以L-酒石酸正己酯-硼酸配合物作为反相液相色谱手性流动相添加剂拆分5种β-受体阻滞剂  被引量:5

Chiral separation of five β-blockers using di-n-hexyl L-tartrate-boric acid complex as mobile phase additive by reversed-phase liquid chromatography

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作  者:杨娟[1] 王利娟[1] 郭巧玲[1] 杨更亮[1] 

机构地区:[1]河北大学药学院,河北省药物质量研究重点实验室,河北保定071002

出  处:《色谱》2012年第3期280-284,共5页Chinese Journal of Chromatography

基  金:国家自然科学基金项目(No.21175031);河北省应用基础研究计划重点基础研究项目(No.11966411D);河北省高等学校科学技术研究重点项目(No.ZD2010234);河北省药物质量研究重点实验室青年开放课题(No.09265631D-13)

摘  要:以L-酒石酸正己酯-硼酸配合物为手性流动相添加剂,建立了普萘洛尔、艾司洛尔、美托洛尔、比索洛尔和索他洛尔5种β-受体阻滞剂的反相高效液相色谱手性分离方法。对影响对映体分离的主要因素:L-酒石酸正己酯和硼酸的浓度,缓冲溶液的种类、浓度、pH值,有机改性剂甲醇的含量以及对映体分子结构等进行了详细考察。最佳色谱条件为:Venusil MP-C18色谱柱(250 mm×4.6 mm,5μm);流动相为15 mmol/L乙酸铵-甲醇(体积比为20∶80或30∶70(索他洛尔)),含60 mmol/L硼酸,70 mmol/L L-酒石酸正己酯,乙酸调节pH值至6.00;检测波长214 nm。在最佳分离条件下,5对对映体可以分别获得基线分离。A reversed-phase high performance liquid chromatographic (HPLC) method using the di-n-hexyl L-tartrate-boric acid complex as a chiral mobile phase additive was developed for the enantioseparation of five fi-blockers including propranolol, esmolol, metoprolol, bisoprolol and sotalol. In order to obtain a better enantioseparation, the influences of concentrations of di-n-butyl L-tartrate and boric acid, the type, concentration and pH of the buffer, methanol content as well as the molecular structure of analytes were extensively investigated. The sepa-ration of the analytes was performed on a Venusil MP-C18 column (250 mm×4.6 ram, 5 μm). The mobile phase was 15 mmol/L ammonium acetate-methanol containing 60 mmol/L boric acid, 70 mmol/L di-n-hexyl L-tartrate ( pH 6.00 ). The volume ratios of 15 mmol/L ammonium acetate to methanol were 20:80 for propranolol, esmolol, metoprolol, bisoprolol and 30:70 for sotalol. The flow rate was 0. 5 mL/min and the detection wavelength was set at 214 nm. Under the optimized conditions, baseline enantioseparation was obtained separately for the five pairs of analytes.

关 键 词:反相高效液相色谱 手性拆分 手性添加剂 酒石酸酯-硼酸配合物β-受体阻滞剂 

分 类 号:O658[理学—分析化学]

 

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