第 49 卷第 4 期Vol. 49 No. 4
2019 年 8 月Aug 2019

所属栏目:分析与测试

柱前手性衍生化HPLC法拆分D,L-高丝氨酸内酯盐酸盐
解银萍,王滢秀,董文凯,柴洪伟* (山东省农药科学研究院 山东省重点实验室,山东 济南 250100)
摘 要:建立了一种简单、快捷的柱前手性衍生高效液相色谱法拆分D,L-高丝氨酸内酯盐酸盐的方法。以邻苯二甲醛(OPA)和N-乙酰基-L-半胱氨酸(NAC)为手性衍生化试剂,流动相为乙腈-醋酸铵水溶液(v ∶ v=10 ∶ 90),色谱柱为WondaSil C18色谱柱,流速0.8 mL·min-1,柱温25℃,在230 nm紫外检测波长下进行检测。L-高丝氨酸内酯盐酸盐与其光学异构体分离度大于3.5,该方法的线性相关系数为0.999 2,相对标准偏差为0.064%,加标回收率为99.25%。
关键词:L-高丝氨酸内酯盐酸盐;柱前衍生;高效液相色谱;手性拆分
中图分类号:O657.7  文献标识码:A  文章编号:1009-9212(2019)04-0070-03
Chiral Separation of D,L-Homoserine Lactone Hydrochloride by HPLC with Chiral Pre-column Derivatization
XIE Yin-ping, WANG Ying-xiu, DONG Wen-kai, CHAI Hong-wei* (Shandong Pesticide Research Institute, Shandong Province Key Laboratory of Chemical Pesticide, Jinan 250100, China)
Abstract:A simple and rapid chiral pre-colum derivation method for the optical purity of L-homoserine lactone hydrochloride was established. After derivatization with OPA and NAC, D, L-homoserine lactone hydrochloride was separated by HPLC. The chiral separation was carried out on a WondaSil C18 chromatographic column with a mixture of acetonitrile and ammonium acetate at a volume ratio of 10 ∶ 90 as mobile phase, a flow rate of 0.8 mL·min-1, a column temperature of 25℃ and the detection wave length of 230 nm. The results showed that the resolution factor was greater than 3.5 for L-homoserine lactone hydrochlorid and its enantiomer; the linear correlation coefficient was of 0.999 2; the standard deviation was of 0.064% and the average recovery was of 99.25%.
Key words:L-homoserine lactone hydrochloride; precolumn derivatization; HPLC; chiral separation
基金项目:山东省农业科学院农业科技创新工程(CXGC2016B12新型农药创制关键技术)。
作者简介:解银萍(1988-),女,山东临沂人,工程师,硕士研究生,研究方向:农药合成工艺开发(E-mail:xieyinping107@163.com)。
联 系 人:柴洪伟,工程师,研究方向:农药合成工艺开发(E-mail:hwchai@aliyum.com)。
收稿日期:2019-08-19