摘要
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).
出处
《中国医院药学杂志》
CAS
CSCD
北大核心
2011年第18期1487-1489,共3页
Chinese Journal of Hospital Pharmacy
基金
国家"重大新药创制"科技重大专项(编号:2009ZX09103-104)
国家自然科学基金资助项目(编号:30973603和30772682)
山西医科大学08博士启动基金