顶空毛细管气相色谱法检测加替沙星中有机溶剂残留量
投稿时间:2009-08-16    点此下载全文
引用本文:蔡林,晏菊姣,李恒.顶空毛细管气相色谱法检测加替沙星中有机溶剂残留量[J].药学实践杂志,2009,27(5):365~366,387
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作者单位
蔡林 中国人民解放军第181医院,广西桂林541002 
晏菊姣 武汉市药品检验所,湖北武汉430012 
李恒 武汉市药品检验所,湖北武汉430012 
中文摘要:目的:建立加替沙星原料药中乙醇、乙腈、二氯甲烷、乙酸乙酯、甲苯5种有机溶剂残留量的测定方法。方法:采用顶空毛细管气相色谱法,程序升温,色谱柱为DM-624毛细管色谱柱,载气为高纯氮,FID检测器,90%N,N-二甲基甲酰胺水溶液为溶解介质,检测了加替沙星原料药中的乙醇、乙腈、二氯甲烷、乙酸乙酯、甲苯的残留量。结果:5种溶剂残留均达到良好分离,在所考察的浓度范围内具有良好线性,r=0.999 7~0.999 9,乙醇、乙腈、二氯甲烷、乙酸乙酯、甲苯的检测限均小于3μg/g,精密度RSD均小于5%,平均回收率为94.8%~98.6%。结论:本试验建立的方法简单、快捷且灵敏度高,可以用于加替沙星中乙醇、乙腈、二氯甲烷、乙酸乙酯、甲苯5种有机溶剂残留量的测定。
中文关键词:原花青素  PC12细胞  细胞凋亡
 
Determination of residual solvents in gatifloxacin by headspace capillary gas chromatography
Abstract:Objective:To establish a method for determination of five residual solvents in gatifloxacin.Methods: The residual organic solvents which are ethanol,acetonitrile,dichloromethane,ethyl acetate,toluene were quantitatively determined by headspace GC on DM-624 column,90%DMF as solvent media,with FID detector,high purity nitrogen as the carrier gas.Results: Five residual solvents were completely separated.There was a good linearity(r=0.999 7~0.999 9).The detection limit of ethanol,acetonitrile,Dichloromethane,ethyl acetate,toluene were all less than 3μg/g;the RSD of precision was less than 5%;the average recovery rate of the preparation was in the range of 94.8%~98.6%.Conclusion:The method is simple,rapid,sensitive and can be used for the quality control of gatifloxacin.
keywords:gatifloxacin  residual solvents  headspace capillary gas chromatography
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