使用二元环糊精体系毛细管电泳法分离手性药物

采用高效毛细管区带电泳法，分别以羟丙基-β-环糊精（HP-β-CD）和高磺化-β-环糊精（HS-β-CD）及二者混合物为手性选择剂，研究了5种药物的对映体分离，并取得很好的对映体分离结果。比较了HP-β-CD和HS-β-CD手性识别能力，分析了二元环糊精体系的“协同效应”。     

Borate Complexation and Mixed Cyclodextrin Additives for Chiral Separation of Propranolol and Its Metabolites by Capillary Electrophoresis

A buffer system of borate with charged (carboxymethyl-β-CD) and uncharged (β-CD) cyclodextrins (CDs) was employed in the chiral resolution and separation of propranolol and its selected major metabolites. By appropriate choice of buffer and additive conditions, chiral resolution of all of the compounds studied was achieved in a single analysis, where near baseline resolution was found for the difficult to resolve propranolol-glycol (Pr-glycol). This has not been observed in previous studies of propranolol and its metabolites.     

水溶性β-环糊精衍生物的合成及其在毛细管电泳中的应用

研究了七(2, 6-二-O-羧甲基)-β-环糊精(羧甲基-β-CD)和七{2, 6-二-O-[3-(1, 3-二羧基丙氨基)-2-羟丙基]}-β-环糊精(谷氨酸-β-CD)两种水溶性环糊精衍生物的合成及在毛细管电泳中的应用,结果表明它们具有较好的水溶性, 并且对异丙嗪和扑尔敏有较好的分离效果。     

亲和毛细管电泳技术及其应用

对近几年新发展起来的亲和毛细管电泳技术（ACE）的原理、分类及方法作了简要介绍,着重介绍了亲和毛细管区带电泳、毛细管亲和凝胶电泳、胶束电动色谱中的亲和电泳、亲和毛细管等电聚焦、亲和探针毛细管电泳等过程和方法。对ACE在分子生物学、生物化学中的应用及该技术在亲和常数测定、核酸片段识别、竞争免疫分析、药物先导化合物的筛选等方面的应用也作了介绍。     

手性药物的毛细管电泳拆分

以氧氟沙星、扑尔敏、特布它林和普萘洛尔为手性药物,分别采用羟丙基-β环糊精(HP--βCD)、羟丙基-β-环糊精结合羧甲基-β-环糊精(HP--βCD/CM--βCD)作手性拆分试剂,考察环糊精浓度和pH对手性选择性的影响。结果发现环糊精提供手性相互作用,而pH强烈地影响这种相互作用。以HP--βCD/CM-β-CD组成的双环糊精系统能更好地优化手性选择性,而通过调节pH可以获得需要的分离选择性、迁移次序。     

胶束电动毛细管色谱法拆分肾上腺素对映体

胶束电动毛细管色谱法拆分肾上腺素对映体;电化学检测;对映体拆分     

毛细管电泳及其质谱联用技术分析重组人促红细胞生成素

用高效毛细管电泳测定了重组人促红细胞生成素（ｒｈＥＰＯ）的微多相性、肽图，同时采用毛细管电泳质谱联用技术鉴定了部分非糖基化胰酶消解片段和Ｏ－１２６糖基化肽的结构。方法简便、快速，适用于ｒｈＥＰＯ半成品的质量控制。     

纳米技术在毛细管电泳和微流控芯片电泳生物大分子分离中的应用*

在分离领域,纳米技术主要以两种形式改善分离效果,一种是利用金、二氧化硅、聚合物、金属氧化物和碳纳米管等纳米材料,二是通过微机电加工、化学方法或者自组装技术构筑纳米障碍物和纳通道等纳米结构。本文对两种不同形式的纳米技术在毛细管电泳和微流控芯片电泳生物分离中的应用进行了综述。并对该领域未来的发展进行了展望。     

Comprehensive Profiling by Non-targeted Stable Isotope Tracing Capillary Electrophoresis-Mass Spectrometry: A New Tool Complementing Metabolomic Analyses of Polar Metabolites

