高效液相色谱-串联质谱法测定血清中101种新污染物OA

An analytical method was established for the determination of 101 emerging contaminants(ECs)in human serum using high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Serum samples were treated with acetonitrile to precipitate proteins.After thor-ough mixing,vortexing,and centrifugation,the supernatant was purified using phospholipid remov-al columns.Separation was achieved on an ACQUITY HSS T3 column(100 mm×2.1 mm,1.8 μm)with a mobile phase consisting of 0.02％formic acid aqueous solution and acetonitrile-methanol(1∶1,volume ratio).The ion source for the tandem mass spectrometry was an electrospray ioniza-tion source(ESI),mass spectrometric data acquisition was performed in multiple reaction monitoring(MRM)mode,and quantification was carried out using matrix-matched external standards.The re-sults demonstrated good linearity for all 101 contaminants within their respective concentration rang-es,with correlation coefficients(r2)ranging from 0.993 3 to 0.999 9.The limits of detection(LODs)and limits of quantification(LOQs)were 0.01-0.94 ng/mL and 0.03-3.20 ng/mL,respectively.At three spiked levels(5,20,and 50 ng/mL),the recoveries ranged from 75.0％to 122％,with rela-tive standard deviations(RSDs,n=6)of 1.0％-9.8％.The method was applied to analyze 17 human serum samples,detecting 43 pollutants at concentrations ranging from 0.01 to 48.1 ng/mL.This method features efficient sample preparation,high sensitivity,and good stability,making it suit-able for the rapid screening of multiple emerging pollutants in human serum.