高效液相色谱法拆分佐匹克隆对映体

文档编号:ZY096    文档字数:10090,页数:21

摘 要：本文建立了佐匹克隆（ZPC）对映体的反相高效液相色谱拆分方法。使用Chiralcel OD-RH(150 mm×4.6mm，5μm)手性柱分离佐匹克隆对映体，考查了不同流动相组分、流动相中乙腈含量、pH值、柱温和流速对手性拆分结果的影响。确立测定的最佳色谱条件为：流动相为乙腈-磷酸二氢钾缓冲液(pH=6.0，V：V=35：65)；流速1.0 mL/min；检测波长为303nm；柱温30℃。结果表明佐匹克隆在0.5-8μg/mL之间呈良好线性关系，线性相关系数R/S-ZPC： r＝1，平均回收率R/S-ZPC分别为98.23%，RSD＝0.48%（n＝9）和99.19%，RSD＝0.52%（n＝9），溶液在24h内稳定。本法操作简便、易行、准确、重复性好。

关键词：佐匹克隆；拆分；高效液相色谱法

Abstracts: This article develop an RP-HPLC method to separate zopiclone(ZPC) enantiomers. A Chiralcel OD-RH (150mm×4.6mm，5μm) chiral column was used to separate zopiclone enantiomers．The influence of the different mobile phase，the CH3CN content，the pH Value，the column temperature and the velocity of flow on chiral separation were studied. The best analytic condition was: the mobile phase was composed of acetonitrile and potassium dihydrogen phosphate (pH=6.0, V：V=35：65) and the flow rate was 1.0 mL/min, the detection wavelength was set at 303nm and the column temperature was 30℃. The rusults showed that the linear rang of zopiclone was 0.5-8μg/mL，the linear correlation of R/ S-ZPC was1，The average recoveries of R/S-ZPC were 98.23% and 99.19%, respectively, with RSD of 0.48% and 0.52% (n=9). The solution was steady within 24h. This method is simple, accurate and with good reproducibility.
Key words: Zopiclone; Separation; High Performance Liquid Chromatography

目  录
中文摘要 …………………………………………………………………………………Ⅰ
英文摘要 …………………………………………………………………………………Ⅱ
目录 ………………………………………………………………………………………Ⅲ
1. 绪论 ……………………………………………………………………………………1
 1.1前言………………………………………………………………………………1
 1.2佐匹克隆简介……………………………………………………………………1
 1.3佐匹克隆对映体拆分文献综述…………………………………………………2
2. 实验部分 ………………………………………………………………………………6
 2.1 仪器和试剂  ……………………………………………………………………6
 2.2 实验试剂配制……………………………………………………………………6
     2.2.1 缓冲溶液配制……………………………………………………………6
     2.2.2 流动相配制………………………………………………………………6
     2.2.3 对照品溶液配制…………………………………………………………6
     2.2.4 样品溶液配制……………………………………………………………7
 2.3 实验方法…………………………………………………………………………7
     2.3.1 不同色谱条件下分离情况的考察………………………………………7
     2.3.2 线性试验…………………………………………………………………7
 2.3.3 精密度试验………………………………………………………………7
 2.3.4 重复性试验………………………………………………………………7
 2.3.5 回收率试验………………………………………………………………7
 2.3.6 溶液稳定性试验…………………………………………………………7
 2.3.7 样品含量测定……………………………………………………………7
3. 结果与讨论 ……………………………………………………………………………8
 3.1 流动相组成对分离的影响………………………………………………………8
 3.2 乙腈体积分数对分离的影响……………………………………………………8
 3.3 柱温对分离的影响………………………………………………………………9
 3.4 流速对分离的影响………………………………………………………………9
 3.5 流动相pH值对分离的影响……………………………………………………10
 3.6 最佳色谱条件的确立 …………………………………………………………10
 3.7 线性试验结果 …………………………………………………………………11
 3.8 精密度试验结果 ………………………………………………………………12
 3.9 重复性试验结果 ………………………………………………………………12
 3.10 回收率试验结果………………………………………………………………13
 3.11 溶液稳定性试验结果…………………………………………………………14
 3.12 含量测定结果…………………………………………………………………14
4. 总结与展望……………………………………………………………………………15
致谢 ………………………………………………………………………………………16
参考文献 …………………………………………………………………………………17

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