Mass spectrometry (MS) driven metabolomics is a frequently used tool in various areas of life sciences; however, the analysis of polar metabolites is less commonly included. In general, metabolomic analyses lead to the detection of the total amount of all covered metabolites. This is currently a major limitation with respect to metabolites showing high turnover rates, but no changes in their concentration. Such metabolites and pathways could be crucial metabolic nodes (e.g., potential drug targets in cancer metabolism). A stable-isotope tracing capillary electrophoresis–mass spectrometry (CE-MS) metabolomic approach was developed to cover both polar metabolites and isotopologues in a non-targeted way. An in-house developed software enables high throughput processing of complex multidimensional data. The practicability is demonstrated analyzing [U-¹³C]-glucose exposed prostate cancer and non-cancer cells. This CE-MS-driven analytical strategy complements polar metabolite profiles through isotopologue labeling patterns, thereby improving not only the metabolomic coverage, but also the understanding of metabolism.     

The Use of Dual Cyclodextrin Chiral Selector Systems in the Enantioseparation of Pharmaceuticals by Capillary Electrophoresis: An Overview

Cyclodextrin (CD) derivatives are the most efficient and frequently used chiral selectors (CSs) in capillary electrophoresis (CE). There are situations when the use of a single CD as CS is not enough to obtain efficient chiral discrimination of the enantiomers; in these cases, sometimes this problem can be resolved using a dual CD system. The use of dual CD systems can often dramatically enhance enantioseparation selectivity and can be applied for the separation of many analytes of pharmaceutical interest for which enantioseparation by CE with another CS systems can be problematic. Usually in a dual CD system an anionic CD is used together with a neutral one, but there are situations when the use of a cationic CD with a neutral one or the use of two neutral CDs or even two ionized CDs can be an efficient solution. In the current review we present general aspects of the use of dual CD systems in the analysis of pharmaceutical substances. Several examples of applications of the use of dual CD systems in the analysis of pharmaceuticals are selected and discussed. Theoretical aspects regarding the separation of enantiomers through simultaneous interaction with the two CSs are also explained. Finally, advantages, disadvantages, potential and new direction in this chiral analysis field are highlighted.     

环糊精衍生物作为气相色谱固定相的发展及应用

从环糊精及其衍生物作为气相色的分离机理出发介绍了影响这固定相的因素及其分离应用的近期发展,共评述56篇文章。     

毛细管电泳手性分离进展*

评述了近年来毛细管电泳手性分离的进展。以各种手性选择剂的发展为线索介绍了毛细管电泳手性分离理论、方法及应用。简要说明了分离中应注意的一些关键问题。     

毛细管电泳法手性拆分合成药物氨氯地平及其中间体

 建立了毛细管电泳手性拆分氨氯地平药物中间体的方法 ,并同时拆分了氨氯地平。考察了不同手性拆分试剂对手性选择性的影响 ,其中羧甲基 β 环糊精 (CM β CD)能够给出满意的拆分结果。在以CM β CD为手性拆分试剂的基础上 ,还考察了各种因素诸如流动相的pH值、环糊精的浓度以及电压对分离的影响。最佳拆分条件为 :30mmol/L磷酸盐 +5 0mmol/LCM β CD(pH 6 12 )。在此条件下 ,药物中间体及氨氯地平的分离度分别为 1 5 5和 1 73,结果令人满意。     

毛细管电泳-电感耦合等离子质谱联用的接口设计

描述了毛细管电泳电感耦合等离子体质谱(CE-ICP-MS)联用技术的单T型接口,自行设计了双T型接口,并对两接口的分析性能作了比较。解决了接口中的常见问题,使用节流阀减小自吸作用并降低了CE分离物的稀释倍数,排气阀使提升量保持稳定。经考察得知,采用自吸作用提升液流流量稳定,其重现性RSD小于5％;双T型接口较单T型接口对CE分离更有利。采用双T型接口联用时,CE分离La、Ce、Nd混合离子迁移时间RSD小于2％,MS信号RSD小于15％,且不同浓度样品经CE分离后其MS信号基本呈线性关系。     

亲和毛细管电泳的研究与应用

近年来,由于毛细管电泳技术理论的不断完善,亲和毛细管电泳技术得到迅速发展,并在生命科学、生物技术、临床医学、药物学等领域具有广泛的应用.对亲和毛细管电泳的原理、优点及分类做了简要介绍,并且着重介绍了近几年ACE技术在蛋白质分析、核苷酸分析、药物分析、手性分离及小分子、离子分析等方面的研究进展,及其在亲和常数测定、蛋白质结构分析、核苷酸的检测中的应用.     

