GC测定二-(2,6-二氟苯甲酰异羟肟酸)二正丁基合锡中有机溶剂残留量  

Determination of Residual Organic Solvents in Di-n-butyl-(2,6-difluorobenzohydroxamato) Tin(IV) by GC

作　　者：郑娟[1] 高竹妍[1] 李云兰[1] 李青山[1] 

机构地区：[1]山西医科大学药学院,太原030001

出　　处：《中国现代应用药学》2011年第1期67-69,共3页Chinese Journal of Modern Applied Pharmacy

基　　金：国家"重大新药创制"科技重大专项(2009ZX09103-104);国家自然科学基金资助项目(30973603和30772682);山西医科大学08博士启动基金;山西省回国留学人员科研资助项目(2010-54)

摘　　要：目的建立原料药二-（2,6-二氟苯甲酰异羟肟酸）二正丁基合锡中的有机溶剂残留量的测定方法。方法采用毛细管气相色谱法,FID检测器,DB-1毛细管柱,柱温50℃,进样口温度200℃,检测器温度220℃,流速为2.0 mL.min-1,分流比为50∶1,以1,2-二氯乙烷为内标测定溶剂残留量。结果甲醇、正己烷、甲苯在考察的浓度范围内线性关系良好,线性范围分别为9~375μg.mL-1（r=0.999 8）,0.87~36.25μg.mL-1（r=0.999 7）,2.67~111.25μg.mL-1（r=0.999 8）,平均回收率分别为99.1%（RSD=2.5%）、98.3%（RSD=2.7%）、99.7%（RSD=1.3%）。结论本方法快速、简单、结果准确,可用于二-（2,6-二氟苯甲酰异羟肟酸）二正丁基合锡中的有机溶剂残留量的测定。OBJECTIVE To develop a method for the determination of residual organic solvents in Di-n-butyl-（2,6-difluorobenzohydroxamato）Tin（IV）.METHODS The capillary gas chromatography method was established with FID detector and DB-1 capillary column with 50 ℃.The temperature at the injector and the detector were 200 ℃ and 220 ℃,respectively.The carrier gas was nitrogen with a flow rate of 2.0 mL-min-1.The split ratio was 50∶1.The 1,2-dichloroethane was used as the internal standard to determine the residual organic solvents.RESULTS Methanol,N-hexane and methylbenzene showed a linear range within 9-375 μg-mL-1（r=0.999 8）,0.87-36.25 μg-mL-1（r=0.999 7）,2.67-111.25 μg-mL-1（r=0.999 8）,respectively.The average recoveries were 99.1%（RSD=2.5%）,98.3%（RSD=2.7%）,99.7%（RSD=1.3%）,respectively.CONCLUSION The method was rapid,simple,accurate and suitable for the analysis of residual organic solvents in Di-n-butyl-（2,6-difluorobenzohydroxamato） Tin（IV）.

关 键 词：毛细管气相色谱法 二-(2 6-二氟苯甲酰异羟肟酸)二正丁基合锡 有机溶剂残留 

分 类 号：R917.101[医药卫生—药物分析学]