超高效液相色谱串联质谱法检测鱼体中的全氟化合物

采用超高效液相色谱-串联质谱联用法(UPLC-ESI-MS/MS),建立了检测1种贝类和2种鱼类的肌肉组织中11种全氟化合物(PFCs)的分析方法.采用碱液消解做为样品前处理法,选Carbon/NH2双层SPE小柱做为净化小柱,并以ACQUITY UPLC BEH C18为分析柱,甲醇和2 mmol.L-15%甲醇乙酸铵溶液为梯度淋洗液.所选定的11种全氟化合物在6 min内就可以达到良好分离,外标法定量.平均回收率在72.1%—93.6%之间,相对标准偏差在0.6%—9.5%之间,实际检出限在3.4—26.7 pg.g-1.

Ultra performance liquid chromatography-tandem mass spectrometry for determination of perfluorinated compounds in biological samples of fish

A method for the determination of 11 perfluorinated compounds(PFCs) in biological muscle samples of two kinds of fish and one kind of shellfish by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-ESI-MS/MS)was developed.The perfluorinated compounds have been analyzed by the method which recommended using alkaline digestion as a sample preparation method,Carbon/NH2 double SPE cartridges as the purification cartridge,the column of ACQUITY UPLC BEH C18 as the analyzing column,and methanol and 2 mmol·L-1 5% methanol ammonium acetate solvent as the binary gradient eluent.The 11 PFCs could be seperated in 6 min,and quantified by the external standard method.The average recoveries of 11 PFCs were determined to be were in the range of 72.1%—93.6%,with the relative standard deviations(RSD) of 0.6%—9.5%.The limits of detection(LODs) were in the range of 3.4—26.7 pg·g-1.