Sensitive Method for Enantioseparation of Rivastigmine with Highly Sulfated Cyclodextrin as Chiral Selector by Capillary Electrophoresis

A sensitive method for enantioseparation of a basic drug rivastigmine and determination of its optical impurityby capillary electrophoresis with highly sulfated β-cyclodextrin(HS-β-CD)as the chiral selector is described.Ingeneral,enantioseparation of basic chiral compounds is carried out in acidic condition(pH 2.5)to prevent analytesfrom adsorption on the capillary wall.However,in the case of rivastigmine,the detection sensitivity was too limitedto determine the optical impurity of S-rivastigmine lower than 1% when buffer pH was 2.5.It was found that thedetection sensitivity was improved 1.6 times just by raising the buffer pH value from 2.5 to 5.8.The poor columnefficiency due to the adsorption of the analytes on the capillary wall was resolved by using dynamical coating of thecapillary wall with the linear polyacrylamide solution.The experirnental parameters such as the concentration ofHS-β-CD,buffer pH and buffer ionic strength were optimized,respectively.The method was validated in terms ofrepeatability,linearity,limit of detection(LOD)and limit of quantitation(LOQ).Using the present method,the op-tical purity of nonracemic rivastigmine with the enantiomeric excess(ee)value of 99.14% was determined.     

毛细管电泳中的毛细管区段灌注及其相关技术

毛细管区段灌注是一种随手性毛细管电泳、亲和毛细管电泳和胶束电动力色谱-质谱发展而产生的实验技术。由于它能消除采用以上方法时遇到的缓冲溶液对检测的影响。因此引起人们的关注。本文对区段灌注技术的原理,区段灌注技术在手性毛细管电泳、亲和毛细管电泳和胶束电动力色谱中的应用,以及目前区段灌注技术存在的一些问题进行了评述。本文还对由区段灌注技术发展而来的逆流毛细管电泳、液相预柱毛细管电泳、多步配体进样等实验技术进行了简介。     

毛细管胶束电动色谱法分离测定胆红素亚组分

用毛细管胶束电动色谱法成功地分离和定量测定了血清及胆汁中α，β，γ及δ等４种胆红素亚组分。二牛磺酸胆红素浓度在５１０μｍｏｌ／Ｌ以下时，峰面积与浓度呈良好的线性关系，二牛磺酸胆红素浓度即使为１．５μｍｏｌ／Ｌ时仍可检测出明显的定量峰。用一份２５５μｍｏｌ／Ｌ的二牛磺酸胆红素标准液进行重复性检测，第１次定量结果为２６０μｍｏｌ／Ｌ，出峰时间１６ｍｉｎ；第５０次电泳结果为２３８μｍｏｌ／Ｌ，出峰时间１６．７ｍｉｎ。     

毛细管电泳-质谱联用法测定清肺抑火片中的四种有效成分

建立了毛细管电泳-电喷雾电离质谱联用法同时测定清肺抑火片中苦参碱、药根碱、氧化苦参碱、栀子苷4种药效成分含量的分析方法.采用未涂层石英毛细管,以35 mmol/L乙酸铵(含20％乙腈,pH=6.5)为缓冲溶液、60％异丙醇(含3.3 mmol/L乙酸)为鞘液,分离电压为28 kV时,各组分在11 min内达到基线分离.苦参碱、药根碱、氧化苦参碱、栀子苷的线性范围分别为0.030～150 mg/L、0.060～20 mg/L、0.060～80 mg/L、0.60～300mg/L,检出限分别为0.010、0.020、0.020、0.20mg/L.样品的加标回收率在91.0％～107％之间,相对标准偏差均小于4.9％.方法简便、快速、灵敏度高,已成功用于清肺抑火片中的苦参碱、药根碱、氧化苦参碱、栀子苷含量的同时测定.