同时测定盐酸马尼地平中5种有机溶剂方法研究  

Simultaneous determination of five kinds of organic solvents in the manidipine hydrochloride

作　　者：马桂霞[1] 曹悦兴 王希信[1] 母锐敏[1] 

机构地区：[1]山东建筑大学市政与环境工程学院,山东济南250101 [2]济南利民制药有限责任公司,山东济南250200

出　　处：《山东建筑大学学报》2012年第1期16-19,共4页Journal of Shandong Jianzhu University

基　　金：山东省中青年科学家奖励基金(BS2011SW024);山东建筑大学博士基金(XNBS0910)

摘　　要：建立了顶空气相色谱法同时测定盐酸马尼地平中的甲醇、乙醇、异丙醇、三氯甲烷和甲苯5种有机溶剂残留量的测定方法,并讨论了进样方法、平衡温度、平衡时间、溶剂对测定的影响。分析结果表明,该方法可将5种有机溶剂完全分离,甲醇、乙醇、异丙醇、三氯甲烷和甲苯的最低检测限分别为:1.52μg/mL、1.252μg/mL、0.622μg/mL、0.302μg/mL、0.042μg/mL;回收率为99.2%～101.4%。实验通过采用50%的N,N-二甲基甲酰胺水溶液为溶剂,减少了有机物在有机相中的溶解度,增大了三氯甲烷在顶空气体中的含量,从而提高检测限,达到控制本品质量的目的。The method is put forward of using headspace GC to determine the assay of methanol,ethanol,isopropyl alcohol,chloroform and toluene in Manidipine hydrochloride.The influence are discussed of the injection method,the equilibrium temperature,the equilibrium time and the solvent on the determination.The analysis shows that the method can be completely separated from five kinds of organic solvents.The lowest detection limits methanol,ethanol,isopropanol,chloroform and toluene are 1.52μg/mL,1.252μg/mL,0.622μg/mL,0.302μg/mL and 0.042μg/mL,respectively.Recovery is 99.2%~101.4%.With 50% N,N-dimethyl formamide solution as the solvent,the organic matter solubility is reduced in the organic phase,the chloroform content in the headspace is increased,thereby the detection limit is improved and the control of the quality of the product is achieved.

关 键 词：气相色谱法 盐酸马尼地平 顶空进样 有机溶剂 

分 类 号：R-331[医药卫生]