第 53 卷第 3 期 Vol. 53 No. 3 2023 年 6 月 Jun 2023

所属栏目：分析与测试 手性HPLC法分析双乙酰科立内酯对映异构体

赵春影1，2，王淑红2，崔佰吉1，杨威龙1，孟繁伟1，蔡建辉1，修志明1* （1. 吉林医药学院，吉林 吉林 132013；2. 长春百纯和成医药科技有限公司，吉林 长春 130012）

摘　要：建立了前列腺素中间体双乙酰科立内酯对映异构体的手性高效液相色谱测定方法。采用硅胶表面涂覆有纤维素-三（3，5-二甲基苯基氨基甲酸酯）的手性色谱柱（OD-H，4.6 mm×250 mm，5 μm），以正己烷-异丙醇（V∶V=80∶20）为流动相，流速1.0 mL/min，柱温40 ℃，检测波长205 nm，外标法测定对映异构体超量值。结果双乙酰科立内酯对映异构体分离度为3.5，（+）-双乙酰科立内酯在0.199~3.980 mg/mL（R2=0.999 4）、（-）-双乙酰科立内酯在0.198~3.960 mg/mL（R2=0.999 4）浓度范围线性关系良好。（+）-双乙酰科立内酯低、中、高浓度平均加样回收率（RSD）分别为99.38%（0.43%）、99.30%（0.88%）、100.10%（0.51%），（-）-双乙酰科立内酯低、中、高浓度平均加样回收率（RSD）为99.76%（0.86%）、100.07%（0.26%）、99.27%（0.20%）。3批样品平均对映异构体超量值为4.75%、70.10%、-75.33%。方法简便、快速，能准确测定双乙酰科立内酯对映异构体超量值，为前列腺素药物手性中间体提供新的分离和检测方法。

关键词：HPLC；手性；双乙酰科立内酯；对映异构体超量

中图分类号：R917　　文献标识码：A　　文章编号：1009-9212（2023）03-0062-06

Determination of Diacetylation Corey Lactone Enantiomers by Chiral HPLC

ZHAO Chun-ying1,2, WANG Shu-hong2, CUI Bai-ji1, YANG Wei-long1, MENG Fan-wei1, CAI Jian-hui1, XIU Zhi-ming1* (1. Jilin Medical University, Jilin 132013, China; 2. Changchun BC & HC Pharmaceutical Technology Co., Ltd., Changchun 130012, China)

Abstract：A method for determination of the prostaglandin intermediates diacetylation corey lactone enantiomers by chiral HPLC were established. The optimal chromatographic conditions were as follows: chiral column (OD-H, 4.6 mm×250 mm, 5 μm) coated with Cellulose-tri(3,5-dimethylphenylcarbamate), mobile phase: n-hexane-isopropyl alcohol (V∶V=80∶20), flow rate 1.0 mL/min, column temperature 40 ℃, detection wavelength 205 nm, the enantiomeric excess value was calculated by external standard method. The results showed that the resolution between the corey lactone diol enantiomers was 3.5, and (+)-diacetylation corey lactone had a good linear relationship (R2=0.999 4) in the concentration range of 0.199~3.980 mg/mL as well as (-)-diacetylation corey lactone in the concentration range of 0.198~3.960 mg/mL (R2=0.999 4). The average recoveries (RSD) of (+)-diacetylation corey lactone at low, medium and high concentrations were 99.38%(0.43%), 99.30%(0.88%), 100.10%(0.51%). The average recoveries (RSD) of (-)-diacetylation corey lactone at low, medium and high concentrations were 99.76%(0.86%), 100.07%(0.26%), 99.27%(0.20%). The average enantiomeric excess values of three samples were 4.75%, 70.10%, -75.33%. The established method is simple, rapid and accurate, and can accurately determine the enantiomeric excess value of diacetylation corey lactone enantiomers. It provides a new method for the separation and detection of chiral intermediates of prostaglandin drugs.

Key words：HPLC; chiral; diacetylation corey lactone; enantiomeric excess

基金项目：吉林省科技厅项目（20200708090YY）。

作者简介：赵春影（1978—），女，吉林松原人，工程师，研究方向：前列腺素类药物分析（E-mail：3464245416@qq.com）。

联 系 人：修志明，教授，硕士生导师，研究方向：前列腺素药物筛选与设计（E-mail：Xiuzm10@mails.jlu.edu.cn）。

收稿日期：2023-05-05