气相色谱法测定拉呋替丁中有机溶剂的残留量

Determination of residual organic solvents in Lafutidine by GC

目的建立拉呋替丁中有机溶剂(氯仿、乙腈)残留量的测定方法.方法采用气相色谱顶空进样法,色谱柱为CP Select 624 CB毛细管柱,以N,N'-二甲基甲酰胺为溶剂.结果两者的检测限分别为2.96、15.67 μg·ml-1,线性关系良好(r>0.9970),线性范围分别为 10～80 μg·ml-1和 50～400 μg·ml-1,平均回收率分别为100.2%和 98.9%.结论所用方法快速、简便,适合原料的质量控制.

OBJECTIVE To establish a headspace GC method for the detet＇mination of residual organic solvents （ acetonitrile and chloroform） in Lafutidine. METIRODS A CP Select 624 CB capillary column was used with N, N-dimethylfonnamide （DMF） as the solvent. RESULTS The detection limits of acetonitrile and chloroform were 2.96 and 15.67μg·ml^-1, respectively. The calibration curves of the two solvents were linear （ r 〉 0. 9970） within the ranges of 10 - 80 and 50 - 400μg·ml ^-1, respectively. The average recoveries of chloroform and acetonitrile were 100.2% and 98.9% , respectively. CONCLUSION The method is simple, rapid and suitable for the quality control of the bulk substance of Lafutidine.