一种氯法拉滨及其对映异构体的分离测定方法

本发明公开了一种氯法拉滨及其对映异构体的分离测定方法,本发明采用高效液相色谱法,分离测定氯法拉滨及其对映异构体,可用于氯法拉滨和含有氯法拉滨的药物组合物的质量控制。     

一种替格瑞洛对映异构体、非对映异构体的分离检测方法

本发明涉及一种替格瑞洛对映异构体(A)、非对映异构体(B,C)分离检测的方法,该方法以纤维衍生物为填充剂的色谱柱为手性色谱柱,低级烷烃与低级醇混合液为流动相,通过高效液相色谱法对替格瑞洛对映异构体(A)、非对映异构体(B,C)进行分离鉴定。该分离检测方法能将替格瑞洛与其异构体进行有效的分离,进而高效的控制替格瑞洛原料药和其制剂产品的质量。本检测方法具有较高的准确度和精密度,耐用性强,可用于替格瑞洛原料药及制剂的研发和生产过程中质量控制。     

拟除虫菊酯混合制剂中非对映异构体的HPLC分离与测定

研究了高胺菊酯和苯醚氰菊酯的非对映异构体反相高效液相色谱的分析方法，选用紫外检测器，通用的ＯＤＳ－Ｃ１８色谱柱，甲醇＋水为流动相，在选定的梯度洗脱色谱条件下，高胺菊酯和苯醚氰菊酯的顺反非对映异构体得到完全分离。该法快速简便，重现性好，可同时完成混合物中顺反非对映异构体的含量及总量的定量分析。     

α-CF_3芳香仲醇类对映体的高效液相色谱法分离

利用正相高效液相色谱法在一种纤维素衍生物手性固定相(OJ-H或OD-H)上成功分离了一系列(23个)α位取代的CF3芳香醇及其酯化后的对映异构体。通过考察流动相组成、流速、进样浓度和温度等因素对对映体分离的影响,优化色谱分离条件,并且利用得到的数据计算出对映异构体的分离因子和分离度。     

高效液相色谱环糊精键合固定相

环糊精是由Ｄ（＋）－葡萄糖单元通过α－１，４糖苷键连接的环状齐聚糖，其最典型的性质是能与许多客体分子形成包容配合物。高效液相色谱环糊精键合固定相广泛用于对映异构体，非对映异构体，结构异构体和常规化合物的分离。     

3，5-二硝基苯甲酰化β-环糊精键合硅胶手性固定相的合成及高效液相色谱中的手性分离研究

合成了3,5-二硝基苯甲酰化β-环糊精键合硅胶手性固定相,并用红外光谱和X射线光电子能谱进行了表征.制备了相应的高效液相色谱柱,在高效液相色谱中,考察了该手性柱的柱效和对于一些位置异构体和对映异构体的手性分离能力.结果表明,该固定相对于一些位置异构体和对映异构体具有较好的分离能力.     

高效液相色谱手性固定相的研究Ⅴ——二肽叔丁酰胺型手性固定相拆分α-氨基酸、二茂铁基氨基酸及二肽衍生物对映异构体

]本文应用高效液相色谱(L，L)-二肽叔丁酰胺型键合硅胶手性固定相拆分N-乙酰基--氨基酸甲酰、N-乙酰基--二茂铁基丙氨酸乙酯及N-叔丁氧羰驶基亮氨酰亮氨酸甲酯等对映异构体、结果表明：部分固定相对氨基酸衍生物对映异构体有拆分效果；大部分固定相对二茂铁基丙氨酸衍生物对映异构体有较好拆分效果；所有固定相对由（D，D）-及（L，L）-亮氨酰亮氨酸衍生物构成的外消旋体均有良好的拆分效果，分离系数最高达1.79。本文对部分化合物对映异构体的拆分机制进行了初步探讨。     

