毛细管区带电泳法分离盐酸美沙酮对映体

目的:采用毛细管区带电泳法对盐酸美沙酮对映体进行了拆分。方法:比较了3种衍生化β-环糊精为手性添加剂的分离效果,对缓冲液的pH及浓度、手性添加剂的浓度、柱温、分离电压等方面进行了考察及优化。结果:确定采用75μm×75 cm未凃渍石英玻璃管柱,运行缓冲液为含50 mmol.L-1的Tris和10 mmol.L-1的HP-β-环糊精的水溶液(以磷酸调节pH至2.0),分离电压为25 kV,柱温25℃,检测波长为205 nm,结论:该方法简便、快速,在15 min内分离度可达到1.9。     

Chiral separation of tamsulosin by capillary electrophoresis

Enantiomers of (+/-) 5-[2 (R,S)-{[2-(o-ethoxyphenoxy) ethyl] amino} propyl]-2-methoxy-benzenesulfonamide (tamsulosin, drug frequently used in the treatment of prostate diseases) were separated by capillary electrophoresis (CE). An acidic background electrolyte (BGE) with sulfated-beta-cyclodextrin (S-beta-CD) was used to create a chiral separation environment. Baseline separation of the isomers was achieved during 5 min using cathodic electro-osmotic flow (EOF) (countercurrent mode). The quantification limits were 5.3 x 10(-6) moll(-1) for R-isomer and 5.7 x 10(-6) moll(-1) for S-isomer. The R.S.D. values of peak area were 0.54% for R-isomer and 0.75% for S-isomer. The results achieved enable determination of 0.5% of optical impurity.     

左舒必利的毛细管电泳手性分离与纯度检查

目的:建立手性分离方法并检查左舒必利光学纯度。方法:通过手性拆分剂的种类及浓度、缓冲液的pH及浓度、温度及电压的优化,选择最佳的手性分离条件。结果:最佳分离条件缓冲液为100 mmol·L~(-1)磷酸盐缓冲液(用磷酸调pH4．0,内含18 mmol·L~(-1)β-环糊精硫酸钠盐);检测波长为254 nm;电压为15 kV;温度为22℃,基线分离了舒必利2个对映体。结论:建立的毛细管电泳法可用于左舒必利的质量控制和稳定性研究。     

Chiral separation of fluvastatin enantiomers by capillary electrophoresis

An analytical CE method was developed for the enantiomeric purity determination of fluvastatin enantiomers. Fluvastatin enantiomers were separated on an uncoated fused silica with 100 mM-borate solution containing 30 mg/mL of (2-hydroxypropyl)-beta-cyclodextrin (HP-beta-CD) as running buffer and fenoprofen as an internal standard. The linearity was observed within a 400-700 microg/mL concentration range (r(2)>or=0.995) for both fluvastatin enantiomers. The repeatability expressed as coefficient of variation (CV) of the method were 0.96 and 0.92% for (+)-3R, 5S and (-)-3S, 5R-fluvastatin, respectively. The limit of detection and quantification for both fluvastatin enantiomers were 1.5 microg/mL and 2.5 microg/mL, respectively.     

盐酸昂丹司琼的高效毛细管电泳手性分离

目的:建立盐酸昂丹司琼的高效毛细管电泳的手性分离方法。方法:通过手性拆分剂的种类及浓度、缓冲液的pH及浓度、温度及电压的优化,选择最佳的手性分离条件。结果:最佳分离条件缓冲液为33 mmol.L-1三羟甲基氨基甲烷(Tris)(用磷酸调节pH 2.2,含30 mg.mL-1羧甲基-β-环糊精);检测波长为214 nm;电压为30 kV;温度为25℃,基线分离了盐酸昂丹司琼的2个对映体。结论:新建立的方法可用于这一新药研究开发过程中的产品质量控制。     

