高效液相色谱法直接拆分泮托拉唑钠对映体

首次使用Kromasil CHI-TBB手性柱在正相条件下直接拆分了泮托拉唑钠对映异构体,考察了流动相组成、酸碱调节剂用量以及流速对对映体分离的影响。优化后的分析条件为:流动相组成为正己烷-异丙醇-乙酸(体积比为95∶5∶0.1)混合溶液,流速2.0 mL/min,柱温25 ℃。所建立的方法具有柱效高、简便快捷及重复性好等优点。     

高效液相色谱法直接拆分非甾体解热镇痛药物对映体

使用Kromasil CHI-TBB手性固定相,分离了非甾体解热镇痛药卡洛芬,氟吡洛芬,非诺洛芬,酮洛芬,吡咯芬和萘普生等对映体。结果表明,这种以酒石酸二酰胺为手性中心的商业化手性固定相,适合于在正相条件下分离上述药物对映体,对映体分离因子和分析时间可以通过向流动相中添加极性物质如异丙醇,甲基叔丁醚等来进行调节。     

高效液相色谱法直接分离单环β-内酰胺对映体

本文介绍在一种手性固定相(键合在硅胶上的(R)-N-3,5-二硝基苯甲酰苯甘氨酸固定相)上一系列取代单环β-内酰胺对映体的直接分离,考察了流动相组成对容量因子k’,对映体选择性α和峰分离度P的影响,比较了具有不同取代基的β-内酰胺对映体的分离。     

薄层色谱法拆分手性药物对映体

用性能稳定的薄层色谱用β-环糊精(β-CD)、硅胶手性固定相拆分手性药物对映体.在适当比例的乙腈-1%乙酸三乙胺(TEAA)、己烷-异丙醇、乙腈-甲醇-乙酸-三乙胺、甲醇-1%TEAA及乙腈-1%TEAA-三乙胺溶剂系统中展开,8种临床常用的手性药物对映体得到有效分离,对映异构体之间的相对比移值α为1.53～4.89.     

反相高效液相色谱法直接拆分舒必利对映体

以反相高效液相色谱法,建立了舒必利在大环抗生素类固定相(chirobiotic T)上手性拆分的方法。考察了不同流动相组成对分离的影响。推荐流动相条件为V(甲醇)：V(磷酸)：V(三乙胺)=100：1．5：3。     

联苯类对映体在直链淀粉类手性固定相上的高效液相色谱法直接拆分

 涂敷直链淀粉 三 (3,5 二甲基苯基氨基甲酸酯 )于自制的球形氨丙基硅胶上 ,制备了手性固定相。用该固定相直接拆分了一系列外消旋联苯类保肝药物 ,考察了一系列伯醇 (乙醇、正丙醇、正丁醇 )和异丙醇等流动相改性剂对保留和立体选择性的影响 ,讨论了固定相对样品的作用机理。     

高效液相色谱法拆分硅氟唑对映体

在纤维素-三-(3,5-二甲基苯基氨基甲酸酯)(Chiralcel OD-H)手性柱上对硅氟唑对映体的分离进行了研究.考察了流动相中改性剂的种类和浓度、流速以及柱温对分离效果的影响,并对手性拆分机制进行了讨论.实验结果表明:5种醇改性剂中,异丙醇的改性效果最佳,当异丙醇含量为2%时,分离度(Rs)达最大值10.19;在...     

脲型手性固定相高效液相色谱拆分苯基琥珀酸对映体

苯基琥珀酸(PSA)是药物原料N 甲基 α 苯基琥珀酰亚胺(phensuximide)的重要中间体。(S) ( ) PSA是一种很好的扑尔敏药物手性拆分剂,并可作为手性选择子合成液相色谱手性固定相[1]。外消旋的PSA通常采用光活性的番木鳖碱或(-) 脯氨酸化学衍生结晶拆分[2,3]。PSA对映体的高效液相色谱(HPLC)拆分未见文献报道。1　实验部分　　仪器　美国TSP公司HPLC仪:3500 3200型高压梯度泵,UV2000型双波长紫外吸收检测器,Rheodyne7725i进样阀,PC1000色谱工作站。PE341型旋光仪。　　试剂　正己烷、1,2 二氯乙烷、乙醇、三氟乙酸,均为国产分…     

直链淀粉手性固定相高效液相色谱法拆分比索洛尔对映体

采用直链淀粉手性固定相高效液相色谱法在正相条件下直接拆分了比索洛尔对映异构体。分别以异丙醇、乙醇为有机改性剂,考察了流动相的组成与配比、流速及柱温等因素对比索洛尔对映体分离的影响。确定了比索洛尔对映体的最佳拆分条件:流动相正己烷-乙醇-二乙胺(体积比为88∶12∶0.1),流速0.6 mL/min,检测波长270 nm,柱温20 ℃。该方法可快捷、简便地拆分比索洛尔对映体。     

农药甲霜林对映体的高效液相色谱分离及手性拆分热力学研究

以正己烷/异丙醇为流动相，在纤维素-三（3，5-二甲基苯基氨基甲酸酯）（CDMPC）涂敷型手性固定相上，对农药甲霜灵外消旋体进行了拆分，考察了流动相组成、柱温等对甲霜灵对映体的保留和分离的影响；对甲霜灵R、S对映体与固定相之间的保留和分离的热力学机理进行了讨论。     

