固相萃取-液相色谱-串联质谱法测定牛奶中辛基酚和正辛基酚  

Determination of 4-tert-Octyl phenol and 4-n-Octyl phenol in Milk by Solid Phase Extraction Coupled with High Liquid Chromatography-Tandem Mass Spectrometry

作　　者：王浩[1] 李星 张文超 陈江龙 巴冬梅 冉令磊 WANG Hao;LI Xing;ZHANG Wenchao;CHENG Jianglong;BA Dongmei;RAN Linglei(China National Food&Safety Supervision and Inspection Center,Beijing 100094,China)

机构地区：[1]国家食品质量安全监督检验中心,北京100094

出　　处：《中国乳品工业》2022年第1期52-55,共4页China Dairy Industry

基　　金：科技部重点科技计划项目(2017YFC1601003);北京市科技计划项目(Z181100009318011)。

摘　　要：建立了牛奶中辛基酚和正辛基酚的液相色谱-串联三重四极杆质谱测定方法。样品经氨水乙腈(1∶9,体积比)溶解,超声提取,PRiME HLB固相萃取柱净化后,经安捷伦Poroshell 120 PFP色谱柱(100 mm×4.6 mm,2.7μm)分离,采用多反应监测负离子模式监测,内标法定量。在该优化条件下,牛奶中辛基酚和正辛基酚定量限均为2.0μg/kg,在2.0,4.0,10.0μg/kg 3个加标水平下,平均方法回收率在88.1%~100.4%之间,平均相对标准偏差范围为3.48%~7.29%(n=6)。此方法的准确性和重复性良好,适用于牛奶中辛基酚和正辛基酚残留的检测。A high Liquid Chromatography-Tandem Mass Spectrometry method with Solid Phase Extraction was established for the determination of 4-tert-Octyl phenol and 4-n-Octyl phenolin milk.The sample was dissolved in ammonia and acetonitrile(1∶9,v/v),extracted with ultrasound,purified by PRiME HLB solid phase extraction column,and separated on an Agilent Poroshell 120 PFP column(100 mm×4.6 mm,2.7μm).Multi-reaction monitoring of negative ions Model monitoring,internal standard method quantification.The analytes were detected with mass spectrometer in multiple reaction monitoring mode withinternal standard.After method developing,the limit of quantification of octylphenol and n-octylphenol in milk are both 2.0μg/kg.Method recovery was at the range of 88.1%to 100.4%,also the relative standard deviations was at the range of 3.48%to 7.29%(n=6).This method was proved to be more accrate and repeatable and is suitable for the determination of 4-tert-Octyl phenol and 4-n-Octyl phenol in milk.

关 键 词：液相色谱-串联质谱法 牛奶 辛基酚 正辛基酚 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]