毛细管气相色谱法测定奥美沙坦酯中14种有机溶剂的残留量
投稿时间:2007-05-14    点此下载全文
引用本文:胡建国,刘长海.毛细管气相色谱法测定奥美沙坦酯中14种有机溶剂的残留量[J].药学实践杂志,2007,(5):300~302
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作者单位
胡建国 上海市药品检验所,上海200233 
刘长海 上海市药品检验所,上海200233 
中文摘要:目的:采用高效毛细管气相色谱法,溶液直接进样法测定奥美沙坦酯原料药中甲醇、乙醇、乙醚、丙酮、乙腈、二氯甲烷、正己烷、异丙醚、醋酸乙酯、氯仿、二氧六环、甲苯、二甲基甲酰胺和二甲苯等14种有机溶剂的残留量,并进行方法学的研究。方法:采用6%氰丙基苯基,94%二甲基聚硅氧烷毛细管色谱柱(30m×0.53 mm,涂层厚3μm),程序升温的色谱条件,以二甲亚砜为溶剂,直接进样测定。结果:甲醇、乙醇、乙醚、丙酮、乙腈、二氯甲烷、正己烷、异丙醚、醋酸乙酯、氯仿、二氧六环、甲苯、二甲基甲酰胺和二甲苯呈良好的线性关系。平均回收率良好,最小检测限分别为0.4、0.4、1.6、1.2、0.7、2.0、0.5、1.5、0.8、3.3、0.6、0.3、2.8 ng和0.8 ng。结论:本方法可用于奥美沙坦酯中甲醇等14种有机溶剂的残留量的检测,灵敏度高,重复性好。
中文关键词:奥美沙坦酯  高效毛细管气相色谱法  有机溶剂残留量  溶液直接进样法
 
Determination of fourteen kinds of organic residual in olmesartan medoxomil by capillary gas chromatography
Abstract:Objective:To establish by capillary gas chromatography for the analysis of organic residual in olmesartan medoxomil by direct injection of solution,and compare with the results.Methods:Wide-bore capillary column(30m ×0.53mm) packed with 6% cyanopropylphenyl-94% dimethylpoly-siloxane(deep film 3μm)was used on a programmed column temperature.DMSO was used as solvent,and samples were injected for the analysis.Results:The calibration curves of methanol,ethanol,ether,acetone,acetonitrile,dichloromethane,n-hexane,isopropylether,ethyl acetate,chloroform,dioxane,toluene,dimethylformam-ide and xylene showed good linearity.The average recoveries were good.The detection limits were 0.4 ng,0.4 ng,1.6 ng,1.2 ng,0.7 ng,2.0 ng,0.5 ng,1.5 ng,0.8 ng,3.3 ng,0.6 ng,0.3 ng,2.8 ng和0.8 ng,respectively.Conclusion:The results showed that the method can be used to detect the organic residual in olmesartan medoxomil,the method have high sensitivity and good repetition.
keywords:olmesartan medoxomil  capillary gas chromatography  residual organic solvents  direct injection of solution
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