气相色谱内标法测定氟康唑中间体间二氟苯  

Determination of m-difluorobenzene in Edaravone by GC Using an Internal Standard Analysis Method

作　　者：李艳霞[1] 叶发青[1] 胡黎川[2] 郭平[2] 陈旭[2] 叶研[2] 

机构地区：[1]温州医学院分析测试中心 [2]温州医学院药学院,浙江温州325035

出　　处：《中国现代应用药学》2007年第2期138-139,共2页Chinese Journal of Modern Applied Pharmacy

基　　金：温州市科技计划项目(G2004082)

摘　　要：目的建立氟康唑中间体间二氟苯含量测定的毛细管气相色谱法。方法样品经甲醇稀释,采用分流进样方式,用HP-5弹性石英毛细管柱经柱程序升温技术分离,FID检测器检测,内标法计算含量。结果三水平的相对回收率为98.29-102.68%,绝对回收率为98.38-99.79%,RSD为1.12-3.76%,被测样品中间二氟苯具有较高的含量。结论本方法方便可靠,可用于药物中间体间二氟苯含量的测定。OBJECTIVE To determine fluconazole intermediate m-difluorobenzene by capillary gas chromatography. METHODS Samples were diluted with methanol. Split stream sampling was applied and the split ratio was 25： 1. Samples were isolated by HP- 5 capillary column （30 m ×320 μm ×0.5 μm） ,and the temperature was gradually raised at 30℃/min. The results were detected by FID and calculated by internal standard method. RESULTS The relative and absolute recoveries were 98.29 - 102.68% and 98.38 - 99.79% with relative standard deviations of 1.12 - 3.76% at three concentration levels. CONCLUSION The method was convenience and reliability and could be used for the determination of m-difluorobenzene in medicinal intermediate.

关 键 词：气相色谱 内标法 间二氟苯 

分 类 号：R917.740.1[医药卫生—药物分析学]