摘要
建立了测定醋酸卡泊芬净原料药中甲醇、乙醇、异丙醇、乙腈、二氯甲烷、四氢呋喃和乙酸乙酯等7种残留溶剂的顶空气相色谱法,该法可以将异丙醇与乙腈峰、乙酸乙酯与四氢呋喃峰有效分离并准确定量。采用Inert Cap 624毛细管色谱柱,顶空进样,程序升温,检测器为氢火焰离子化检测器,温度为250℃,进样量为1 mL。实验结果表明:7种溶剂的线性系数均大于0.9999;各溶剂检测限为0.041~0.654μg;精密度实验的RSD均小于10%;平均回收率为95.4%~111.5%。该方法灵敏度高,准确度好,适用于醋酸卡泊芬净原料药中残留溶剂的测定。
A headspace gas chromatographic method was established for the determination of seven kinds of residual solvents in caspofungin acetate API,including methanol,ethanol,isopropanol,acetonitrile,dichloromethane,tetrahydrofuran and ethyl acetate.The peaks of isopropanol and acetonitrile,ethyl acetate and tetrahydrofuran were effectively separated and accurately quantified by this method with Inert Cap 624 capillary chromatographic column,headspace injection,programmed temperature rising,hydrogen flame ionization detector at 250℃ and injection volume 1 mL.The results showed that the linear coefficients of the seven solvents were greater than 0.9999;The detection limits of each solvent were 0.041~0.654μg;RSDs of precision test were all less than 10%;The average recoveries were 95.4%~111.5%.The method has high sensitivity and accuracy,and is suitable for the determination of residual solvents in caspofungin acetate API.
作者
张波
王秀龙
郭朝江
刘志钰
朱兵峰
张贵民
ZHANG Bo;WANG Xiulong;GUO Chaojiang;LIU Zhiyu;ZHU Bingfeng;ZHANG Guimin(Lunan Pharmaceutical Group Co.,Ltd.,Linyi 276000,China;Lunan New Time Biotechnology Co.,Ltd.,Feixian 273400,China)
出处
《发酵科技通讯》
CAS
2022年第4期202-205,235,共5页
Bulletin of Fermentation Science and Technology
关键词
醋酸卡泊芬净
顶空气相色谱法
残留溶剂
caspofungin acetate
headspace gas chromatography
residual solvent