高效液相色谱手性固定相的研究Ⅴ——二肽叔丁酰胺型手性固定相拆分α-氨基酸、二茂铁基氨基酸及二肽衍生物对映异构体

 ]本文应用高效液相色谱(L，L)-二肽叔丁酰胺型键合硅胶手性固定相拆分N-乙酰基--氨基酸甲酰、N-乙酰基--二茂铁基丙氨酸乙酯及N-叔丁氧羰驶基亮氨酰亮氨酸甲酯等对映异构体、结果表明：部分固定相对氨基酸衍生物对映异构体有拆分效果；大部分固定相对二茂铁基丙氨酸衍生物对映异构体有较好拆分效果；所有固定相对由（D，D）-及（L，L）-亮氨酰亮氨酸衍生物构成的外消旋体均有良好的拆分效果，分离系数最高达1.79。本文对部分化合物对映异构体的拆分机制进行了初步探讨。     

(S)-与(R)-五味子丙素的HPLC手性分离及质谱研究

建立了一种反相高效液相色谱法分析(S)-和(R)-五味子丙素对映异构体的方法.选用Chiralcel OD-RH手性色谱柱,以甲醇和水(体积比78 : 22、97 : 3)为流动相,流速0.5 mL/min,254 nm波长下检测,五味子丙素合成中间体噁唑啉取代联苯对映异构体2和2'的保留时间分别为22.2 min和19.9 min,分离度为2.5,五味子丙素对映异构体3'和3的保留时间分别为7.5、9.0 min,与相邻杂质峰分离度分别为3.2和2.7.经液相色谱-质谱实现了分离与鉴定.方法灵敏度高、重复性好,可用于五味子丙素对映异构体的立体选择性研究及质量控制.     

苯丙氨酸酯类衍生物对映异构体的拆分

利用手性Ｃｈｉｒａｌｃｅｌ ＯＤ柱高效液相色谱对一系列苯丙氨酸酯类衍生物对映异构体进行了拆分，获得了良好的分离结果。讨论了化合物的结构对拆分效果的影响。     

高效毛细管电泳分离手性物质

本文对近年来发展起来的高效毛细管电泳技术（ＨＰＣＥ）在手性分离方面的工作做了评述，讨论了高效毛细管电泳手性对映体的分离方式和定量方面，并对在这一重要领域中可能的发展趋势做了展望。     

Enantiomeric separation of citalopram analogues by HPLC using macrocyclic glycopeptide and cyclodextrin based chiral stationary phases

The enantiomeric separation of a novel series of twenty-eight racemic mixtures of citalopram analogues was performed by high performance liquid chromatography (HPLC). Due to the effectiveness of citalopram as an antidepressant drug, the development of new compounds based on its chemical structure is interesting, and their enantiomeric separation is needed to allow further pharmacokinetic studies. Several bonded cyclodextrin (both native and derivatized) and macrocyclic glycopeptide based chiral stationary phases (CSPs) were evaluated for their ability to separate this set of compounds via HPLC. Polar ionic, polar organic, and reversed phase modes were tested. Twenty-five of the racemic mixtures were separated with resolutions and enantiomeric selectivities up to 2.9 and 1.33, respectively. A total of eighteen baseline separations were achieved, while seven compounds were partially separated. Vancomycin based columns operated in the polar ionic mode resulted in the greatest number of separations. Lastly, the chromatographic behaviors of similar compounds were compared based on their chemical structure and also on the chiral selectors used.     

高效毛细管电泳离子分析

高效毛细管电泳是近年来发起来的一种高效、快速的新型分离技术，在分析化学和生物医学中有着广泛的应用，它可以分析从离子到分子，从小分子到生物大分子的一系列化合物。离子型化合物的分离测定是其中的一个重要领域，其中包括无机和有机阴阳离子、生物分子、形态与价态，以及表面活性剂的分析等方面内容，本文对这些方面作一概述。     

高效毛细管电泳分离中的化学平衡

在高效毛细管电泳（ＨＰＣＥ）中缓冲对分离有重要影响，缓冲中的化学平衡决定了待测组分的存在状态或形态，从而决定了组分的电泳尚度，淌度的差异是ＨＰＣＥ分离之基础，因此，溶液化学平衡在ＨＰＣＥ分离中起着重要作用，本文综述了电泳淌度，ＨＰＣＥ分离与化学平衡的关系，并要介绍了电泳淌度与酸碱平衡，络合平衡的关系，从化学平衡的角度，讨论了酸碱性化合物，金属离子，对映异构体等几大类化合物的ＨＰＣＥ分离。     

