Huang Lu, Lin Jin-Ming, Yu Lishuang, Xu Liangjun, Chen Guonan
Fuzhou University, Fuzhou, Fujian, China.
Electrophoresis. 2008 Sep;29(17):3588-94. doi: 10.1002/elps.200700811.
A capillary electrophoresis method using carboxymethyl-beta-cyclodextrin as the chiral selector and mixture of methanol and ethanol as the organic additive was successfully developed for the simultaneous enantioseparation and determination of six beta-blockers, namely, carteolol, atenolol, sotalol, metoprolol, esmolol and propranolol in this paper. The most suitable running buffer for enantioseparation was found to be the solution of 20 mmol/L NaH(2)PO(4)-Na(2)HOP(4) (pH 5.5) containing 1.5% w/v carboxymethyl-beta-cyclodextrin, 5% v/v methanol and 5% v/v ethanol. Furthermore, field-amplified sample injection as an on-line sample stacking method was developed in order to increase the detection sensitivity. The experimental conditions for both simultaneous enantioseparation and the field-amplified sample injection method had been investigated in detail. Under the optimum conditions, the detection limits (defined as S/N=3) of this method were 0.01, 0.05, 0.05, 0.05, 0.05 and 0.5 microg /mL for (+/-) carteolol, (+/-) atenolol, (+/-) sotalol, (+/-) metoprolol, (+/-) esmolol and (+/-) propranolol, respectively, which were much lower than those of the conventional methods. The enhancement factors were greatly improved by 25-fold for the enantiomers of the beta-blockers except five-fold for (+/-) propranolol. Eventually, the proposed method has been applied for the analysis of human serum sample.
本文成功开发了一种毛细管电泳方法,该方法以羧甲基-β-环糊精作为手性选择剂,甲醇和乙醇的混合物作为有机添加剂,用于同时对六种β受体阻滞剂进行对映体分离和测定,这六种β受体阻滞剂分别是卡替洛尔、阿替洛尔、索他洛尔、美托洛尔、艾司洛尔和普萘洛尔。结果发现,最适合对映体分离的运行缓冲液是含有1.5% (w/v)羧甲基-β-环糊精、5% (v/v)甲醇和5% (v/v)乙醇的20 mmol/L NaH₂PO₄-Na₂HPO₄(pH 5.5)溶液。此外,为了提高检测灵敏度,开发了场放大进样作为一种在线样品堆积方法。详细研究了同时进行对映体分离和场放大进样方法的实验条件。在最佳条件下,该方法对(±)卡替洛尔、(±)阿替洛尔、(±)索他洛尔、(±)美托洛尔、(±)艾司洛尔和(±)普萘洛尔的检测限(定义为S/N = 3)分别为0.01、0.05、0.05、0.05、0.05和0.5 μg/mL,远低于传统方法。除了(±)普萘洛尔提高了5倍外,β受体阻滞剂对映体的增强因子大幅提高了25倍。最终,该方法已应用于人血清样品的分析。