毛细管GC法测定头孢地尼中5种残留的有机溶剂  

Determination of five residual organic solvents in Cefdinir by CGC

作　　者：谢赞[1] 史颖[1] 耿佳[1] 何晓燕[1] 

机构地区：[1]石药集团中奇制药技术(石家庄)有限公司,河北石家庄050035

出　　处：《华西药学杂志》2012年第1期96-97,共2页West China Journal of Pharmaceutical Sciences

基　　金：国家科技支撑计划(No.2007BAI26B04)

摘　　要：目的建立头孢地尼中5种残留有机溶剂(甲醇、三乙胺、乙腈、甲苯、N,N-二甲基乙酰胺)的分离测定方法。方法采用GC法测定,毛细管柱为HP-FFAP(30 m×0.53 mm,1.00μm),以氮气为载气,FID检测器,采用程序升温,柱温为80℃,保持5 min,以20℃.min-1升至200℃,保持5 min,进样口温度为200℃,检测器温度为250℃,分流直接进样,用外标法计算残留溶剂的含量。结果 5种残留成分的峰面积和浓度在测定范围内均具有良好的线性关系,进样精密度的RSD<4.0%,平均回收率为97.1%～99.4%。结论所用方法简单准确、灵敏度好,适用于同时测定头孢地尼中5种残留的有机溶剂。OBJECTIVE To establish a capillary gas chromatography method for the determination of five residual organic solvents（methanol,triethylamine,acetonitrile,methylbenzene and n,n-dimethylacetamide） in Cefdinir.METHODS Residual organic solvents in Cefdinir were determined by direct injection on a HP-FFAP capillary column（30 m×0.53 mm,1 μm） with a FID detector.The carrier gas was nitrogen gas.The injector temperature was 200 ℃ and the detector temperature was 250 ℃.The column temperature program was initial temperature 80 ℃（hold 5 min）,with the increase rate of 20 ℃·min-1 to 200 ℃（maintaining for 5 min）.The conent of residual solvents were calculated by external standard method.RESULTS The calibration curves of five residual organic solvents showed good linearity,and the RSD were all less than 4.0%.The average recoveries were 97.1%-99.4%.CONCLUSION The method is simple,accurate and sensitive,and can be used for detection of the five residual solvents in Cefdinir.

关 键 词：头孢地尼 毛细管气相色谱法 残留溶剂 

分 类 号：R917[医药卫生—药物分析学]