosanoids with a molar radioactivity of 1.8–8.8 TBq/mmol obtained by selective hydrogenation and by chemical or enzymic methods. We demonstrate the possibility of analyzing reaction mixtures and isolating individual multiply labelled eicosanoids with a chemical and radiochemical purity of 95–98%. Special features of HPLC for high molar radioactivity eicosanoids are considered.     

植物皂甙测定方法的进展

对从1979年至2005年期间植物皂甙的测定方法的进展作了评述。内容主要涉及薄层色谱法、气相色谱法、高效液相色谱法（HPLC）、HPLC与其他方法联用及毛细管电泳等,引用文献35篇。     

Determination of cortisol in guinea pig urine by high performance thin-layer chromatography, high performance liquid chromatography, and thin-layer chromatography/radioimmunoassay

Summary In order to collect urinary samples from unrestrained guinea pigs, animals were kept in their familiar home cages with wood shavings for bedding. Cortisol was removed from shavings by a simple washing step, and an attempt was made to measure its concentrations by high performance thin-layer chromatography (HPTLC), high performance liquid chromatography (HPLC), or thin layer chromatography/radioimmunoassay (TLC-RIA). After intramuscular administration of 25 mg cortisol, cortisol excretion increased from about 20–30 μg/day to 400–500 μg/day (HPTLC: 531 μg/day, HPLC: 493 μg/day; TLC-RIA: 394 μg/day). Similarly, the treatment of the animals with 20 IU ACTH resulted in an augmented cortisol excretion, with mean values of 294 μg/day (HPTLC), 256 μg/day (HPLC) and 143 μg/day (TLC-RIA), respectively. The present study shows, for the first time, that cortisol excretion in unrestrained laboratory animals can be determined. Whilst the cortisol values measured by HPTLC and HPLC agree, the amounts measured by TLC-RIA were significantly lower. These differences are probably due to the presence of substances in urine or shavings which interfere with the radioimmunological determination. Hence, cortisol should be determined either by HPTLC or HPLC. Beside having a desirable specificity, these methods are more suited than TLC/RIA for steroid analysis since they confer the possibility of measuring additional steroids (e.g. precursors and/or metabolites of cortisol) in a single urine extract. This is especially the case for the HPTLC method since substances can be transformed into fluorescent derivatives.     

Separation of peptides on Empore thin-layer chromatography sheets and blotting onto polyvinylidene difluoride membranes with subsequent gas phase sequencing.

Methods for the separation of peptides on a new type of thin-layer chromatography (TLC) sheet and blotting onto polyvinylidene difluoride (PVDF) membranes with subsequent gas phase sequencing are described. For validation, the A and B chain of insulin were chromatographed on Empore TLC sheets and either extracted or blotted onto PVDF membranes. The advantages and disadvantages of thin-layer chromatography on Empore sheets versus high performance liquid chromatography (HPLC) are discussed, along with the possibility of combining the two methods. In addition, TLC was combined with electrophoresis (fingerprinting) for the separation of complex peptide mixtures. Blotting from TLC sheets onto PVDF membranes was performed in two ways: contact diffusion and electrophoretic transfer. In our experiments electroblotting was more effective. Amino acid sequence determination of the B chain of insulin was possible both after extraction from the TLC sheet and after blotting onto PVDF membranes. In the former case, liquid phase sequencing and, in the latter case, gas phase sequencing was performed. The possibility to blot from TLC sheets onto membranes, e.g. PVDF, may prove useful in many fields, for example in biochemistry, and in molecular and cell biology.     

Chromatographic identification of pesticides

The chromatographic properties of 51 common pesticides have been measured using seven different chromatographic systems involving gas-liquid chromatography (GLC), high-performance liquid chromatography (HPLC) with diode-array spectrophotometric detection and thin-layer chromatography (TLC) with different spray reagents. Correlation coefficients were calculated for combinations of all systems. The best combination of the chromatographic systems examined for the identification of an unknown compound is GLC on OV-17, HPLC on ODS-Hypersil with acetonitrile-water as eluent and TLC using an isooctane-ethyl acetate solvent system.     

Determination of theophylline in serum by high performance liquid chromatography/mass spectrometry with atmospheric pressure chemical-ionization (APCI HPLC/MS)

 A method for the determination of theophylline (TH), without derivatization, in serum by isotope dilution mass spectrometry using labelled [1, 3-¹⁵N₂-2-¹³C]theophylline (LTH) as internal standard is described. After deproteinization, the analyte is directly injected into a high performance liquid chromatography – mass spectrometer operating with atmospheric-pressure chemical-ionization (APCI HPLC/MS). The concentrations of TH in sera measured by APCI HPLC/MS are compared with results from gas chromatography – isotope dilution mass spectrometry (GC-ID/MS), high performance liquid chromatography (HPLC) and fluorescence polarization immunoassay (FPIA). The accuracy, precision and recovery of the APCI HPLC/MS and GC-ID/MS methods are discussed. The coefficient of variation (CV) determined from duplicate samples was less than 2%. The detection limit was 10 ng/ml at a signal-to-noise ratio of 3:1. Received: 17 January 1996/Revised: 26 March 1996/Accepted: 5 April 1996     

Simultaneous Determination of Carbinoxamine,Pholcodine, and Ephedrine in Antitussive Preparation by High-Performance Liquid Chromatography and Thin-Layer Chromatography-Densitometry

JPC – Journal of Planar Chromatography – Modern TLC - Simple, accurate, precise, sensitive, and validated high-performance liquid chromatography (HPLC) and thin-layer chromatography...     

