Simultaneous Determination of 8 Residual Organic Solvents in Esomeprazole Magnesium Raw Material by Capillary GC / 中国药房

ABSTRACT

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.