【摘要】 目的　用气相色谱的顶空进样法建立布洛芬中的残留溶剂乙醇和 1,2 二氯乙烷的测定方法。方法　使用配置顶空进样器的气相色谱仪 ,采用HP - 6 2 4 (94 %二甲基聚硅氧烷和 6 %氰丙基苯聚硅氧烷 ) ,0 .5 3mm× 30m色谱柱 ,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的含量。结果　布洛芬中有残留乙醇检出 ;标准曲线的线性范围 :乙醇为0 .4 3～ 4 2 .9μg·mL-1(r =0 .9994 ) ,1,2 二氯乙烷为 0 .0 2 1～ 2 .14 μg·mL-1(r =0 .9972 ) ;定量限乙醇为 0 .4 μg·mL-1,1,2 二氯乙烷为 0 .0 5 μg·mL-1;平均回收率乙醇为 95 .0 % (RSD =2 .0 % ,n =5 )和 1,2 二氯乙烷为 98.8% (RSD =2 .7% ,n =5 ) ;结论　本方法简便、灵敏度高 ,重复性好 ,结果准确更多还原

【Abstract】 OBJECTIVE To establish a method for determining residual solvents such as ethanol and 1,2 dichloroethane in ibuprofen by headspace gas chromatography.METHOD The GC was equipped with a headspace injector and a flame ionization detector. A 0.53 mm×30 m HP-624 chromatographic column (coated with 94% dimethylpolysiloxane and 6% cyanopropylpolysiloxane stationary phase) was adopted.The carrier gas was nitrogen.The assay of residual solvents were calculated according to the external standard method.RESULTS Only ethanol was found in the sample of ibuprofen. The standard curves were linear over the ranges of 0.43～42.9 μg·mL -1 ( r =0.999 4) for ethanol and 0.02～2.14 μg·mL -1 ( r =0.997 2)for 1,2 dichloroethane,respectively.The limits of quantitation were 0.4 μg·mL -1 for ethanol and 0.05 μg·mL -1 for 1,2 dichloroethane,respectively.The average recoveries were 95.0%( RSD =2.0%, n =5) for ethanol and 98.8%( RSD =2.7, n =5)for 1,2 dichloroethane.CONCLUSION This method appeared to be sensitive,accurate,repeatable and easy to op erate.更多还原