摘要
采用手性多羟基化合物—硼酸络合酸为手性选择剂,建立了分离盐酸莱克多巴胺4个立体异构体的手性毛细管电泳(NACE)方法。实验考察了手性选择剂的种类、浓度和三乙胺浓度对手性分离效果的影响。结果表明,双丙酮-D-甘露糖醇—硼酸络合酸手性选择剂的分离效果最好,优化的缓冲溶液组成为含100 mmol/L双丙酮-D-甘露糖醇、100 mmol/L硼酸和72 mmol/L三乙胺的甲醇溶液。在优化的实验条件下,盐酸莱克多巴胺的4个立体异构体均可以达到基线分离,质量浓度在6.2~200.0μg/mL范围内与峰面积分别呈现良好的线性关系,检测限和定量限分别为0.6μg/mL和2.0μg/mL,加标回收率为97.5%~102.5%,饲料中的提取回收率为66.4%~72.5%。方法可用于盐酸莱克多巴胺4个立体异构体的手性分离和含量测定。
A new method for chiral separation of ractopamine hydrochloride stereoisomers was developed by nonaqueous capillary electrophoresis(NACE).4 chiral stereoisomers of ractopamine hydrochloride were separated by NACE using chiral polyhydroxyls—boric acid complex as chiral selector.In order to achieve good resolution,the effects of the type and concentration of chiral selector and the concentration of triethylamine on the chiral separation were investigated.Results showed that diacetone-D-mannitol—boric acid complex was the best chiral selector.The optimized buffer solution was 100 mmol/L diacetone-D-mannitol,100 mmol/L boric acid and 72 mmol/L triethylamine in methanol.Injections were performed hydrostatically for 5 s at a 17.5 cm height difference.The running voltage and detection wavelength were 20 kV and 224 nm,respectively.The experiments were performed at room temperature.Under the above optimized conditions,4 stereoisomers of ractopamine hydrochloride could all achieve baseline separation.Their concentrations showed good linear relationships with the peak area in the range of 6.2-200.0μg/mL.The detection limits and quantitative limits were 0.6μg/mL and 2.0μg/mL,respectively;the recoveries were 97.5%-102.5%;the extraction recoveries in fodder samples were 66.4%-72.5%.This method is feasible for the separation and determination of4 stereoisomers of ractopamine hydrochloride.
作者
张旭
任怡梦
刘莹
董妙雪
王利娟
闫宏远
张磊
ZHANG Xu;REN Yimeng;LIU Ying;DONG Miaoxue;WANG Lijuan;YAN Hongyuan;ZHANG Lei(Key Laboratory of Pharmaceutical Quality Control of Hebei Province,Institute of Life Science and Green Development,College of Pharmaceutical Sciences,Hebei University,Baoding 071002;Tianjin Alta Scientific Co.,Ltd.,Tianjin 300457)
出处
《分析试验室》
CAS
CSCD
北大核心
2021年第2期125-129,共5页
Chinese Journal of Analysis Laboratory
基金
国家自然科学基金项目(21405031)资助。