色谱

色谱 ›› 2014, Vol. 32 ›› Issue (11): 1219-1224.DOI: 10.3724/SP.J.1123.2014.07018

• 研究论文 • 上一篇    下一篇

衍生化β-环糊精手性固定相液相色谱拆分和测定药片中的阿替洛尔对映体

程彪平, 李来生, 周仁丹, 聂桂珍, 张宏福   

  1. 南昌大学分析测试中心, 江西 南昌 330047
  • 收稿日期:2014-07-09 修回日期:2014-08-21 出版日期:2014-11-08 发布日期:2014-10-31
  • 通讯作者: 李来生,E-mail:lilaishengcn@163.com.
  • 基金资助:

    国家自然科学基金项目(21165012);江西省自然科学基金项目(2010GZH0089);江西省教育厅科技项目(GJJ11274).

Enantioseparation and determination of atenolol enantiomers in tablets on a β-cyclodextrin-based chiral stationary phase by high performance liquid chromatography

CHENG Biaoping, LI Laisheng, ZHOU Rendan, NIE Guizhen, ZHANG Hongfu   

  1. Center of Analysis and Testing, Nanchang University, Nanchang 330047, China
  • Received:2014-07-09 Revised:2014-08-21 Online:2014-11-08 Published:2014-10-31

PDF

207

摘要：

以有序介孔材料(SBA-15)为基质,制备了一种二硝基苯醚化β-环糊精键合SBA-15液相色谱手性固定相(NESP)。优化了流动相和温度等色谱条件,在极性有机溶剂模式下,采用实验室自制的手性柱,实现了阿替洛尔对映体的快速拆分。优化的流动相组成为乙腈/甲醇/冰醋酸/三乙胺(90:10:2.5:3.0,v/v/v/v),流速为0.5 mL/min,柱温为20 ℃,检测波长为275 nm。在上述色谱条件下,阿替洛尔对映体的分离度为1.73,分析时间约为20 min。阿替洛尔药片经甲醇提取并直接进样分析,实现了阿替洛尔片剂中对映体含量的测定。阿替洛尔的两对映体的质量浓度在2.5~100 mg/L范围内呈良好的线性关系(r分别为0.9992和0.9989)。采用标准添加法测得两对映体在片剂中的回收率为94.60%~97.24%。样品测定结果的日内和日间相对标准偏差(RSD)分别不大于0.92%和1.86%(n=5)。按3倍信噪比确定出最小检测质量浓度为0.2 mg/L。该方法简便、选择性好、回收率较高,自制环糊精手性柱可降低测试成本,在手性药物的快速质量监测和药代动力学研究中具有良好的应用前景。

关键词: β-环糊精键合SBA-15固定相, β-受体阻滞剂, 阿替洛尔, 对映体含量测定, 高效液相色谱法, 片剂

Abstract:

A novel dinitrophenyl ether β-cyclodextrin-bonded chiral stationary phase (NESP) for HPLC was prepared with ordered mesoporous SBA-15 as matrix. The fast enantioseparation of atenolol enantiomers on the new stationary phase was achieved through the optimization of mobile phase composition, column temperature and other factors in polar organic solvent mode. The optimized composition of mobile phase was acetonitrile/methanol/glacial acetic acid/triethylamine (90:10:2.5:3.0, v/v/v/v) at the flow rate of 0.5 mL/min. The column temperature was set at 20 ℃. The detection wavelength was 275 nm. The resolution of atenolol enantiomers was 1.73 with a rather short analysis time, about 20 min, under the above conditions. The atenolol was extracted with methanol from the tablets and analyzed by direct injection for HPLC. A new quantitative method of atenolol enantiomers in tablets was established after the condition optimization. The good linear relationships for two atenolol enantiomers were observed in the range of 2.5-100 mg/L with r of 0.9992 and 0.9989, respectively. The recoveries of atenolol enantiomers in tablet samples were 94.60%-97.24%. The relative standard deviations (RSDs) of this method were not greater than 0.92% for intra-day and 1.86% for inter-day, respectively. The detection limits (S/N=3) of concentrations were less than 0.2 mg/L for both enantiomers. The established method is simple and of high selectivity, high recovery and low cost for enantiomer analysis by using homemade cyclodextrin-based chiral column. It has a good application prospect for the fast quality control and the pharmacokinetics study of chiral drugs.

Key words: β-adrenergic blockers, β-cyclodextrin-bonded SBA-15 stationary phase (NESP), atenolol, high performance liquid chromatography (HPLC), quantification of enantiomers, tablets

中图分类号: