OBJECTIVE:To establish a method for simultaneous determination of 4 residual organic solvents such as ethanol,dichloromethane,isopropanol and ethyl acetate in lacidipine raw material.METHODS:GC method was adopted.The determination was performed on DB-624 capillary column at the rate of 2.0 mL/min using nitrogen gas as carrier and FID as the detector by temperature programming.The temperature of detector was set at 250 ℃.Carries gas was nitrogen.The split ratio was 10 ∶ 1.The sample size was 10 μL.RESULTS:The linear ranges of ethanol,dichloromethane,isopropanol and ethyl acetate were 0.259 5-2.076 mg/mL (r=0.999 6),0.055 3-0.316 mg/mL (r=0.999 2),0.342 3-1.956 mg/mL (r=0.999 5),0.370 6-2.118 mg/mL(r=0.999 4),respectively.The limits of quantification were 2.96,2.24,4.4,4.44 μg/mL,and the detection limits were 0.887,0.672,1.3,1.32 μg/ mL,respectively.RSDs of precision,stability and reproducibility tests were all lower than 4.0％.The recoveries were 95.00％-101.17％ (RSD=2.19％,n=9),96.22％-104.53％ (RSD=3.27％,n=9),96.20％-104.90％ (RSD=2.41％,n=9),95.60 ％-104.48 ％ (RSD=2.85 ％,n=9).CONCLUSIONS:The method is simple,sensitive and reliable,and is suitable for simultaneous determination of 4 residual organic solvents in lacidipine raw material.%目的:建立同时测定拉西地平原料药中乙醇、二氯甲烷、异丙醇、乙酸乙酯4种有机溶剂残留量的方法.方法:采用气相色谱法.色谱柱为DB-624毛细管柱,程序升温,检测器为氢火焰离子化检测器,检测器温度为250℃,载气为氮气,流速为2.0mL/min,分流比为10∶1,进样量为1.0 μL.结果:乙醇、二氯甲烷、异丙醇、乙酸乙酯检测质量浓度线性范围分别为0.259 5～2.076mg/mL(r=0.999 6)、0.055 3～0.316 mg/mL(r=0.999 2)、0.342 3～1.956 mg/mL(r=0.999 5)、0.370 6～2.118 mg/mL(r=0.999 4);定量限分别为2.96、2.24、4.4、4.44 μg/mL,检测限分别为0.887、0.672、1.3、1.32 μg/mL;精密度、稳定性、重复性试验的RSD＜4.0％;加样回收率分别为95.00％～101.17％(RSD=2.19％,n=9)、96.22％～104.53％(RSD=3.27％,n=9)、96.20％～104.90％ (RSD=2.41％,n=9)、95.60％～104.48％ (RSD=2.85％,n=9).结论:该方法简单、灵敏、可靠,适用于拉西地平原料药中4种有机溶剂残留量的同时测定.
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