摘要
目的:建立盐酸氨溴索原料药中乙醇、醋酸和甲苯3种有机溶剂残留量的测定方法。方法:采用直接进样法,二甲基甲酰胺为溶剂。气相色谱条件:采用 DM-624(化学组成:6%氰丙苯基-94%二甲基聚氧硅烷)毛细管气相色谱柱,30m×0.53mm×3.00μm。程序升温:60℃保持3min,以每分钟5℃升至108℃,再以每分钟30℃升至180℃,保持5min。氮气(纯度:99.9999%)为载气,柱前压为42kPa。分流进样,分流比1∶20。进样口温度250℃,FID 检测器,检测器温度270℃。结果:3种溶剂残留均达到良好分离。乙醇、醋酸和甲苯线性范围分别为15.85-396.3μg·mL^(-1)(r=0.9995),38.33-574.9μg·mL^(-1)(r=0.9999),0.8360-20.90μg·mL^(-1)(r=0.9996,);回收率分别为95.2%-101.9%(RSD≤4.3%,n=3),95.0%-102.3%(RSD≤3.9%,n=3),94.8%-102.0%(RSD≤4.8%,n=3);检出限分别小于20μg·g^(-1),20μg·g^(-1),5μg·g^(-1)。结论:本方法简单、快捷且灵敏度高,可以用于盐酸氨溴索中乙醇、醋酸、甲苯3种有机溶剂残留量的控制。
Objective:To establish a method for determination of ethanol,acetic acid and toluene simultaneously in ambroxol hydrochloride.Method:3 residues were separated and identified on DM-624 capillary column(coated with cross-linked 6 percent polycyanopropylphenylsiloxane and 94 percent polydimethylsiloxane),30m×0.53 mm×3.00μm.A temperature programm was applied.The temperature was initialized at 60℃ for 3 min,then raised to 108℃ at a rate of 5℃·min^(-1),subsequently raised to 180℃ at a rate of 30℃·min^(-1) and finally kept for 5 min.Split injection,split ratio 1:20,injector temperature 250℃.Detector:FID,temperature 270℃.N_2 (99.9999%)was used as carrier gas,column press was 42 kPa.Results:The three residues were well resolved.The linear ranges of ethanol,acetic acid and toluene were:15.85-396.3μg·mL^(-1),38.33-574.9μg·mL^(-1),0.83 -20.90μg·mL^(-1),with the correlation coefficients 0.9995,0.9999,0.9996 respectively.The average recoveries of ethanol,acetic acid and toluene were 95.2%-101.9%(RSD≤4.3%,n=3),95.0%-102.3%(RSD≤ 3.9%,n=3),94.8%-102.0%(RSD≤4.8%,n=3).The detect limits of ethanol,acetic acid and toluene were less than 20μg·g^(-1),20μg·g^(-1),5μg·g^(-1).Conclusion:This method is simple,rapid and has good sensitivity.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2005年第4期466-468,共3页
Chinese Journal of Pharmaceutical Analysis
