顶空固相微萃取-气相色谱法测定匹伐他汀钙原料药中6种溶剂残留  

Determination of Six Kinds of Residual Solvents in Pitavastatin Calcium by Headspace Solid Phase Microextraction Combined with Gas Chromatography

作　　者：程晓昆[1] 祝仕清 王娅莉[1] 张晴[1] 马欢欢[1] 刘月[1] 孙勇军[2] CHENG Xiaokun;ZHU Shiqing;WANG Yali;ZHANG Qing;MA Huanhuan;LIU Yue;SUN Yongjun(New Drug Research and Development Co. , Ltd. , North Chir~ Pharmaceutical Group, Shijiazhuang 050015, China;College of Chemical and Pharmaceutical Engineering, Hebei University of Science and Technology, Shijiazhuang 050018, China)

机构地区：[1]华北制药集团新药研究开发有限责任公司,石家庄050015 [2]河北科技大学化学与制药工程学院,石家庄050018

出　　处：《理化检验（化学分册）》2018年第6期665-668,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：将样品用N,N-二甲基甲酰胺溶解配制成100g·L-1的样品溶液,取样品溶液10mL置于顶空瓶中,于40℃水浴加热5min后,进行固相微萃取,采用聚二甲基硅氧烷萃取头,萃取温度为40℃,吸附时间和脱附时间分别为30,10s。甲醇、四氢呋喃、乙酸乙酯、乙醇、乙腈、甲苯在SE-54毛细管色谱柱上分离,采用火焰离子化检测器。上述6种溶剂的峰面积与其质量浓度在一定范围内呈线性关系,检出限(3S/N)在1.0~2.3mg·L-1之间。加标回收率在95.8%~104%之间,测定值的相对标准偏差(n=8)小于9.0%。The sample was dissolved with N,N-dimethylformamide to prepare a sample solution of 100 g·L-1.The sample solution（10 mL）was taken into a headspace vial and heated in a water bath at 40 ℃ for 5 min.Then solid-phase microextraction was carried out at 40 ℃ using polydimethylsiloxane extraction head,with adsorption time and desorption time of 30,10 s,respectively.Methanol,tetrahydrofuran,ethyl acetate,ethanol,acetonitrile,and toluene were separated on a SE-54 capillary column and detected using a flame ionization detector.Linear relationships were found between peak areas and mass concentrations of the above six solvents within definite ranges,with detection limits（3 S/N）in the range of 1.0-2.3 mg·L-1.Values of recovery obtained by standard addition method ranged from 95.8%to 104%,and RSDs（n=8）were less than 9.0%.

关 键 词：匹伐他汀钙 顶空固相微萃取 气相色谱法 溶剂残留 

分 类 号：O657.7[理学—分析化学]