(2S,3S)-1,2-环氧基-3-叔丁氧酰胺基-4-苯丁烷的合成

以(S)-苯丙氨酸为原料,经氨基保护、与对硝基苯酚成酯后与硫叶立德反应制得(S)-1-氯-3-叔丁氧酰胺基-4-苯基-2-丁酮(3);3经Meerwein-Poondrf-Verley还原、环合等反应合成了HIV-1蛋白酶抑制剂的关键中单体——(2S,3S)-1,2-环氧基-3-叔丁氧酰胺基-4-苯丁烷,总收率约45%,其结构经1H NMR和MS确证。     

Resolution of enantiomers by HPLC on cellulose derivatives

Summary Various polysaccharide derivatives, particularly cellulose derivatives, were synthesized and used as chiral stationary phases for optical resolution by HPLC after being adsorbed on macroporous silica gel. Cellulose triacetate (CTA-II), which was synthesized under homogeneous conditions, showed a chiral recognition ability for many racemates. Other cellulose derivatives such as cellulose tribenzoate (OB), cellulose-trisphenylcarbamate (OC), cellulose tribenzyl ether (OE), and cellulose tricinnamate (OK) also showed unique chiral recognition. Among other polysaccharide derivatives, curdlan triacetate was also exhibited an effective chiral recognition. Presented at the 15th International Symposium on Chromatography, Nürnberg, October 1984     

Resolution of enantiomers of ketoprofen by HPLC: a review

Today, a heightened awareness of the applicability of enantiomers in medicine and clinical practice has been gene-rated due to the continuous evolvement of the field of chirality. In this context, this article provides a review of separation of ketoprofen, an important drug, in a popular class of non-steroidal anti-inflammatory drugs (i.e. profens). This review highlights various methodologies, logistical considerations for separation and provides an exhaustive list of applications mainly focusing on the pharmacokinetic aspects. Clearly, the application of enantioselective methods for drug racemates paves the way to understand the in vivo behavior of individual enantiomer and hence an opportunity for an alternate and/or better option for treating the disease.     

Resolution of enantiomers of a series of chiral alkoxy-modified phthalocyaninato nickel(II) complexes by enantioselective HPLC

We have resolved the enantiomers of a series of chiral modified metallophthalocyaninato complexes of nickel bearing alkoxy groups at the 14 and 28 positions on what would otherwise be a normal phthalocyaninato ligand and conforming to the general formula [14,28-(RO)(2)Pc]Ni(ii), where R = Me, Et, or n-Pr. The complex for which R = n-Pr is reported here for the first time. Resolution of the enantiomers of these complexes was accomplished via HPLC utilizing an immobilized carbohydrate-based stationary phase, resulting in baseline resolution of peaks corresponding to enantiomers of the complexes, with R(s) values in excess of five. Isolation of milligram quantities of the complexes bearing methoxy and n-propoxy groups in high enantiomeric excess has been achieved via semi-preparative-scale HPLC on the same stationary phase. Resolved samples of these compounds do not appear to racemize at an appreciable rate, nor do they readily exchange alkoxy groups with alcohols while stirring in alcoholic solution. The spectroscopic details and the crystallographically-determined solid-state structure for the complex where R = n-Pr are reported, and are highly similar to those that have been observed for the previously reported analogues. It has been shown by NMR that the chirality and C(2) molecular symmetry of the complex bearing n-propoxy groups is maintained in solution.     

高效液相色谱法分离2-(4-羟基苯氧基)丙酸酯的对映体

采用高效液相色谱法在手性柱上分离芳氧基苯氧基丙酸类除草剂中间体(±)-2-(4-羟基苯氧基)丙酸酯的对映体。实验结果表明,在三苯甲酸纤维素酯的手性柱上,以无水乙醇为流动相能较好地分离(±)-2-(4-羟基苯氧基)丙酸乙酯和甲酯,其分离因子α值分别为1.44和1.29;同时还发现在三苯甲酸纤维素酯的手性柱上2-取代芳氧基或芳基丙酸酯结构中的酯基团的大小对其对映体的分离有明显的影响,其中以乙基为最佳。并通过对照试验证实了2-(4-羟基苯氧基)丙酸乙酯的右旋体先流出,其左旋体后流出。     

Hydrolysis Reactions and Resolution of (±)-2-Acetamido-3-hydroxy-1-(4-nitrophenyl)-1-propanone

IntroductionChloramphenicol,which was isolated fromStreptomyces venezuelae in 1 947[1] ,is used as abroad- spectrum antibiotic possessing activityagainst many Gram- negative and Gram- positivemicroorganisms. (± ) - 2 - Acetamido- 3 - hydroxy- 1 -(4- nitrophenyl) - 1 - propanone[(± ) - 1 ]is one of theintermediates of producing chloramphenicol.Petrow et al.[2 ] reported some transformations of(± ) - 1 in hydrolysis reactions. However,thereaction products were complicated under multiplehydr…     

A short and convenient chemoenzymatic synthesis of both enantiomers of 3-phenylGABA and 3-(4-chlorophenyl)GABA (Baclofen)

Both enantiomers of the pharmacologically active GABA analogues 4-amino-3-phenyl and 4-amino-3-(4-chlorophenyl)butyric acid (Baclofen) with high enantiomeric excesses were synthesized by a chemoenzymatic method involving α-chymotrypsin mediated kinetic resolutions of the corresponding 3-phenyl- and 3-(4-chlorophenyl)-4-nitrobutyric acid methyl ester precursors.     

Resolution of racemic 2-isobornyl-4-methylphenol into enantiomers

Resolution of racemic 2-isobornyl-4-methylphenol into enantiomers was performed following its transformation into diastereomers by the reaction with (1S)-camphanoyl chloride.