利福昔明中有机溶剂残留量的测定

Determination of residual organic solvents in rifaximin by GC

目的 建立用气相色谱的顶空进样法测定利福昔明中二氯甲烷的残留量的方法。方法 使用配置顶空进样器的气相色谱仪 ,采用DB 6 2 4毛细管色谱柱 (94 %二甲基聚硅氧烷和 6 %氰丙基苯聚硅氧烷 ) ,0 5 3mm× 30m ,液膜厚度为 3μm ,以氮气为载气 ,FID检测器 ,顶空进样 ,通过外标法计算残留溶剂含量。结果 利福昔明样品中未检出二氯甲烷 ;标准曲线的线性范围为 3 2 80～ 8 5 2 8mg·L-1 (r =0 9998) ;检出限为 0 2mg·L-1 ;平均回收率为 1 0 0 5 % (RSD =2 3% ,n =5 ) ;结论 该方法简便、灵敏度高 ,重复性好 。

AIM A headspace GC method for determination of residual solvents(dichloromethane)in rifaximin was estabished.METHODS The GC was equiped with a headspace injector and a flame ionization detector.A 0 53 mm×30 m DB 624 capillary chromatographic colum(coated with 94% dimethylpolysiloxane and 6% cyanopropylplysiloxane stationary phase)was adopted.The carrier gas was nitrogen.The assay of residual solvents were calculated according to the external standard method.RESULTS Dichloromethane was not found in the sample of rifaximin.The standard curves were linear over the ranges of 3 280～8 528 mg·L -1 ( r= 0 999 8 ).The limits of detection were 0 2 mg·L -1 .The average recoveries were 100 5%(RSD=2 3%, n=5 ).CONCLUSION This method appeared to be sensitive,accurate,repeatable and easy to operate.