摘要
目的:开发一个高灵敏度、高精确度的静态顶空气相色谱法测定原料药硫酸氢氯吡格雷中有机溶剂残留量.方法:以DMF为溶剂,Agilent DB-624毛细管柱(60 m×0.53 mm,3.0μm)为色谱柱,氮气为载气,FID检测器,外标法测定硫酸氢氯吡格雷中甲醇、丙酮、异丙醇、乙腈、二氯甲烷、正己烷、乙酸异丙酯和甲苯的残留量.结果:在最优条件下,上述8种溶剂均能得到良好的分离度,空白无干扰;检测浓度在所考察的范围内与峰面积具有良好的线性,R2=0.998 5～0.999 7;精密度试验RSD均小于5.0%;准确度试验回收率在90.0%～107.0%范围内.结论:本色谱方法简便、准确。
Objective： To develop a precise static headspace gas chromatography method for determination of residual solvents in the drug substance of Clopidogrel Bisulfate. Methods ： The sample was dissolved in N, N-dimethylformamide. An Agilent DB -624 capillary column（60 m x 0.53 mm, 3.0um）, using N2 as the carrier gas and FID as the detector, was used to separate methanol, acetone, propanol, acetonitrile, dichloromethane, n-hexane, isopropyl acetate and toluene in drug substance of Clopidogrel Bisulfate. Results： Complete baseline separation of the eight solvents with no interference in the blank sample was obtained under the optimized conditions ; good linearity （ R^2 = 0. 998 5 - 0. 999 7 ） with excellent precision （ RSD less than 5.0% ） and accuracy （ recovery in the range of 90.0% ~ 107.0% ） were also observed in the investigated concentration range. Conclusions ： The proposed method is simple, accurate, sensitive, and can be used for the determination of residual solvents in the drug substance of Clopidogrel Bisulfate.
出处
《晓庄学院自然科学学报》
CAS
北大核心
2013年第1期58-62,共5页
Journal of Natural Science of Hunan Normal University
关键词
静态顶空气相色谱
残留溶剂
硫酸氢氯吡格雷
原料药
Static headspace gas chromatography
Residual solvent
Clopidogrel Bisulfate
drug substance
