Determination of Residual Organic Solvents in Pidotimod Tablets by GC / 中国药房

ABSTRACT

OBJECTIVE:To establish a method for separation and determination of ethanol,dichloromethane and N,N-dimethylformamide in pidotimod tablets.METHODS:The residual organic solvents were quantitatively determined by GC on DB-624 capillary column with FID detector,using nitrogen as the carries gas.Temperature programming was carried out in which the column temperature was initially maintained at 40 ℃ for 5 minutes,then increased at a rate of 50 ℃ per minute to 200 ℃,and maintained at 200 ℃ for at least 10 minutes.The temperature at injection mouth was maintained at 160 ℃;the detector temperature was maintained at 280 ℃.The split ratio was 5∶1.RESULTS:3 residual organic solvents were completely separated and their determination was free of inference from hidden foreign substances.The linear ranges of the ethanol,dichloromethane and N,N-dimethylformamide were 10.036～802.88 (r=0.999 9),26.44～105.76 (r=0.999 6),and 1.76～140.8 (r=0.999 5) ?g?mL-1,respectively,and their average recovery rates were 102.4%,99.0%,and 99.2%,respectively,with RSD at 1.99%,3.34%,and 0.55%,respectively.CONCLUSION:The method is sensitive,accurate and rapid,and it is suitable for determination of residual organic solvents in pidotimod tablets.