负电性和中性环糊精在毛细管电泳手性分离中的协同效应

１引言环糊精及其电中性衍生物（二甲基－β－环糊精（ＤＭ－β－ＣＤ）、三甲基－β－环糊精（ＴＭ－β－ＣＤ）、羟丙基－β－环糊精（ＨＰ－β－ＣＤ））是毛细管电泳（ＨＰＣＥ）手性分离中最常采用的手性选择剂,带电环糊精是ＨＰＣＥ手性分离中另一类重要的手性选择剂,它的带电性质使其在手性拆分过程中起到非常重要的作用。本文分别考察了带电的磺丁基－β－环糊精（ＳＢＢ－β－ＣＤ）与电中性的ＤＭ－β－ＣＤ、ＴＭ－β－ＣＤ以及ＨＰ－β－ＣＤ等３种双环糊精体系的手性拆分性能,研究了双环糊精在手性分离中所体现出的协同效应…     

以β-环糊精及其衍生物为手性选择剂毛细管电泳拆分几种药物的旋光对映体

在毛细管电泳中，采用β－环糊精（β－ＣＤ）及其衍生物为手性选择剂对扑尔敏、异丙嗪、二氧异丙嗪和氧氟沙星对映体进行了分离。优化了分离条件；讨论了环糊精空腔边缘与溶．质分子作用的基团的种类和分离效果的联系，通过计算手性分离的热力学常数比较了不同手性选择剂对扑尔敏对映体的分离能力。最后，讨论了乙腈在手性分离中的作用。     

羧甲基—β—环糊精用于毛细管电泳中的手性分离

本文将水溶性良好的羧甲基－β－ＣＤ（ＣＭ－β－ＣＤ＿用于分离氯霉素中间体，考察了ＣＭ－β－ＣＤ作为毛细管电泳手性选择剂的分离性能。     

以β—环糊精及其衍生物为手性选择性毛细管电泳拆分几种药物的旋光…

在毛细管电泳中，采用β－环糊精（β－ＣＤ）及其衍生物为手性选择剂对扑尔敏、异丙嗪、二氧异丙嗪和氧氟沙星对映体进行了分离。优化了分离条件；讨论了环糊精空腔边缘与溶质分子作用的基团的种类和分离效果的联系，通过计算手性分离的热力学常数比较了不同手性选择剂对扑尔敏对映体的分离能力。最后，讨论了乙腈在手性分离中的作用。     

γ－环糊精－SDS胶束电动色谱法分离十八甲基炔诺酮光学异构体

 研究了ＣＤ－ＳＤＳ胶束电动色谱（ＣＤ－ＭＥＫＣ）对电中性及疏水性的手性化合物的分离，并讨论了不同类型ＣＤ的手性识别作用。使用γ－ＣＤ可以有效地拆分十八甲基块诺酮（ＮＯＧ）旋光异构体。选择了最佳分离条件，通过调节ＣＤ和ＳＤＳ浓度以及其它操作条件可以把ＮＯＧ异构体很好的分离。     

γ－环糊精－SDS胶束电动色谱法分离十八甲基炔诺酮光学异构体

研究了ＣＤ－ＳＤＳ胶束电动色谱（ＣＤ－ＭＥＫＣ）对电中性及疏水性的手性化合物的分离，并讨论了不同类型ＣＤ的手性识别作用。使用γ－ＣＤ可以有效地拆分十八甲基块诺酮（ＮＯＧ）旋光异构体。选择了最佳分离条件，通过调节ＣＤ和ＳＤＳ浓度以及其它操作条件可以把ＮＯＧ异构体很好的分离。     

对萘普生和萘普生甲酯的毛细管电泳手性分离

以磺化β－ＣＤ作为手性分离添加剂,分别对萘普生和萘普生甲酯进行了手性分离研究,当磺化β－ＣＤ的浓度为３．５％（Ｗ／Ｖ）时,萘普生和萘普生甲酯的手性分离度都可大于２,但萘普生与萘普生甲酯不能达到同时拆分。如果同时以磺化β－ＣＤ和ＨＰ－β－ＣＤ作为作为手性分离添加剂,则可对萘普生甲酯达到同时拆分,当磺化β－ＣＤ和ＨＰ－β－ＣＤ的浓度分别为３．５％和１．５％（Ｗ／Ｖ）时,对萘磺生和萘普生甲酯两种消旋体的     

毛细管区带电泳拆分肾上腺素类药物

考察各种因素对β-环糊精及其衍生物分离肾上腺素类药物的影响.采用毛细管区带电泳法(CZE)对去甲肾上腺素、肾上腺素和异丙肾上腺素的手性分离进行研究.未涂渍熔融石英毛细管50 μm×58.5 cm(有效长度50 cm);温度20℃,操作电压30 kV,正极进样50 mbar×3 s,检测波长204 nm.β-环糊精(β-CD)及其两种衍生物作为手性选择剂.异丙肾上腺素得到了基线分离,肾上腺素和去甲肾上腺素未分离.     

