毛细管气相色谱法同时测定埃索美拉唑镁原料药中8种有机溶剂的残留量

摘要

OBJECTIVE:To develop a method for simultaneous determination of 8 residual organic solvents in esomeprazole magnesium raw material,including ethanol,ethyl acetate,isopropylenzene,methanol,methylbenzene,2-phenyl-2-propanol,dichloromethane and acetonitrile.METHODS:Capillary GC was adopted.The determination was performed on HP-1 column by programmed temperature.The temperature of injector port was 220 ℃,with flame ionization detector at temperate of 250 ℃,using nitrogen as carrier gas,at the flow rate of 4.0 mL/min,with split ratio of 10∶1 and injection volume of 1 μL.RESULTS:The linear ranges of ethanol,ethyl acetate,isopropylenzene,methanol,methylbenzene,2-phenyl-2-propanol,dichloromethane and acetonitrile were 45.2-904 μg/mL(r=0.999 7),45.5-909 μg/mL(r=0.999 7),9.0-180 μg/mL(r=0.999 8),27.1-542 μg/mL(r=0.999 8),8.7-174 μg/mL(r=0.999 7),9.1-183 μg/mL(r=0.999 4),5.8-115 μg/mL(r=0.999 4),3.7-74 μg/mL(r=0.999 4),respectively.The quantitation limits were 4.5,3.0,1.4,2.7,0.6,3.0,3.9,2.8 ng,and the limits of detection were 2.2,1.0,0.4,1.4,0.3,1.0,2.0,1.4 ng,respectively.RSDs of precision tests were all lower than 2.0％.Only ethanol,methanol and methylbenzene were detected in reproducibility test,RSDs of their peak area were lower than 2.0％.The recoveries were 95.6％-104.9％ (RSD=3.3％,n=9),98.7％-102.0％ (RSD=1.1％,n=9),100.0％-103.1％ (RSD=1.1％,n=9),95.7％-104.4％ (RSD=3.0％,n=9),99.3％-104.4％ (RSD=1.7 ％,n=9),95.6％-102.2％ (RSD=2.6％,n=9),95.1％-103.3％ (RSD=2.6％,n=9),97.5％-103.3％ (RSD =1.7 ％,n =9),respectively.CONCLUSIONS:The method is sensitive and simple,and it is suitable for simultaneous determination of 8 residual organic solvents in esomerarazole magnesium raw material.%目的:建立同时测定埃索美拉唑镁原料药中乙醇、乙酸乙酯、异丙苯、甲醇、甲苯、2-苯基-2-丙醇、二氯甲烷、乙腈8种有机溶剂残留量的方法.方法:采用毛细管气相色谱法.色谱柱为HP-1,程序升温,进样口温度220℃,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4.0 mL/min,分流比为10∶1,进样量为1μL.结果:乙醇、乙酸乙酯、异丙苯、甲醇、甲苯、2-苯基-2-丙醇、二氯甲烷、乙腈检测质量浓度线性范围分别为45.2～904 μg/mL(r=0.999 7)、45.5～909 μg/mL(r=0.999 7)、9.0～180 μg/mL(r=0.999 8)、27.1～542 μg/mL(r=0.999 8)、8.7～174 μg/mL(r=0.999 7)、9.1～183 μg/mL(r=0.999 4)、5.8～115μg/mL(r=0.999 4)、3.7～74 μg/mL(r=0.999 4);定量限分别为4.5、3.0、1.4、2.7、0.6、3.0、3.9、2.8 ng,检测限分别为2.2、1.0、0.4、1.4、0.3、1.0、2.0、1.4 ng;精密度试验的RSD＜2.0％,重复性试验中只检出乙醇、甲醇、甲苯,其峰面积的RSD均＜2.0％;加样回收率分别为95.6％～104.9％(RSD=3.3％,n-9)、98.7％～102.0％(RSD=1.1％,n=9)、100.0％～103.1％(RSD=1.1％,n=9)、95.7％～104.4％ (RSD=3.0％,n=9)、99.3％～104.4％ (RSD=1.7％,n=9)、95.6％～102.2％(RSD=2.6％,n=9)、95.1％～103.3％(RSD=2.6％,n=9)、97.5％～103.3％(RSD=1.7％,n=9).结论:该方法灵敏度好、操作简单,适用于埃索美拉唑镁原料药中8种有机溶剂残留量的同时测定.