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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 establish a capillary gas chromatographic method for the determination of difluorobenzene in fluconazole intermediates. Methods The samples were diluted with methanol and separated by flow injection. The samples were separated by HP-5 flexible quartz capillary column by column temperature-programmed technique. FID detector was used to detect the contents of the samples. Results The relative recoveries of the three levels were 98.29 ~ 102.68%, the absolute recoveries were 98.38 ~ 99.79%, and the RSDs were 1.12 ~ 3.76%. The middifluorobenzene content of the tested samples was relatively high. Conclusion The method is convenient and reliable and can be used for the determination of difluorobenzene in drug intermediates.