Determination of 14 kinds of perfluorinated and polyfluoroalkyl compounds in meconium by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry
Perfluorinated and polyfluoroalkyl compounds(PFASs)are a kind of synthetic substances,which have been widely used in daily life and production because of their excellent properties such as heat stability,hydrophobic and oleophobic.PFASs have the characteristics of environmental persistence,bioaccumulation,and multiple toxicity,and can pass across the placental barrier into the fetal,thus posing potential exposure risk to fetal health.Generally,the meconium accumulates exogenous compounds that were exposed to the fetus during pregnancy,as such,the meconium can be used to monitor the exposure characteristics of PFASs to the fetus.A method was established for the determination of 14 kinds of PFASs in meconium by solid phase extraction high performance liquid chromatography-tandem mass spectrometry(SPE HPLC-MS/MS).The freeze-drying meconium sample(0.2 g)was ultrasonically extracted by acetonitrile(ACN)/water(9:1,V/V)and then was extracted by Envi-carb and Oasis WAX cartridges,eluted with 0.1%ammonia in methanol.The sample was separated by using an Acquity UPLC BEH C18 column and eluted gradiently with 10 mmol·L-1 ammonium acetate and acetonitrile as the mobile phase.The samples were detected by tandem mass spectrometry under multiple reaction monitoring(MRM)mode with negative electrospray ionization,and quantified by internal standard method.Results showed that the recoveries of PFASs were 65%-149%at spiked levels of 2,5,and 20 ng·g-1,and the relative standard deviations(RSD)were 3%-22%.The method detection limits(MDLs)and the method quantitation limits(MQLs)were in the range of 0.001-0.149 ng·g-1 and 0.003-0.495 ng·g1,respectively.The method was used to detect 10 meconium samples,and the concentrations ranged from<MDLs to 2.49 ng·g-1.This established method is simple,convenient,sensitive and accurate,which will provide a technical basis for the systematic study of the occurrence as well as exposure risk of PFASs in meconium.
meconiumperfluorinated and polyfluoroalkyl compounds(PFASs)high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)solid phase extraction(SPE)