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

ABSTRACT

OBJECTIVE:To establish a gas chromatography(GC)method for determination of seven residual solvents in clofarabine.METHODS:The capillary column was AT-1301;the carrier gas was nitrogen gas and the detector was FID.By temperature programming was applied for the column temperature with an initial temperature of 40 ℃,which rose to 80 ℃ with an increase rate of 7 ℃?min-1,then rose to 200 ℃(kept at this temperature for 2 min)with the increase rate of 20 ℃?min-1.The injector temperature was 250 ℃ and the detector temperature was 280 ℃.The sample was injected directly for determination of residual levels of methanol,acetonitrile,dichlormethane,t-butyl alcohol,ethyl acetate,n-heptane and acetic acid in 3 batches of clofarabine.RESULTS:All the organic solvents were effectively separated and they showed good linearity within a concentration range(r=0.999 41～0.999 93)with average recovery rate ranged from 96.5% to 102.4%(RSDs of all were less than 4.0%).7 kinds of organic solvents in 3 batches of samples were all up to the standard specified in Chinese Pharmacopeia.CONCLUSION:The method is sensitive,accurate and reliable,and it is applicable for the determination of the residual solvents in clofarabine.