毛细管电泳法分离4种手性药物对映体

目的建立以羧甲基-β-环糊精(carboxymethyl-β-cyclodextrin,CM-β-CD)为手性选择剂的毛细管电泳法拆分氯苯那敏、羟氯喹、班布特罗和沙丁胺醇4种手性药物。方法采用未涂层石英毛细管柱,背景电解质为Na H2PO4缓冲溶液,分离电压为20 k V。考察了CM-β-CD的质量浓度、缓冲溶液质量浓度和p H值对拆分的影响。结果在最佳分离条件下,氯苯那敏、羟氯喹、班布特罗和沙丁胺醇的分离度分别为10.49、6.97、3.75和1.56。结论 CM-β-CD对研究的4种药物有非常高的对映体选择性。     

毛细管电泳法手性分离5种碱性药物

目的:采用自制的羧甲基-β-环糊精作为手性选择剂,用毛细管电泳法手性分离氧氟沙星、扑尔敏、普萘洛尔、沙丁胺醇和维拉帕米5种碱性药物。方法:改变影响手性分离的主要因素:缓冲溶液的 pH、羧甲基-β-环糊精的浓度、电压和温度,对分离条件进行优化,并采用对照品加入法将手性药物单体加入到对映体混合物中,研究了普萘洛尔和氧氟沙星的出峰顺序。结果:氧氟沙星、扑尔敏、维拉帕米3种手性药物均达到基线分离,确定了氧氟沙星对映体和普萘洛尔对映体的出峰顺序。结论:合适的电泳条件下可以实现氧氟沙星等5种碱性药物的手性分离,按手性药物出峰顺序可对同类药物的进行定性分析。     

以盐酸去甲万古霉素为手性选择剂毛细管电泳法分离西替利嗪对映体

目的:建立以阳离子表面活性剂碘化四丁基铵为电渗流改性剂,以盐酸去甲万古霉素为手性选择剂的毛细管电泳法分离西替利嗪对映体。方法:考察了盐酸去甲万古霉素浓度、Tris 浓度和缓冲液 pH 对分离的影响,对分离条件进行了优化。结果:在含0.04 g·L~(-1)碘化四丁基铵和1.0 mmol·L~(-1)盐酸去甲万古霉素的25 mmol·L~(-1)Tris 磷酸缓冲液(pH 4.5)的运行电解质体系中,西替利嗪对映体在分离电压为20 kV 的条件下得到良好分离,西替利嗪对映体分离度达1.8。结论:本法可用于西替利嗪对映体的分离。     

磺胺类药物的毛细管高效液相色谱与电色谱研究

目的 研究毛细管高效液相色谱(μ-HPLC)和毛细管电色谱(CEC)分离磺胺类药物,建立药物微分离分析方法。方法 用ODS柱为固定相,甲醇和2 mmol·L^-1磷酸缓冲液（pH 3.0～7.0）为流动相,电压为0～-15 kV,流速为10 μL·min^-1,紫外检测波长254 nm。结果μ-HPLC在甲醇-2 mmol·L^-1磷酸缓冲液（30∶70）,pH 3.0时5种磺胺类药物实现基线分离;CEC在电压为-5 kV,甲醇-2 mmol·L^-1磷酸缓冲液（30∶70）,pH 5.0时5种磺胺类药物实现基线分离。结论电渗流随甲醇含量、缓冲液浓度增加而下降,随pH值、电压的增加而增加;溶质的保留值（k）随甲醇含量、缓冲液浓度、电压的增加而下降,随电压增加下降明显的是TMP,随pH值变化较复杂。在相同条件下对5种磺胺类药物的分离,μ-HPLC需67 min,CEC只需25 min,后者更适合于磺胺类药物的快速分离分析。     

