Simultaneous determination of seven residual solvents in clopidogrel bisulfate by headspace gas chromatography
陈露 1耿雪 1林秋婕 1蔡姗英 1陈赞民1
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作者信息
1. 海南省检验检测研究院,海口 570216
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摘要
目的:建立硫酸氢氯吡格雷原料药中所含7种有机溶剂(甲苯、四氢呋喃、正己烷、甲醇、二氯甲烷、丙酮和异丙醇)残留量的测定方法.方法:以DB-1毛细管柱(30 m ×0.32 mm,3.0 μm)为色谱柱,程序升温,火焰离子化检测器.进样口温度为200℃,分流比为5∶1,检测器温度为270 ℃.载气为高纯N2,恒流控制,流速为4 mL·min-1.顶空进样器的平衡温度为85℃,平衡时间为20 min.结果:7种溶剂均能完全分离,各组分的质量浓度与峰面积呈良好的线性关系(r＞0.999 3),方法的专属性、重复性和准确度均符合要求.结论:本法适用于硫酸氢氯吡格雷原料药中有机溶剂残留量的测定.
Abstract
Objective:A gas chromatography(GC)method was established for the simultaneous determination of seven residual solvents in clopidogrel bisulfate,including methanol,acetone,isopropanol,dichloromethane,n-hexane,tetrahydrofuran and methylbenzene.Methods:The analysis was performed on an Agilent DB-1 capillary column(30 m ×0.32 mm,3.0 μm)under the programmed temperature.The carrier gas was high purity nitrogen,and the flow rate was 4.0 mL·min-1 with constant flow control.The detector was a hydrogen flame ionization detector(FID).The inlet temperature was 200 ℃,the detector temperature was 270 ℃ and the split ratio was 5∶1.The temperature of headspace injector was 85 ℃,and the equilibrium time was 20 min.Results:Seven residual solvents were separated completely.The linear relationship between peak area and the concentration range of seven residual solvents were good enough(r＞0.9993).The results of specificity,precision and recovery met the requirements.Conclusion:This method can be used for the determination of residual organic solvents in clopidogrel bisulfate.
关键词
气相色谱法/顶空进样/硫酸氢氯吡格雷/有机溶剂/残留量/程序升温
Key words
gas chromatography/headspace sampling/clopidogrel bisulfate/organic solvent/residual content/programmed temperature
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