顶空气相色谱法测定原料药他唑巴坦中残留溶剂  

HS-GC determination of residual solvents in the drug substance of tazobactam

作　　者：梁祈[1] 罗卓雅[1] 李晨辉[1] 李延志[1] 张炫[2] 陈韵正[2] 

机构地区：[1]广东省药品检验所,广州510180 [2]中山大学药学院,广州510070

出　　处：《药物分析杂志》2007年第8期1274-1277,共4页Chinese Journal of Pharmaceutical Analysis

基　　金：国家药典会资助专项课题(国药典发[2005]146号)

摘　　要：目的:建立原料药他唑巴坦中残留溶剂:甲醇、乙醇、乙醚、丙酮、甲基异丁基酮、二氯甲烷、三氯甲烷和甲苯的限度检查的测定方法。方法:顶空气相色谱法,氢火焰离子化检测器,以5%二乙醇胺溶液为溶剂,丁酮为内标,色谱柱为石英毛细管色谱柱:HP-1(30 m×0.32 mm,膜厚1.05μm)。结果:9种残留溶剂在对应于限度的50%～150%浓度范围内有良好的线性关系(r=0.9927～0.9999),平均回收率为95.4%～111.0%。结论:方法简单、可靠,精确,可用于原料药残留溶剂含量控制。Objective： An HS - GC method was established for the determination of residual solvents ： methanol, ethanol, acetone, ethyl ether, dichloromethane, chloroform, methylisobutyl ketone and toluene in the drug substance of tazobactam. Method ：Using 5% diethanolamine as the solvent and butanone as the internal standard,the determination was performed with an Headspace - gas chromatography with a HP - 1 capillary column （30 m × 0. 32 mm, thick 1.05 μm） and an FID. Results：The correlation coefficients of linearity ranged from 0.9927 to 0. 9999 for the four residual solvents within the concentration of 50% to 150% of relative individual limit specified. Conclusion： The method appears simple, dependable and accurate. It can be applied to the quality control of drug substance of tazobactam.

关 键 词：顶空气相色谱法 他唑巴坦 甲醇 乙醇 乙醚 丙酮 甲基异丁基酮 二氯甲烷 三氯甲烷 甲苯 

分 类 号：R917[医药卫生—药物分析学]