毛细管区带电泳对5种三唑类化合物的手性分离

目的:考察毛细管区带电泳法(CZE)中各种因素对β-环糊精衍生物手性分离三唑类化合物的影响.方法:采用CZE对5个三唑类化合物的手性分离进行研究.BECKMAN P/ACE System 5 000毛细管电泳仪.紫外检测器.未涂渍熔融石英毛细管50μm×47 cm(有效长度40 cm);正极压力进样50 mbar×3 s,检测波长200 nm.3-环糊精的3种衍生物做为手性添加剂.结果:羧甲醚-β-环糊精为手性选择剂是5个化合物都能达到较好的手性分离,而硫酸酯-β-环糊精和二氟代羧甲醚-β-环糊精对这5个化合物无手性分离能力.在羧甲醚-β-环糊精环境下,优化选择30 mmol/L的NaH2PO4缓冲液含羧甲醚-β-环糊精5 mmol/L,用H3PO4调节pH2.2,温度20℃,电压20 KV,在此条件下5个化合物都能达到良好的手性分离.结论:β-环糊精的种类和缓冲液的pH是影响这5对三唑类对映异构体分离的关键因素.     

Chiral separation of pemoline enantiomers by cyclodextrin-modified micellar capillary chromatography

Micellar electrokinetic chromatography (MEKC) was successfully applied to the chiral separation with the addition of cyclodextrins (CDs) as chiral selector to running buffer. Chiral separation depended on the type of CDs. Mono-3-O-phenylcarbamoyl-beta-CD was effective for the chiral separation of pemoline. We investigated the type and concentration of CD and other parameters such as buffer pH, the concentration of SDS and the effect of organic modifier. The conditions for enantiomeric separation of pemoline were as follows: 40 mmol/l borate buffer at pH 9.0 with 40 mmol/l SDS, 20 mmol/l mono-3-O-phenylcarbamoyl-beta-CD and 10% 2-propanol. Baseline separation (Rs=2.21) of pemoline can be achieved.     

苯磺酸左旋氨氯地平的毛细管电泳手性分离与纯度检查

目的：建立手性分离方法并检查苯磺酸左旋氨氯地平的光学纯度。方法：通过手性拆分剂的种类及浓度、缓冲液的pH及浓度、温度及电压的优化，选择最佳的手性分离条件。结果：最佳分离条件缓冲液为50mmol·L^-1，Tris（用磷酸调节pH2.5，含10mmol·L^-1羧甲基-β-环糊精）；检测波长为214nm;电压为25kV；温度为22℃，基线分离氨氯地平2个对映体，对建立的方法进行方法学验证，并检查实际样品的光学纯度。结论：建立的毛细管电泳法实用性强，费用低，因此采用了高效毛细管电泳法测定光学纯度，为该药的质量控制和稳定性研究提供了可靠的分析方法。     

Rapid separation and determination of structurally related anthraquinones in Rhubarb by pressurized capillary electrochromatography

A pressurized capillary electrochromatography (pCEC) with monolithic column has been developed for the rapid separation and determination of five structurally related anthraquinones in Rhubarb. The possibility of rapid separation resulted from the unique pore structure with high permeability and favorable mass transfer characteristics of the monolithic stationary phase. The effect factors such as organic modifier, acidity and concentration of running buffer, separation voltage were investigated to acquire the optimum condition. In the 220 nm wavelengths, the five anthraquinones could be baseline-separated rapidly within 5 min with the separation voltage of -20 kV in 10 mmol/L phosphate buffer (pH 6.2) containing 65% acetonitrile. The calibration graphs of rhein, aloe-emodin, emodin chrysophanol and physcion were linear by plotting the peak area against the analytes concentration over the range of 0.2-65, 0.1-30, 0.1-55, 0.5-30 and 0.5-55 microg/mL, respectively. The detection limits of five anthraquinones were ranged from 0.06 to 0.2 microg/mL and the recoveries of Rhubarb samples were about 81.3-86.4% (R.S.D.< or = 5.2%). This proposed method was successfully applied to determination of the five analytes in Rhubarb with satisfactory results.     

