固相萃取-液相色谱-串联质谱法同时测定牛奶中双酚A、双酚F和双酚S  

Determination of Bisphenol A, Bisphenol F and Bisphenol S in Milk by High Liquid Chromatography-Tandem Mass Spectrometry with Solid-Phase Extraction

作　　者：李星 王浩[1] 张文超 张烨 巴冬梅 冉令磊 Li Xing;Wang Hao;Zhang Wenchao;Zhang Ye;Ba Dongmei;Ran Linglei(China National Food&Safety Supervision and Inspection Center,Beijing 100094)

机构地区：[1]国家食品质量安全监督检验中心,北京100094

出　　处：《中国食品学报》2022年第4期382-386,共5页Journal of Chinese Institute Of Food Science and Technology

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：为建立同时测定牛奶中双酚A、双酚F和双酚S含量的液相色谱-串联三重四极杆质谱联用方法,将样品用氨水∶乙腈溶液(1∶9,体积比)溶解,超声提取,PRiME HLB固相萃取柱净化,用安捷伦Poroshell 120 PFP色谱柱(100 mm×4.6 mm,2.7μm)分离,采用负离子多反应监测模式监测,内标法定量。在此优化条件下,牛奶中双酚A、双酚F和双酚S的定量限均为2.0μg/kg,平均方法回收率在90.4%~103.1%范围,平均相对标准偏差为2.76%~7.34%(n=6)。此方法的准确性和重复性良好,适用于牛奶中双酚A、双酚F和双酚S含量的检测。A high liquid chromatography-tandem mass spectrometry method with solid phase extraction was established for the determination of bisphenol A,bisphenol F and bisphenol S in milk. The samples were ultrasonically extracted with ammonia and acetonitrile(1 ∶ 9, V/V), purified by PRiME HLB solid phase extraction column, and separated on an Agilent Poroshell 120 PFP column(100 mm×4.6 mm, 2.7 μm). Bisphenol A, bisphenol F and bisphenol S were detected in a multiple reaction monitoring mode, and quantified by the external standard method. Under the optimized conditions,the limits of quantification of bisphenol A, bisphenol F and bisphenol S in milk were all 2.0 μg/kg. Method recovery was at the range of 90.4%-103.1% and the relative standard deviations from 2.76%-7.34%(n=6). This method had good accuracy and reproducibility, and was suitable for the detection of bisphenol A, bisphenol F and bisphenol S residues in milk.

关 键 词：液相色谱-串联三重四极杆质谱 牛奶 双酚A 双酚F 双酚S 

分 类 号：O657.63[理学—分析化学] TS252.7[理学—化学]