硫酸氢氯吡格雷中有机溶剂残留量的顶空毛细管气相色谱法测定

建立了顶空毛细管气相色谱法测定硫酸氢氯吡格雷中的甲醇、丙酮、异丙醇、二氯甲烷、异丙醚与乙酸乙酯.样品采用氧化镁进行预处理,采用DB-624毛细管色谱柱,程序升温,FID检测器,顶空平衡温度70℃,平衡时间30 min.上述溶剂分别在7.5～750、5～500、12.5～1 250、1.5～150、12.5～1 250和12.5～1 250μg/ml浓度范围内线性关系良好,回收率分别为100.4％、101.2％、100.5％、98.2％、99.2％和99.6％,RSD均小于2.0％.

Determination of Residual Organic Solvents in Clopidogrel Hydrogen Sulfate by Headspace Capillary Gas Chromatography

A headspace capillary gas chromatography method was established for the determination of methanol,acetone,isopropanol,dichlormethane,isopropyl ether and ethyl acetate in clopidogrel hydrogen sulfate.The samples were pre-treated with magnesium oxide.A DB-624 capillary column was used with temperature program and FID detector,at injection temperature of 70 ℃ and equilibrium time of 30 min.The calibration curves of these solvents were linear in the concentration ranges of 7.5-750,5-500,12.5-1 250,1.5-150,12.5-1 250 and 12.5-1 250 μg/ml,respectively.The recoveries were 100.4%,101.2%,100.5%,98.2%,99.2% and 99.6%,with RSDs less than 2.0%.