用环瑚精分离取代四氢—β—咔啉类手性化合物

毛细管电泳是一种分离手性化合物极为有效的工具。本文用β－环糊精作为手性选择剂在ＣＺＥ的模式下对取代四氢β－咔啉类手性化合物进行了成功的拆分。     

用去氧胆酸盐和β-环糊精的毛细管胶束电动色谱拆分手性药物

 用β－环糊精（β－ＣＤ）和去氧胆酸钠（ＳＤＣ）的环糊精改性毛细管胶束电动色谱，实际拆分了ＥＭＤ－５６４３１和扑尔敏两种手性药物，研究了ＳＤＣ和β－ＣＤ浓度及ｐＨ值对分离的影响。初步讨论了分离的机理。认为ＣＤ－ＳＤＣ体系中胶束单体分子几乎均被ＣＤ包合；ＣＤ可能与部分胶束单体包合而存在于ＳＤＣ的胶束中；该拆分体系中ＳＤＣ与β－ＣＤ的浓度比在４∶１～４∶３时拆分效果最好。并发现ＳＤＣ对β－ＣＤ有显著的增溶作用。     

以L-白氨酸为手性选择剂用毛细管电泳法拆分12种手性药物

 建立了一种以L 白氨酸为手性选择剂用毛细管区带电泳法快速分离 12种手性药物的方法。实验结果表明 ,手性对映体的分离度受L 白氨酸浓度和缓冲液 pH的影响。在含有 70mmol/LL 白氨酸 ,5 0mmol/L硼砂 (pH9.0 )的溶液中 ,12种手性药物在 11min之内得到了基线分离。     

Investigation of beta-CD-derivatized erythromycin as chiral selector in CE

A novel water-soluble beta-CD-derivatized erythromycin (EM) was synthesized and used as an effective chiral selector for the resolution of chiral compounds in CZE. The purpose of substitution at the primary hydroxyl site of beta-CD with 1-oxygen-2,3-epoxypropane is to produce a compound having functions of both beta-CD and EM. beta-CD-derivatized EM exhibited excellent enantioselectivities compared with single beta-CD and EM for chiral separation in CE. We also investigated the influence of pH and concentration of BGE, concentration of chiral selector, applied potential, and organic modifier on chiral compounds' separation.     

应用四甲基氢氧化铵控制电渗流的毛细管电泳方法分离多沙唑嗪及其中间体的对映体

建立了毛细管电泳手性分离多沙唑嗪中间体对映体的方法,并同时分离了多沙唑嗪对映体。考察了不同种类季铵盐对电渗流及分离的影响,其中四甲基氢氧化铵(TMB)能有效控制电渗流并提高组分的分离度。实验还考察了其他因素,如pH值、分离电压和磷酸二氢钠浓度对分离的影响。所用的毛细管为40 cm(有效长度30 cm)×50 μm,缓冲液为12 mmol/L β-环糊精、30 mmol/L TMB、60 mmol/L 磷酸二氢钠(pH 2.2),分离电压为20 kV。在此条件下多沙唑嗪及其中间体的对映体均达到了基线分离。实验结果表明,一些用β-环糊精不能完全分离的对映体通过加入TMB控制电渗流能达到满意的分离效果。     

Enantiomeric separation of a group of chiral dihydropyridines by electrokinetic chromatography

Electrokinetic chromatography (EKC) was employed to achieve the enantiomeric separation of a group of chiral 1,4-dihydropyridines (DHPs) with pharmacological activity. Micelles of bile salts alone or mixed with neutral cyclodextrins, micelles of sodium dodecyl sulfate (SDS) mixed with neutral cyclodextrins, and anionic cyclodextrin derivatives, i.e., carboxymethyl-gamma-cyclodextrin (CM-gamma-CD), carboxymethyl-beta-cyclodextrin (CM-beta-CD), and succinylated beta-cyclodextrin (Succ-beta-CD), were employed as pseudostationary phases. The enantiomeric separation ability of these chiral selectors with respect to DHPs was studied in different experimental conditions. CM-beta-CD was shown to be the best chiral selector to perform the enantiomeric separation of DHPs by EKC. Next, the influence of the CM-beta-CD concentration, the pH and nature of the buffer, the temperature, and the applied voltage on the enantiomeric resolution of DHPs was studied. The use of a 50 mM ammonium acetate buffer, pH 6.7, 25 mM in CM-beta-CD together with an applied voltage of 15 or 20 kV, and a temperature of 15 degrees C enabled the individual enantiomeric separation of twelve DHPs, each one into its two enantiomers, and their separation in multicomponent mixtures of up to six DHPs into all their enantiomers.     

