顶空气相色谱法测定克林霉素磷酸酯中溶媒残留量

Determination of Residual Solvents in Clindamycin Phosphate by Headspace GC Method

目的:建立克林霉素磷酸酯药物中溶媒残留量测定方法。方法:采用顶空进样法,FID检测器,DB-624毛细管色谱柱,初温40℃(保持5min),以10℃/min升温至150℃(保持4min)进行检测。结果:甲醇、乙醇、丙酮、四氢呋喃、吡啶、甲苯检测质量浓度在50～500μg/mL;二氯甲烷在5～50μg/mL;1,2-二氯乙烷在2.5～10μg/mL范围内峰面积响应值与浓度线性关系良好,平均回收率分别为:98.00%,98.00%,99.00%,100.00%,97.00%,102.00%,103.00%和103.00%。结论:本方法学灵敏、准确,适用于克林霉素磷酸酯原料药中有机溶剂残留量的测定。

Objective： To establish a method for determination of the residual solvents in clindamycin phosphate by headspace GC method. Methods： With headspace method, FID detector, DB-624 capillary column, holding at 40 ℃ for 5 minutes, increasing to 150 ℃ at 10 ℃/min and holding for 4 minutes. Results： The linearity is good at 50～500 μg/mL for methanol, ethanol, acetone, tetrahydrofuran, pyridine and toluene, 5～50 μg/mL for methylenechloride, and 2.5～10 μg/mL for 1,2-dichloroethane. The average recovery is 98.00%,99.00%, 100.00%, 97.00%, 102.00%, 103.00%, 10.00% respectively. Conclusion： The method is sensitive, accurate, reproducible and specified for determination of the residual solvents in clindamycin phosphate.