顶空气相色谱法测定盐酸头孢替安酯原料药中残留溶剂含量

摘要

目的：建立顶空气相色谱法同时测定盐酸头孢替安酯原料药中丙酮、乙酸乙酯、异丙醇、二氯甲烷、乙腈5种残留溶剂。方法采用Agilent DB-624(6％氰丙基苯基-94％二甲基聚硅氧烷固定相)石英毛细管柱(30 m×0.53 mm，3.0μm)，火焰离子化检测仪( FID)检测器，N，N-二甲基甲酰胺( DMF)为溶剂。结果5种残留溶剂在各自的浓度范围内呈现良好的线性关系( r＝0.9996~0.9999，n＝5)，最低检出限范围为0.071~0.847μg；5种残留溶剂检测的稳定性RSD为0.40％~2.12％(n＝3)，平均加样回收率为99.03％~103.33％，RSD为0.54％~3.41％( n＝3)。结论该方法简单、灵敏、可靠，适用于盐酸头孢替安酯原料药中残留溶剂的分析检测。%Objective To establish a method of gas chromatography with head-space sampling for determination of five residual solvents ( acetone, ethyl acetate, isopropanol, dichloromethane, acetonitrile ) in raw material drug of cefotiam hexetil hydrochloride. Methods Agilent DB-624 capillary column(30 m×0.53 mm,3.0 μm)was used,with FID served as detector and DMF as the solvent. Results Linear relationships were obtained for the 5 residual solvents in their respective concentration ranges ( r=0.999 6-0.999 9,n=5) ,and the detection range was from 0.071 to 0.847μg. The stabilities measured as relative standard deviations ( RSD) for the 5 residual solvents were from 0.40% to 2.12% ( n=3) . The average recovery rates were 99.03% to 103.33%,and RSD were 0.54% to 3.41% ( n=3) . Conclusion The method is simple,sensitive and accurate for the residual solvent analysis in raw material drug of cefotiam hexetil hydrochloride.