Separation of some amino acids by supercritical fluid chromatography after a pre-derivatization step with classical reagents

Summary The separation of polar compounds by supercritical fluid chromatography is a difficult problem to solve. In this work, we have used a pre-derivatization method to obtain apolar or less polar compounds. Amino acids have been chosen as model polar compounds of biological interest, and 9-fluorenylmethyl chloroformate (FMOC) and (+)-1-(9-fluorenyl)ethyl chloroformate (FLEC) have been used as derivatizating reagents.With this procedure, the amino acids studied have been separated in less than 40 minutes with a good efficiency. Furthermore, with FLEC reagent, the enantiomeric separation was rapid in comparison with liquid chromatography techniques and the selectivities obtained were in the same order of magnitude.     

Enantiomeric separation of ketoconazole and terconazole antifungals by electrokinetic chromatography: Rapid quantitative analysis of ketoconazole in pharmaceutical formulations

EKC using a neutral CD as chiral selector was applied in this work to the development of a method enabling the enantiomeric separation of ketoconazole and terconazole antifungals. The influence of different experimental conditions such as temperature, CD concentration, pH, and nature and concentration of the buffer on the enantiomeric resolution of the compounds studied was investigated. The use of 10 mM heptakis-(2,3,6-tri-O-methyl)-beta-CD in a 100 mM phosphate buffer (pH 3.5) with a temperature of 15 degrees C allowed the separation of the enantiomers of ketoconazole and terconazole with high resolution (R(s) > 2.0). The rapid separation of ketoconazole enantiomers with an analysis time less than 3 min was carried out after fitting some experimental parameters. The developed method was applied to the determination of ketoconazole in different pharmaceutical formulations.     

用超分子化学观点研究毛细管电泳法拆分十八甲基炔诺酮

以超分子化学观点作ＨＰＣＥ手性选择剂的理论基础，研究ＨＰＣＥ法分离十八甲基炔诺酮对映体，讨论了操作条件对分离的影响，使十八甲基炔诺酮对映异构体达基线分离。     

Enantiomeric distribution of major chiral volatile organic compounds in juniper‐flavored distillates

The enantiomeric ratios of chiral volatile organic compounds in juniper‐flavored spirits produced by various processing technologies in different EU countries were determined by multidimensional GC using solid‐phase microextraction and liquid–liquid extraction as a sample pretreatment procedure. In total, more than 260 compounds were detected in studied spirits from which linalool, α‐terpineol, 4‐terpineol, linalool oxides, α‐pinene, and verbenone were selected for enantiomeric separation. The significant differences in enantiomeric ratio of linalool and cis‐linalool oxide allowed us to distinguish between samples produced in Slovakia and the United Kingdom from those produced in Germany, Czech Republic, and Belgium. The pure enantiomer of trans‐linalool oxide was found only in samples from Germany. It was shown that the enantiomeric ratio is independent of the sample treatment procedure, and only small differences up to 1% were observed.     

Enantiomeric separations by means of nano‐LC

Enantiomers represent a class of compounds extensively investigated since they can show totally different behaviors when they interact with a chiral environment. Because of their identical chemical structure (they differ only in the spatial arrangement of the atoms in the molecule), the separation of optical isomers is a challenging task of analytical chemistry. So far employed methods for the separation of enantiomers are mainly based on chromatography. CE as well was considered as an analytical technique suitable for chiral separations, characterized by high efficiency and low consumption of reagent. Recently, miniaturization was introduced in LC to answer the needs to perform analyses in the minimum time, to use the smallest amount of samples and to reduce environmental pollution. Nano‐LC represents nowadays a valid alternative to the abovementioned conventional analytical techniques, and can be advantageously exploited for enantiomeric separation especially because it needs minute amounts of the chiral material necessary to carry out enantiomeric separations. This review describes the development and applications of nano‐LC in the field of chiral separations. The data reported in literature show its relevance for the study enantiomers‐chiral selectors interaction, as well as for application in pharmaceutical and clinical research.     

毛细管电泳在农药分析中的应用

 综述了高效毛细管电泳技术在农药分离方面的应用及发展状况 ,包括各种不同分离模式和手性选择剂的选择 ,另外还指出了该方法的优点及其发展方向。参考文献 5 0篇。