气相色谱法测定新型抗癌化合物二-(2,4-二氟苯甲酰异羟肟酸)二苯基合锡中有机溶剂残留量

Determination of residual organic solvents in di-phenyl-di-(2,4-difluobenzohydroxamato) tin(Ⅳ) by gas chromatography

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 develop a method for the determination of residual organic solvents in di-phenyl-di-（2,4-difluobenzohydroxamato） tin（Ⅳ）（DPDFT）. METHODS The capillary gas chromatography method was established with FID detector and Agilent HP-5（30 m×0.32 mm×0.25 μm） capillary column at 30 ℃.The temperature at the injector and the detector were 200 ℃ and 220 ℃,respectively.The carrier gas was nitrogen with a flow rate of 31.90 mL· min-1.The split ratio was 20∶1.The 1,2-dichloroethane was used as the internal standard and the toluene was used as the solvent to determine the residual organic solvents. RESULTS Methanol,n-hexane and ethyl-acetate showed a linear range within 150-450 μg·mL-1（r=0.999 7）,14.5-43.5 μg·mL-1（r=0.999 9）,250-750 μg·mL-1（r=0.999 9）.The average recoveries were 99.6%（RSD=1.0%）,100.0%（RSD=1.5%）,99.0%（RSD=1.0%）,respectively. CONCLUSION The method was rapid,simple,accurate and suitable for the analysis of residual organic solvents in di-phenyl-di-（2,4-difluobenzohydroxamato） tin（Ⅳ）.