固相萃取-气相色谱/质谱联用-内标法测定食品中9种防腐剂  

Determination of 9 preservatives in food by solid phase extraction-gas chromatography-mass spectrometry-internal standard method

作　　者：杨明[1] 邵鹏[1] 陈啟荣[1] 杨一帆 梁颖 贾丽[1] YANG Ming;SHAO Peng;CHEN Qirong;YANG Yifan;LIANG Ying;JIA Li(Beijing Center for Physical and Chemical Analysis,Beijing 100089)

机构地区：[1]北京市理化分析测试中心,北京100089

出　　处：《分析试验室》2020年第7期834-838,共5页Chinese Journal of Analysis Laboratory

基　　金：北京市科学技术研究院青年骨干计划项目(YC-201804)资助。

摘　　要：建立了固相萃取-气质联用-内标法同时测定食品中9种防腐剂的分析方法。样品经过酸化后用乙酸乙酯提取,利用固相萃取柱净化,通过配备DB-FFAP毛细管柱的气相色谱-质谱仪分离,在选择离子监测(SIM)模式的条件下,采用内标法定量。9种防腐剂含量在0.1~10μg/mL范围内线性良好,相关系数均大于0.995;检出限为0.01~0.37 mg/kg,定量限为0.04~1.22 mg/kg。实验选取了果汁、糕点、果酱3种类型基质,分别在3个加标水平下验证方法的准确度和精密度,9种防腐剂的平均回收率为81.9%~98.3%,相对标准偏差为1.3%~6.9%。该方法适用于食品中防腐剂的检测。A method was established for the simultaneous determination of 9 preservatives in food by solid phase extraction-gas chromatography-mass spectrometry.After acidification,the sample was extracted with ethyl acetate,and cleaned up with solid phase extraction columns.The preservatives were separated by using gas chromatography-mass spectrometry equipped with a DB-FFAP capillary column,and quantitatived by internal standard method under selective ion monitoring(SIM)detection mode.The method had a good linearity in the range of 0.1~10μg/m L with correlation coefficients more than 0.995,and the limits of detection and limits of quantification were in the ranges of 0.01-0.37 mg/kg and 0.04-1.22 mg/kg,repectively.Three types of food,as well as juice,cake and jam were selected to verify the accuracy and precision of the method at three levels.The average spiked recoveries ranged from 81.9%to 98.3%with relative standard deviations of less than6.9%.The method is suitable for the determination of preservatives in food.

关 键 词：固相萃取 防腐剂 内标法 气相色谱-质谱联用 

分 类 号：O657.63[理学—分析化学]