Micro-HPLC/TLC/FTIR

Identification problems often encountered in high performance liquid chromatography (HPLC)/Fourier transform infrared spectrometry (FTIR) can be circumvented through the use of a thin-layer chromatographic (TLC) plate as deposition and infra-red sampling medium. The combination of complementary separation modes is shown to demonstrate increased resolution of the components of complex mixtures. In this particular work, the effluent from a reversed-phase microcolumn is continuously deposited on a TLC plate with alumina stationary phase. The solute remains on the plate as a continuous record of the HPLC separation, which is then analyzed by diffuse reflectance FTIR. When the HPLC separation is inadequate for full separation of the components, the immobilized HPLC chromatogram serves as a starting point for subsequent TLC separation. A number of FTIR reconstructed chromatograms and spectra which are derived from the TLC plate aid in the interpretation.     

(R)‐N,N,N‐Trimethyl‐2‐Aminobutanol‐Bis(Trifluoromethane‐Sulfon)Imidate Chiral Ionic Liquid Used as Chiral Selector in HPCE,HPLC, and CGC

Abstract

In this work, the (R)‐N,N,N‐trimethyl‐2‐aminobutanol‐bis(trifluoromethanesulfon)imidate chiral ionic liquid was first used in chromatography and exhibited a excellent chiral recognition ability in high performance capillary electrophoresis (HPCE), high performance liquid chromatography (HPLC), and capillary gas chromatography (CGC), which also showed for the first time that chrial ionic liquid was an effective chiral selector in HPCE and HPLC. The compounds that have been separated using this chiral ionic liquid at least included alcohol, amine, acid, and amino acid, et al. enantiomers. As the chiral ionic liquid can be easily synthesized from relatively inexpensive materials, it should have a great potentiality for chiral separation in chromatographic science.     

Improvement of chemical analysis of antibiotics. X. Determination of eight tetracyclines using thin-layer and high-performance liquid chromatography

Analytical methods for eight tetracyclines (TCs) were established using silica gel high-performance thin-layer chromatography (HPTLC), reversed-phase thin-layer chromatography (RP-TLC) and high-performance liquid chromatography (HPLC). Good separations of eight TCs were obtained using chloroform-methanol-5% disodium ethylenediaminetetraacetate solution (65:20:5) (lower layer) and methanol acetonitrile 0.5 M oxalic acid solution (1:1:4) (pH 3.0) on silica gel HPTLC and C8 TLC plates, respectively. A combination of HPTLC and RP-TLC made possible the identification of the eight TCs. Each calibration graph was linear between 0.1 and 1.0 microgram using UV densitometry except for rolitetracycline. For detection reagents, the diazonium salts including Fast Violet B gave variously coloured spots with the eight TCs and good sensitivities were obtained except with minocycline. In HPLC, the simultaneous analysis of the eight TCs on a C8 column was possible using methanol-acetonitrile-0.01 M oxalic acid solution (1:1.5:7) adjusted to pH 3.0 as the mobile phase. A linear relationship was obtained between 1.0 and 10 ng using the usual sample preparation except for rolitetracycline. The direct determination of rolitetracycline was possible using tetrahydrofuran, dimethyl sulphoxide and the mobile phase as solvents for preparation of the sample. For the determination of residual rolitetracycline, it was effective to measure the amount of rolitetracycline as tetracycline by HPLC, HPTLC and RP-TLC after conversion of rolitetracycline to tetracycline by incubating for 5 min in methanol at 50 degrees C.     

Chromatographic methods as tools in the field of mycotoxins

Achievements in the applications of chromatographic techniques in mycotoxicology are reviewed. Historically, column chromatography (CC) and paper chromatography (PC) were applied first, followed by thin-layer chromatography (TLC), high-performance liquid chromatography (HPLC) and gas chromatography (GC). Although PC techniques are no longer used in the analysis of mycotoxins, selected applications of PC are included to underline historical continuity. The most important achievements published from 1980 onwards are described. They include clean-up methods, TLC, CC, HPLC and GC of mycotoxins in environmental samples, foods, feeds, body fluids and in studies on biosynthesis and biotransformations of mycotoxins. Advantages and disadvantages of chromatographic techniques used in mycotoxicology are also evaluated.     

反相液相色谱法制备纯化柠檬苦素类似物配糖体

 利用反相制备液相色谱结合吸附树脂柱色谱和离子交换色谱方法 ,从甜橙种子的提取物中纯化制备了一种柠檬苦素类似物配糖体 ,经 NMR测定为奥巴叩酮配糖体。     

Separation of a Homologous Series of Long-Chain Fatty Alcohols (C49-C58) From Mycobacterium Tuberculosis H37Ra by High Performance Liquid Chromatography

Abstract

Fatty alcohols were obtained from the saponified chloro-form-methanol extract of Mycobacterium tuberculosis H37Ra by extraction with diethyl ether and partially purified by silicic acid column chromatography. The long-chain fatty alcohols (C₄₉-C₅₈) were separated from the shorter-chain alcohols by Sephadex LH-20 column chromatography and further fractionated into saturated and unsaturated alcohols by argentation thin-layer chromatography. These two fractions were analyzed by proton nuclear magnetic resonance spectro-scopy, derivatized to the 3,5-dinitrobenzoyl esters, and fractionated on a C₁₈-bonded silica column by high performance liquid chromatography (HPLC). Complete separation of esters differing by two carbon units and partial separation