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机构地区:[1]天津中医药大学,天津300193 [2]天津药物研究院分析测试中心,天津300193
出 处:《现代仪器与医疗》2016年第3期67-69,共3页Modern Instruments & Medical Treatment
摘 要:目的:建立伊潘立酮起始原料中1,2-二氯乙烷残留溶剂的测定方法。方法:采用顶空进样毛细管气相色谱法。色谱柱:Agilent DB-624毛细管柱(30m×0.53mm×3.0μm);程序升温;检测器:电子捕获检测器(ECD),温度:250℃;恒压:2.5psi;载气为高纯氮气。结果:1,2-二氯乙烷在0.55-2.00μg/mL浓度范围内线性关系良好(r=0.9999),平均回收率为101.1%;定量限为2.75ppm;检测限为0.75ppm。结论:建立的方法操作简便、灵敏度高,结果准确,可有效检测伊潘立酮起始原料中一类溶剂1,2-二氯乙烷的残留量。Objective: To establish the method for the determination of 1,2-dichloroethane in iloperidonestartingmaterial. Methods: Headspace capillary gas chromatography. The determination was performed on Agilent DB-624capillary column by temperature programming.The temperature of electron capture detector was set at 250℃,steadypressure was set at 2.5psiand high purity N2was used as carrier gas. Results: The good linear range of 1,2-dichloroethaneorganic solvent had been obtained at 0.55μg / ml - 2.00μg / ml concentration range(r=0.9999)with average recoveryof 101.1%.The limit of quantification was2.75ppm. The limit of detection was0.75ppm. Conclusion: The establishedmethod is simple, sensitive, accurate,and it can be effectively used in the determination of 1,2-dichloroethaneiniloperidonestarting material.
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