建立了HPLC-ESI-MS/MS联用技术测定奶制品中12种全氟化合物(PFCs)的方法。12种全氟化合物包括9种常见PFCs和2种调聚酸及一种全氟磺酰胺。对比了MTBE液-液萃取、甲酸、乙腈和甲醇萃取这4种萃取方法对12种全氟化合物的萃取和回收效果。最终选用甲醇作为萃取溶剂,并选取WAX作为固相萃取柱对萃取的溶液进行净化,方法对12种PFCs的加标回收在83.5%-113.3%之间,检出限0.005-0.092μg/L。最后完成了对纯牛奶,早餐奶和母乳样品中12种PFCs的分析。
A method has been established for the determination of 12 perfluorinated compounds(PFCs) including PFHxS,PFHpA,PFOA,PFOS,PFNA,PFDA,PFUnDA,PFDoDA,PFTA,POEA,FOUEA and FOSA in milk products with high performance liquid chromatography/electrospray tandem mass spectrometry(HPLC-ESI-MS/MS).The extraction efficiencies of four kinds of solvents were studied,including MTBE,formic acid,acetonitrile and methanol.Methanol was selected as the best one.Under the optimal conditions,the recoveries of PFCs in milk were in the range of 83.5 % - 113.3 % with RSDs of (n = 4) 2.1% -9.7 %. The method detection limit for the real samples ranged from 0. 005 to 0.092 μg/L. Finally, the method was applied to the analysis of PFCs in pure milk, breakfast milk and breast milk.