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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 establish a method for the determination of residual organic solvents in di (n-butyl) tin bis (2, 6-difluorobenzoylhydroxamate) Methods The capillary gas chromatography, FID detector and DB-1 capillary column were used. The column temperature was 50 ℃, the inlet temperature was 200 ℃, the detector temperature was 220 ℃, the flow rate was 2.0 mL.min-1 and the split ratio was 50:1 , 1,2 - dichloroethane as the internal standard solvent residual amount. The results showed that methanol, n-hexane and toluene showed a good linearity in the range of the concentrations investigated. The linear range was 9 ~ 375μg.mL-1 (r = 0.999 8), 0.87 ~ 36.25μg.mL-1 The average recoveries were 99.1% (RSD = 2.5%), 98.3% (RSD = 2.7%) and 99.7% (RSD = 1.3%), respectively. Conclusion The method is rapid, simple and accurate. It can be used for the determination of organic solvent residues in di-n-butyltin di (2,6-difluorobenzoylhydroxamate).