Simultaneous Determination of 4 Residual Organic Solvents in Lacidipine Raw Material by GC / 中国药房

ABSTRACT

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.