美托拉腙中有机溶剂残留量的测定  

GC Determination of Residual Organic Solvents in Metolazone

作　　者：张君[1] 王飞利[1] 王胜强[2] 柴晓华[1] 王文侠[3] 石梅[1] 

机构地区：[1]西北大学化工学院,西安710069 [2]西安近代化学研究所,西安710065 [3]西安力邦制药有限公司,西安710075

出　　处：《理化检验（化学分册）》2007年第12期1012-1014,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：陕西省科技厅自然科学基金资助项目(2006B02);西北大学科学研究基金(03NW23)

摘　　要：建立美托拉腙中异丙醇、乙醇、1,4-二氧六环和正丁醇4种有机溶剂残留量的气相色谱测定方法。用PEG-20M毛细管色谱柱(0.53 mm×30 m),采取程序控制柱温升温,在27.75 min内柱温从40℃经90℃升至180℃。采用FID检测器,检测器温度为250℃,进样口温度为145℃;氮气为载气,流速1.5 mL.min-1;氢气流速为35 mL.min-1,空气流速为350 mL.min-1,尾吹气流速为46 mL.min-1,四种有机溶剂完全分离。所得4种溶剂的线性回归方程证实了峰面积与浓度呈良好的线性关系,其相关系数在0.999 3至0.999 8之间。测定了方法的检出限(S/N=3)依次为0.25,5.89,1.66,2.47 mg.L-1,方法的测定限(S/N=10)依次为17.57,10.99,8.51,6.11 mg.L-1,回收率试验的结果在97.9%~101.5%之间。Four residual organic solvents,i.e.iso-propanol,ethanol,1,4-dioxane and n-butanol in the drug metolazone were determined by gas chromatography,with PEG-20M capillary column(30 m×0.53 mm) and FID detector under programmed column temperature control,raising from 40 ℃ through 90 ℃ to 180 ℃ within 27.75 min.Temperature at the detector was 250 ℃ and at the sample injector was 145 ℃.Nitrogen was used as the carrier gas with flow-rate of 1.5 mL·min-1.Flow-rates used for hydrogen,air and make-up gas were 35,350 and...

关 键 词：气相色谱法 毛细管色谱柱 有机溶剂残留量 美托拉腙 

分 类 号：R927[医药卫生—药学]