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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%。
A capillary gas chromatography was developed for the determination of methanol, acetone, isopropanol, methylene chloride, isopropyl ether and ethyl acetate in clopidogrel hydrogen sulfate. The samples were pretreated with magnesia. DB-624 capillary column was used to program temperature and FID detector. The equilibrium temperature was 70 ℃ and the equilibrium time was 30 min. The above solvents showed good linearity in the range 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, and the recovery rates were 100.4%, 101.2% and 100.5 %, 98.2%, 99.2% and 99.6% respectively, with RSD less than 2.0%.