三种1,4-二氢吡啶类药物的双水相手性萃取拆分研究  

Chiral Separation of Three 1,4-dihydropyridine Drugs by Aqueous Two-phase Chiral Extraction

作　　者：樊轻亚[1] 王万好 程晓梅 FAN Qingya;WANG Wanhao;CHENG Xiaomei(Xinyang Vocational and Technical College,Xinyang464000,Henan,China;Henan Tongyuan Pharmaceutical Co.,Ltd.,Xinyang464000,Henan,China)

机构地区：[1]信阳职业技术学院,河南信阳464000 [2]河南同源制药有限公司,河南信阳464000

出　　处：《四川化工》2024年第5期1-7,11,共8页Sichuan Chemical Industry

基　　金：河南省高等学校重点科研项目(23B350004);信阳市科技局软科学研究项目(20220074);信阳职业技术学院校级重点科研项目(LXZD221201);中共河南省委教育工委高校“双带头人”教师党支部书记工作室建设项目。

摘　　要：建立了一种以乙醇/硫酸铵作为双水相体系拆分三种1,4-二氢吡啶类手性对映体的方法。采用单因素实验分别考察了手性识别剂的种类、识别剂的浓度、待分离组分的浓度、pH值等几个方面的影响,确定了最佳分离条件:体系pH值为3,ME-β-CD浓度为0.3 mmol/L,L-酒石酸辛酯浓度为0.4 mmol/L,三种1,4-二氢吡啶类药物浓度均为0.4 mmol/L。以0.1%三乙胺正己烷-0.1%三乙胺乙醇(90:10)为流动相分离三种1,4-二氢吡啶类药物对映体,并考察了三种药物对映体的检出限、线性范围、回收率等。结果表明,三种药物对映体的检出限在0.020~0.035 mg/L之间,相关系数均不低于0.999,方法的线性关系良好,回收率为92.2%~105.3%,相对标准偏差为0.53%~1.87%。该方法准确、简便,可满足三种药物及其制剂的拆分及含量测定。A method was established for the separation of three 1,4-dihydropyridine chiral enantiomers using ethanol/ammonium sulfate as a biphasic system.Single factor experiments were conducted to investigate the effects of the type of chiral recognition agent,recognition agent concentration,concentration of the components to be separated,pH value,and other factors.The optimal separation conditions were determined as follows:system pH value of 3,ME-β-CD concentration of 0.3 mmol/L,L-tartrate octyl ester concentration of 0.4 mmol/L,and three1,4-dihydropyridine drug concentrations of 0.4 mmol/L.Three 1,4-dihydropyridine drug enantiomers were separated using 0.1% triethylamine n-hexane-0.1% triethylamine ethanol(90:10) as the mobile phase,and the detection limits,linear ranges,and recovery rates of the three drug enantiomers were investigated.The results showed that the detection limits of the enantiomers of the three drugs were between 0.020~0.035 mg/L,and the correlation coefficients were not less than 0.999.The linear relationship of the method was good,with a recovery rate of 92.2%~105.3% and a relative standard deviation of 0.53%~1.87%.This method is accurate,simple,and can be used for the separation and content determination of three drugs and their formulations.

关 键 词：1 4-二氢吡啶类药物 双水相体系 手性萃取 分离条件 

分 类 号：TQ460.1[化学工程—制药化工]