氰戊菊酯立体异构体在手性键合相上的分析

本文介绍了采用高效液相色谱法在(R)-N-3,5-二硝基苯甲酰苯甘氨酸手性键合相上氰戊菊酯的四个立体异构体的分离,以外消旋氰戊菊酯样品为参照,计算了光学活性氰戊菊酯样品的四个立体异构体的百分含量,确定了在手性键合相上氰戊菊酯四个立体异构体构型的流出顺序为SR→RS→SS→RR。     

Liquid chromatographic enantiomer resolution of N-fluorenylmethoxycarbonyl alpha-amino acids and their ester derivatives on polysaccharide-derived chiral stationary phases

The liquid chromatographic enantiomer separation of N-fluorenylmethoxycarbonyl (FMOC) protected alpha-amino acids and their ethyl ester derivatives was performed on polysaccharide-derived chiral stationary phases, Chiralcel OD, Chiralpak AD, and Chiralpak AS. In general, Chiralcel OD and Chiralpak AD showed good performance for resolution of N-FMOC alpha-amino acids and their ethyl esters, respectively. All investigated N-FMOC alpha-amino acid enantiomers were baseline separated on Chiralcel OD or Chiralpak AD, whereas N-FMOC alpha-amino acid ethyl ester enantiomers were baseline resolved (alpha = 1.15-3.03) on Chiralpak AD, except for two analytes. The L-enantiomers of all examined FMOC alpha-amino acid ethyl ester derivatives are preferentially retained on Chiralpak AD, while the elution orders of the other enantiomer separations are not consistent.     

用两种相似多糖类手性固定相拆分阿托品外消旋对映体的比较

分别涂敷纤维素-三（3，5-二甲基苯基氨基甲酸酯）（CDMPC）与直链淀粉-三（3，5-二甲基苯基氰基甲酸酯）（ADMPC）于自制的球形氨丙基硅胶上，制备了两种多糖类手性崮定相。用高效液相色谱法（HPLC）在正相条件下，用两种固定相直接拆分了阿托品（atmpine）外消旋体、在正己烷中加入了不同的醇类改性剂对阿托品进行拆分，并优化了流动相中醇类改性剂的比例：结果发现，阿托品在CDMPC固定相上可以得到基线拆分，而在ADMPC固定相上只能得到部分拆分。     

手性高效液相色谱法测定1—（6‘—甲氧基萘）乙醇不对称氢酯基化反应

在自制的硅基纤维素－三（３，５－二甲基苯基氨基甲酸酯）高效液相色谱手性固定相上（ＨＰＬＣ－ＣＳＰ），优化了１－（６＇－甲氧基萘）乙醇氢酯基化反应产物－萘普生甲酯手性分离的条件，测定了相应的一系列不对称氢酯基化反应产物的对映体过剩值（ｅ．ｅ．值）。结果表明，在ＣＤＭＰＣ－ＣＳＰ手性柱上用ＨＰＬＣ测定此类不对称催化反应的光学产率，评价催化剂体系的手性选择是一种非常理想的方法。     

HPLC of synthetic polymers characterization of polystyrenes by high performance precipitation liquid chromatography (HPPLC)

Summary The advantages and disadvantages of high performance precipitation liquid chromatography have been demonstrated for polystyrene homopolymers. Depending on the mobile phase composition at the dissolution point of the polymeric sample and surface properties of the stationary phase, elution is governed either by a solution process or by adsorption. A contribution by adsorption was noticed on silica as well as on reversed phases based on silica with a normal phase gradient of increasing polarity (heptane to dichloromethane). Elution was solely governed by solubility of the polymers on both types of stationary phase for polystyrenes with a molecular weight above 35 000 and reversed phase gradient of decreasing polarity (methanol to dichloromethane). Under these conditions an identical dependence of elution solvent composition on sample size was found as for turbidity titrations. Due to differences in the velocity of the eluent front and the polymeric sample with porous stationary phases the polymers can be eluted as colloidal solutions Non-porous stationary phases are superior in this respect because the velocities of eluent and solutes are identical.     

High performance liquid chromatographic separation of dipeptide and tripeptide enantiomers using a chiral crown ether stationary phase

A chiral stationary phase (CSP) based on (-)-(18-crown-6)-2,3,11,12-tetracarboxylic acid was evaluated for the direct resolution of the enantiomers of dipeptides and tripeptides. The type and concentration of the acid and the methanol content were optimized with regard to retention time and resolution using Ala-Phe as model peptide. A mobile phase consisting of 10 mM sulfuric acid in 70% aqueous methanol was applied to the separation of a set of 16 structurally diverse dipeptides and tripeptides. Generally, the configuration of the amino acid at the N-terminus determined the enantiomer elution order. With a few exceptions the LL- and LD-enantiomers interacted stronger with the CSP compared to the corresponding DD- or DL-enantiomers. The experimental conditions also allowed the simultaneous separation of all four stereoisomers of Ala-Phe. Addition of ammonium sulfate generally reduced retention times and enantiomer resolution. Addition of triethylamine as modifier led to an overall increase of the retention times while the resolution did not show a general trend, increasing in the case of Ala-Ala but decreasing in the case of Ala-Phe.     

Crystal hydrates: an investigation of the use of crystal hydrates as stationary phases in gas chromatography

Summary The use of crystallohydrates, crystallohydrate solutions and melts as stationary phases in gas chromatography has been proposed. Crystallohydrates have been shown to display high selectivity in the separation of polar organic compounds when use is made of water vapours as the mobile phase. Some aspects of gas-liquid chromatography in water vapours and with the stationary phase comprising crystallohydrates have been studied, and the preliminary results obtained point to the desirability of further progress in this field.Presented at the 14th International Symposium on Chromatography London, September, 1982     

高效液相色谱蛋白质手性固定相

本文综述了近年文献中已报道的各种高效液相色谱蛋白质（酶）手性固定相及其在手性拆分中的应用，并阐述了蛋白质作为手性选择剂拆分机理的研究进展。     

Analysis of nitro-PAHs in diesel exhaust particulate extracts with multicolumn HPLC

Summary A method is described for the determination of nitrated polynuclear aromatic hydrocarbons (nitro-PAHs), in particular 1-nitropyrene, in diesel particulate extracts. The method employs a multidimensional HPLC (column switching) technique with final on-line peak identification by UV-VIS spectral comparison with standards. To achieve exceptional chromatographic selectivity for nitro-PAHs, a new pyrene butyric acid amide phase has been prepared which is capable of forming donor-acceptor complexes with them. With this technique it is possible to confirm the presence of 1-nitropyrene in the range 3–100 ng/mg on filter-collected diesel soot. Its utility was demonstrated with diesel exhaust extracts spiked with varying levels of 1-nitropyrene and proved to be highly selective.Parts of this work have been presented at the 15th International Symposium on Chromatography, Nürnberg, October 1984.Dedicated to Prof. J. F. K. Huber at the occasion of his 60th birthday.