用羧甲基聚合环糊精作手性剂的毛细管电泳法分离3种碱性药物

 采用 5种环糊精衍生物对碱性药物硫喷妥钠、盐酸氟桂利嗪、山梗菜碱进行了毛细管区带电泳的手性拆分。结果表明 ,采用含 2 % (质量分数 ,其余相同 )聚合 β 环糊精 (P β CD)或 0 5%羧甲基聚合 β 环糊精 (CM P β CD) 30mmol/L的Tris H3PO4缓冲液可使这 3种药物达到基线分离 ;使用CM P β CD时 ,分离度高达 4～35。     

Enatiomeric analysis of simendan by CE with beta-CD as chiral selector compared with CMPA-HPLC

The chiral separation of simendan enantiomers using capillary electrophoresis was studied with beta-cyclodextrin (beta-CD) as chiral selector. The influences of the concentration and pH of borate buffer solution, beta-CD concentration and methanol content in the background electrolyte were investigated. These factors were compared with those in an HPLC with beta-CD as chiral mobile phase additive (CMPA-HPLC). The quantification properties of the developed CE method were examined. A baseline separation of simendan enantiomers was achieved in the background electrolyte of 20 mmol/L borate buffer (pH 11.0) containing 12 mmol/L beta-CD-methanol (50:50 in volume ratio). The CE method is comparable with CMPA-HPLC in chiral resolution, although the optimal pH in CE (11.0) is much higher than that (6.0) in CMPA-HPLC. This chiral CE method is applicable to the quantitative ananlysis and enantiomeric excess value determination of L-simendan.     

Enantioseparation of three kinds of adrenaline by capillary electrophoresis using Ser-AuNPs as chiral selectorEI北大核心CSCD

Au nanoparticlesAuNPswere synthesized by chemical reduction methodand its surface was chiral modified with serine to prepare Ser-AuNPs. The synthesis effect and particle size distribution of AuNPs and Ser-AuNPs were characterized by UV-Vis spectrophotometry and laser particle size analyzer. The Ser-AuNPs was used as a chiral selector for the enantiomeric separation of three adrenaline drugs by capillary zone electrophoresis. The influences of the binding concentration of serinebuffer pHseparation voltage and capillary temperature on the enantioseparation were investigated. The results showed that the enantiomeric separation of isoprenaline adrenaline and noradrenaline could achieve baseline separation at the optimal separation conditions. The corresponding resolutions were 3.192.85 and 3.77 for isoprenalineadrenaline and noradrenalinerespectively. And this method possessed good reproducibility and precision. © 2022, Youke Publishing Co.,Ltd. All rights reserved.     

Enantioseparation of warfarin and its metabolites by capillary zone electrophoresis

A capillary zone electrophoresis (CZE) method with direct ultraviolet (UV)-absorbance detection is presented for the simultaneous enantiomeric separation of warfarin and its main metabolites, including warfarin alcohols, 4'-, 6-, and 7-hydroxywarfarin, using highly sulfated beta-cyclodextrin (HS-beta-CD) as the chiral selector. This chiral separation method was optimized in terms of the electrophoretic parameters, which included the concentration of HS-beta-CD used, the type and composition of organic modifier added to the background electrolyte (BGE) buffer, and the BGE buffer pH. Chiral separation of warfarin and its major metabolites was achieved with high resolution, selectivity, efficiency, repeatability, and reproducibility. This optimized chiral analysis of warfarin along with its metabolites was completed within a satisfactory electrophoresis time of 20 min.     

Enantiomeric separation of synthetic 2,3-dihydroxy-3-phenylpropionate compounds by beta-cyclodextrin-modified capillary electrophoresis

A new capillary electrophoretic method was developed for enantiomeric separation and optical impurity analysis of three synthetic 2,3-dihydroxy-3-phenylpropionate compounds using native beta-cyclodextrin (beta-CD) as chiral selector and borate as a background electrolyte. The separation was carried out in uncoated capillary (58.5 cm x 75 microm I.D., effective length 48.5 cm). The results showed that beta-CD as the chiral selector exhibited good enantioselectivity and the baseline separation was obtained at pH 9.8, 200 mM borate buffer containing 1.7% beta-CD at applied voltage 15 kV and capillary temperature 20 degrees C within 15 min. The precision of each tested compound was less than 1.0% at migration time and 5.0% in corrected peak area and the accuracy of the method was in the range of 98.7-105%. Furthermore, the developed method was successfully applied to the determination of the undesirable trace (2S,3R)-(+)-form impurity in the synthetic (2R,3S)-(-)-2,3-dihydroxy-3-phenylpropionate samples.     

Separation and control of the elution order of N-t-butyloxycarbonyl amino acids D/L isomers by reversed-phase HPLC using cyclodextrins as chiral selectors for the mobile phase.

The enantiomeric resolution of N-t-butyloxycarbonyl (N-t-Boc) amino acids D/L isomers by reversed-phase HPLC was investigated using cyclodextrins (CD's) as chiral selectors for the mobile phase. The use of a low pH (pH<4) for the mobile phase enabled the enantioseparation of N-t-Boc amino acids. The opposite elution order of D/L isomers was observed when hydroxypropyl-derivatized beta-CD was used instead of native beta-CD. A computer simulation of the enantioseparation showed that the ratio of the retention factors of the chiral selector and the sample determined the elution order and the resolution. When the retention factor of the chiral selector is smaller than that of the sample, an isomer having larger complex formation constant eluted faster. However, when the chiral selector had a larger retention factor than the sample, an opposite elution order of the isomers was obtained. The large difference in the retention factors between the chiral selector and the sample led to good enantiomeric separation.