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.
出处
《色谱》
CAS
CSCD
北大核心
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)
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
reversed-phase high performance liquid chromatography （RP-HPLC）
chiral sepa-ration
chiral additive
tartrate-boric acid complex
β-blockers
