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使用万古霉素手性固定相柱,通过毛细管液相色谱(CLC)和加压毛细管电色谱(pCEC)分离β受体阻滞剂及其类似物。

Separation of beta-receptor blockers and analogs by capillary liquid chromatography (CLC) and pressurized capillary electrochromatography (pCEC) using a vancomycin chiral stationary phase column.

作者信息

Chen Zhongyi, Zeng Su, Yao Tongwei

机构信息

College of Pharmaceutical Sciences, Zhejiang University, Hangzhou, China.

出版信息

Pharmazie. 2007 Aug;62(8):585-92.

Abstract

Enantiomeric separation of chiral pharmaceuticals was carried out by means of in capillary liquid chromatography (CLC) and pressurized capillary electrochromatography (pCEC) using a vancomycin chiral stationary phase (CSP). A 100 microm I.D. fused-silica capillary was packed with 5 microm diameter silica particles modified with vancomycin. Enantiomeric resolution of fifteen beta3-receptor blockers and analogs was studied by polar organic CLC mode and reversed-phase pCEC mode using mobile phases containing methanol-isopropanol-acetic acid-triethylamine and TEAA buffer-methanol, respectively. Several factors affecting chiral separation were investigated in both CLC and pCEC mode. Good enantiomeric resolution was achieved by CLC mode for propranolol, celiprolol, esmolol, bisoprolol, atenolol, metoprolol and carteolol using methanol-isopropanol-acetic acid-triethylamine (70:30:0.05:0.05, v/v/v/v) as mobile phase and for clenbuterol, bambuterol, terbutaline, and salbutamol using methanol-isopropanol-acetic acid-triethylamine (50:50:0.05:005 or 50:50: 0.025:0.05, v/v/v/v) as mobile phase. The baseline was achieved by pCEC mode for the separation of esmolol, bisoprolol, atenolol, metoprolol, carteolol in the mobile phase containing MeOH-0.05%TEAA (pH 7.0) (90:10, v/v) (-10 kV), and that of propranolol and celiprolol in the mobile phase containing MeOH-0.025%TEAA (pH 7.0) (90:10, v/v)(-10 kV). Comparative enantioseparations performed in polar organic CLC and reversed phase pCEC mode revealed significant difference.

摘要

采用万古霉素手性固定相(CSP),通过毛细管液相色谱(CLC)和加压毛细管电色谱(pCEC)对手性药物进行对映体分离。一根内径为100微米的熔融石英毛细管填充了用万古霉素修饰的5微米直径的硅胶颗粒。采用分别含有甲醇 - 异丙醇 - 乙酸 - 三乙胺和三乙胺乙酸盐缓冲液 - 甲醇的流动相,通过极性有机CLC模式和反相pCEC模式研究了15种β3受体阻滞剂及其类似物的对映体拆分。在CLC和pCEC模式下研究了影响手性分离的几个因素。在CLC模式下,以甲醇 - 异丙醇 - 乙酸 - 三乙胺(70:30:0.05:0.05,v/v/v/v)为流动相时,普萘洛尔、塞利洛尔、艾司洛尔、比索洛尔、阿替洛尔、美托洛尔和卡替洛尔实现了良好的对映体拆分;以甲醇 - 异丙醇 - 乙酸 - 三乙胺(50:50:0.05:0.05或50:50:0.025:0.05,v/v/v/v)为流动相时,克仑特罗、班布特罗、特布他林和沙丁胺醇实现了良好的对映体拆分。在含有甲醇 - 0.05%三乙胺乙酸盐(pH 7.0)(90:10,v/v)(-10 kV)的流动相中,pCEC模式下艾司洛尔、比索洛尔、阿替洛尔、美托洛尔、卡替洛尔实现了基线分离;在含有甲醇 - 0.025%三乙胺乙酸盐(pH 7.0)(90:10,v/v)(-10 kV)的流动相中,普萘洛尔和塞利洛尔实现了基线分离。在极性有机CLC和反相pCEC模式下进行的对比对映体分离显示出显著差异。

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