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 。
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 operate.
出处
《中国药学杂志》
EI
CAS
CSCD
北大核心
2002年第7期537-539,共3页
Chinese Pharmaceutical Journal
