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目的:建立测定抗癌原料药二-(2,4-二氟苯甲酰异羟肟酸)二苯基合锡(DPDFT)中的有机溶剂残留量的方法。方法:采用毛细管气相色谱法,FID检测器,Agilent HP-5(30 m×0.32 mm×0.25μm)毛细管柱,柱温30℃,进样口温度为200℃,检测器温度为220℃,流速为31.90 mL.min-1,分流比为20∶1,以1,2-二氯乙烷为内标,甲苯为溶剂,测定有机溶剂残留量。结果:甲醇、正己烷、醋酸乙酯在考察的浓度范围内线性关系良好,线性范围分别为150～450μg.mL-1(r=0.999 7),14.5～43.5μg.mL-1(r=0.999 9),250～750μg.mL-1(r=0.999 9),平均加样回收率分别为99.6%(RSD=1.0%),100.0%(RSD=1.5%),99.0%(RSD=1.0%)。结论:该方法快速、简便、结果准确,可用于二-(2,4-二氟苯甲酰异羟肟酸)二苯基合锡中的有机溶剂残留量的测定。
OBJECTIVE: To establish a method for the determination of organic solvent residues in the anti-cancer drug di (2,4-difluorobenzoylhydroxamate) diphenyl tin (DPDFT). Methods: The column temperature was 30 ℃, the inlet temperature was 200 ℃, the detector temperature was 220 ℃, and the flow rate was determined by capillary gas chromatography, FID detector and Agilent HP-5 (30 m × 0.32 mm × 0.25 μm) 31.90 mL.min-1, the split ratio was 20: 1, 1,2-dichloroethane as internal standard and toluene as solvent, the residual organic solvent was measured. Results: The calibration curves of methanol, n-hexane and ethyl acetate showed good linearity in the range of 150-450 μg.mL-1 (r = 0.999 7) and 14.5-43.5 μg.mL-1 (r = 0.999 (RSD = 1.0%), 100.0% (RSD = 1.5%), 99.0% (RSD = 1.0%) and the mean recoveries were 99.6% . Conclusion: The method is rapid, simple and accurate. It can be used for the determination of organic solvents in bis (2,4-difluorobenzohydroxamic acid) diphenyltin tin.