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

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）.