顶空气相色谱法测定去氢表雄酮中的残留溶剂  

Determination of Residual Solvents in Prasterone by Headspace Gas Chromatography

作　　者：侯海波 李廿 朱保林 郑建雄 杜金鹏 柳婷婷 付乔 朱小红 HOU Haibo;LI Nian;ZHU Baolin;ZHENG Jianxiong;DU Jinpeng;LIU Tingting;FU Qiao;ZHU Xiaohong(Hubei Zhuxi Humanwell Pharmaceutical Co.,Ltd.,Hubei Shiyan 442300,China)

机构地区：[1]湖北竹溪人福药业有限责任公司,湖北十堰442300

出　　处：《中国医药导刊》2023年第12期1249-1252,共4页Chinese Journal of Medicinal Guide

摘　　要：目的:采用气相色谱(GC)法建立去氢表雄酮中甲醇、丙酮、甲酸乙酯、二氯甲烷、醋酸异丙烯酯残留量的测定方法,旨在为去氢表雄酮的残留溶剂检测提供方法和依据。方法:采用Agilent DB-624型(30 m×0.32 mm×1.8μm)毛细管色谱柱进行测定,程序升温,顶空气相色谱法,火焰离子化检测器(FID),载气为氮气,进样口温度为220℃,检测器温度为250℃,进样体积为1000μL。结果:分别对专属性、重复性、检测限、定量限、线性试验、加样回收试验、耐用性实验、样品测定系统化验证。结果显示,试验结果良好,其中甲醇、丙酮、甲酸乙酯、二氯甲烷、醋酸异丙烯酯残留溶剂在各自的浓度范围内线性关系良好(r=0.9935~0.9995,n=5),平均回收率为98.1%~103.8%,RSD为0.44%~2.10%。结论:该分析方法操作简便、灵敏度高、重复性好、适用性强,结果准确,适用于顶空气相色谱法测定去氢表雄酮中的残留溶剂,为去氢表雄酮的分析检测、质量研究奠定了基础。该方法同样适用于生产工艺中使用甲醇、丙酮、甲酸乙酯、二氯甲烷、醋酸异丙烯酯的其他甾体原料药残留溶剂的检测。Objective:A method for the determination of methanol,acetone,ethyl formate,dichloromethane and isoallyl acetate residues in prasterone was established by gas chromatography(GC)in order to provide methods and basis for the determination of residual solvents in prasterone.Methods:Agilent DB-624(30 m×0.32 mm×1.8μm)capillary column was used for determination.Headspace gas chromatography,flame ionization detector(FID),nitrogen as carrier gas.The inlet temperature was 220℃,and the detector temperature was 250℃.Sample volume was 1000μL.Results:The specificity,repeatability,limit of detection,limit of quantitation,linear test,sample recovery test,durability test and sample detection were systematically verified,and the test results were good.Methanol,acetone,ethyl formate,dichloromethane,isopropenyl acetate residual solvents had good linearity in the range of respective concentrations(r=0.9935-0.9995,n=5).The average recovery rates were between 98.1%-103.8%,RSD:0.44%-2.10%.Conclusion:The method established is simple,sensitive,repeatable and applicable,and the results are accurate.It is suitable for the determination of residual solvents in prasterone by headspace gas chromatography,which lays a foundation for the analysis,detection and quality research of prasterone.The method is also suitable for the detection of residual solvents of other steroid active pharmaceutical ingredients using methanol,acetone,ethyl formate,dichloromethane and isopropenyl acetate in the production process.

关 键 词：去氢表雄酮 顶空气相色谱 残留溶剂 测定 

分 类 号：R917[医药卫生—药物分析学]