학술논문
顶空气相色谱法测定国产米格列奈钙原料药中有机溶剂残留 / Determination of Organic Solvent Residues in Domestic Active Pharmaceutical Ingredients of Mitiglinide Calcium by Headspace Gas Chromatography
Document Type
Academic Journal
Author
Source
中国药业 / China Pharmaceuticals. 30(17):61-64
Subject
Language
Chinese
ISSN
1006-4931
Abstract
目的 建立同时测定国产米格列奈钙原料药中甲醇、乙醇、异丙醇、乙腈、二氯甲烷、正己烷、乙酸乙酯、四氢呋喃、三乙胺等有机溶剂残留量的顶空气相色谱法.方法 色谱柱为DB-624毛细管色谱柱(以6％氰丙基苯基-94％二甲基聚硅氧烷为固定液,60 m×0.53 mm,3μm),程序升温,进样口温度为220℃,检测器为火焰离子化检测器(FID),温度为250℃,载气为氮气,载气流速为2.0 mL/min,分流比为10:1,顶空加热温度为80℃,平衡时间为30 min.结果 甲醇、乙醇、异丙醇、乙腈、二氯甲烷、正己烷、乙酸乙酯、四氢呋喃、三乙胺的质量浓度分别在0.03～0.45 mg/mL,0.05～0.75 mg/mL,0.05～0.75 mg/mL,0.0041～0.0610 mg/mL,0.006～0.089 mg/mL,0.003～0.045 mg/mL,0.05～0.75 mg/mL,0.0073～0.1100 mg/mL,0.002～0.030 mg/mL范围内与峰面积线性关系良好(r均大于0.995);检测限分别为1.50,2.50,1.00,0.41,0.59,0.06,0.50,0.37,0.40μg/mL,定量限分别为3.00,5.00,2.50,2.00,1.20,0.15,1.00,1.50,0.99μg/mL;精密度试验的RSD分别为5.07％,5.46％,5.16％,5.14％,3.91％,4.77％,3.71％,3.75％,4.62％(n=6);平均加样回收率分别为98.73％,98.85％,99.46％,100.91％,95.67％,106.85％,102.35％,100.79％,102.53％,RSD分别为3.17％,3.31％,3.27％,3.34％,2.97％,3.40％,2.78％,2.85％,3.72％(n=6).国内5个厂家的15批次米格列奈钙原料药样品中均未检出上述9种有机溶剂残留.结论 所建立的方法可用于国产米格列奈钙原料药中有机溶剂残留的测定;国产米格列奈钙原料药中有机溶剂残留控制情况较好.