西布曲明对映体的毛细管电泳分离及结合常数的测定

目的 采用毛细管电泳法分离西布曲明对映体并测定其结合常数.方法 考察手性添加剂浓度、缓冲溶液pH及浓度、温度、分离电压等因素对分离度的影响,并采用双倒数法计算西布曲明对映体与2,6-二甲基-β-环糊精(DM-β-CD)的结合常数.结果 在12.5 mmol·L~(-1)DM-β-CD、100 mmol·L~(-1)Tris-H_3PO_4(pH 2.5)缓冲液、16℃柱温,30 kV操作电压的毛细管电泳条件下,西布曲明对映体在9 min内获得了良好分离,分离度达2.0;结合常数分别为154.4、173.3 L·mol~(-1).结论 所用高效毛细管电泳方法快速、准确、可靠,适用于西布曲明对映体的分离;结合常数的计算可为研究西布曲明对映体的拆分机理提供依据.     

托特罗定的高效毛细管电泳手性分离

目的：建立新型M-受体阻断剂托特罗定的高效毛细管电泳的手性分离方法。方法：通过探讨环糊精的种类、浓度、缓冲液的浓度、pH值对分离的影响,选择手性分离的最佳条件,结果：托特罗定的光学异构体得到基线分离,测定了该药的光学纯度。结论：所建立的方法可用于这一新药研究开发过程中的产品质量控制。     

Comparison of the miniaturised techniques capillary electrochromatography and capillary liquid chromatography for the chiral separation of chlorthalidone

The aim of this study was to compare the miniaturised techniques, capillary electrochromatography (CEC) and capillary liquid chromatography (CLC), for the chiral separation of chlorthalidone. In both cases, hydroxypropyl-beta-cyclodextrin was used as a chiral selector in the mobile phase, while an achiral stationary phase was used. Earlier, this separation was already optimised in CEC. Now, the separation was optimised in CLC. The influence of the organic modifier content and the cyclodextrin concentration on the separation was studied by means of a central composite design. Optimal separation conditions were determined, after response modelling, from the response surface contour plots. When these conditions were compared with those of the CEC optimisation, we can see the potential of using CLC as a chiral separation technique since less chiral selector was used, faster separations were obtained and better repeatability was observed in comparison with its electrical-driven counterpart.     

Chiral separation of beta-methyl-amino acids by ligand exchange using capillary electrophoresis and HPLC.

This paper deals with the chiral separation of optical isomers of beta-methyl-amino acids by CE and HPLC using the principle of ligand-exchange. Capillary zone electrophoresis was carried out using Cu(II) complexes of L-4-hydroxyproline (L-4-Hypro), N-(2-hydroxypropyl)-L-4-hydroxyproline (HP-L-4-Hypro) and N-(2-hydroxyoctyl)-L-4-hydroxyproline (HO-L-4-Hypro) as chiral selectors, added to the electrolyte. The HPLC separations were performed on a chiral stationary ligand-exchange chromatography phase containing L-4-Hypro chemically bonded to silica gel. With both techniques nearly all compounds investigated are baseline resolved using different background electrolytes and mobile phases, respectively.     

Chiral separation and quantitation of pentazocine enantiomers in pharmaceuticals by capillary zone electrophoresis using maltodextrins

The chiral separation of pentazocine was achieved by capillary electrophoresis using oligosaccharides. Enantiomers were separated on 100 mM Tris/H3PO4 buffer (pH 2.5) with 5% maltodextrin as a chiral selector, and migration behavior was monitored at 200 nm. Under these conditions, (-)- and (+)-pentazocine and dextromethorphan (internal standard) migrated within 9 min, and the resolution of pentazocine enantiomers was 2.54. Linear calibration curves were obtained in the range 5-50 microg/ml(-1) for each enantiomer. The detection limit of pentazocine enantiomers was 29 pg, and the recoveries of(-)- and (+)-pentazocine were 98.9 (R.S.D., 3.4%) and 101.4% (R.S.D., 4.3%) with 10 microg/ml(-1), respectively.