牛奶中全氟烷基酸的简便萃取与定量研究  

Simple Extraction and Determination of Perfluoroalkyl Acids in Milk

作　　者：李城华 汪嫣 蒋可志 LI Chenghua;WANG Yan;JIANG Kezhi(College of Material,Chemistry and Chemical Engineering,Key Laboratory of Organosilicon Chemistry and Material Technology of Ministry of Education,Hangzhou Normal University,Hangzhou 311121,China)

机构地区：[1]杭州师范大学材料与化学化工学院有机硅化学与材料技术重点实验室,浙江杭州311121

出　　处：《分析测试技术与仪器》2023年第1期54-62,共9页Analysis and Testing Technology and Instruments

基　　金：浙江省分析测试基金项目(LGC20B050011)。

摘　　要：采用阴离子交换树脂和硅胶作为混合填料对牛奶中的全氟烷基酸进行固相萃取,并结合液相色谱质谱联用技术,建立了一种简便的牛奶中21种全氟烷基酸同时定量方法.在牛奶样中加入乙腈析出大量蛋白,萃取液在自制固相萃取小柱采用1.5 mL 80%乙腈水溶液进行洗脱纯化.对纯化液进行液相色谱质谱联用分析,分析条件如下:以乙腈-5 mmol的醋酸铵水溶液为流动相,在XDB-C 18色谱柱上进行梯度洗脱,采用电喷雾负离子模式电离(ESI),质量扫描模式为多反应监测(MRM)模式检测.方法中全氟烷基酸(PFAAs)的检出限为0.01~0.20 ng/mL,定量限为0.03~0.67 ng/mL,方法的线性关系(R2>0.999)和重现性均良好,回收率范围为66%~125%.对13种常见市售牛奶中全氟烷基酸进行分析,主要检出了7种全氟烷基酸,其牛奶质量浓度在2.43~12.00 ng/mL之间.A simple method for the simultaneous quantification of 21 perfluoroalkyl acids in milk has been developed using solid-phase extraction(SPE)with anion-exchange resin and silica gel as the mixed packing material,combined with the liquid chromatography-mass spectrometry(LC-MS/MS)technique.A large amount of protein was precipitated by adding acetonitrile to the milk sample,and the extract solution was purified through the elution in a self-made solid phase extraction column using 1.5 mL of 80%acetonitrile water solution.The purified solution was analyzed using LC-MS under the following conditions:an XDB-C18 column with gradient elution using acetonitrile-5 mmol of aqueous ammonium acetate as the mobile phase,electrospray negative ionization mode ionization(ESI),the mass scan mode was multiple reaction monitoring(MRM)mode detection.The limits of detection(LOD)of perfluoroalkyl acids(PFAAs)were 0.01~0.20 ng/mL and the limits of quantification(LOQ)were 0.03~0.67 ng/mL.The linearity(R2>0.999)and reproducibility of the method were good,and the recoveries ranged from 66%to 125%.Thirteen common commercially available milk were analyzed for perfluoroalkyl acids,and seven perfluoroalkyl acids were mainly detected with milk mass concentrations ranging from 2.43 to 12.00 ng/mL.

关 键 词：全氟羧酸 全氟磺酸 牛奶 液相色谱-串联质谱 固相萃取 

分 类 号：O657.63[理学—分析化学]