| This study focused on the analysis methods of emerging organic pollutants,which has been the hotpot in the environmental health research.Sediment,plastics and serum were important storage matrices for polltants in environment and human bodies.Accurate analysis methods for PBDEs,BPs and PAHs were developed and evaluated in this work.The applicability of the methods is validated by analyzing real filed samples.The one-step pretreatment technology was developed to intergrate the extraction and purification in the current analysis methods,which effectively improved the pretreatment efficiency.The processed samples could meet the requirements of mass spectrometry detection.The method for the determination of low brominated PBDEs by GC-EI-MS isotope dilution mass spectrometry was optimized.The results showed that the method with the best sensitivity could achieve quantitative analysis of PBDEs at the concentration level of 0.1-0.3ng/mL,and the linear fitting was good within the range of 2-200 ng/mL(R~2>0.999).The determination of decabromodiphenyl ether(BDE-209)was studied,which is a difficult point in PBDEs analysis.This study evaluated a variety of chromatography tandem mass spectrometry methods for BDE-209,including GC-NCI-MS,GC-EI-MS,GC-ICP-MS and HPLC-ICP-MS.The limits of quantitation of investigated methods were 3-200 ng/mL;with good linear relationship in the range of 0.5 to 10μg/mL(R~2>0.995).The relative standard deviation of measurement results(RSD,n=5)were between 0.5%and 8.7%.This research could provide a technical basis for the determination of PBDEs(including BDE-209)in sediments.Bisphenol pollutants are widely used in daily consumer products as industrial additives.In this study,the universal detection methods(HPLC-UVD/CAD/ELSD)of 6 bisphenols in food contact plastics were evaluated.The results showed that the sensitivity of ultraviolet detector was better.CAD and ELSD had advantages in detection consistency.In order to better assess environmental exposure,this study also developed the PBDEs,BPs and PAHs simultaneous analysis methods in serum samples with optimized pretreatment procedures.After optimization,the recoveries of the three target substances were 73.3%-89.0%,87.4%-121.0%and 78.8%-84.6%,respectively,with acceptable stability.The optimization of the pretreatment of serum samples has realized the enrichment and purification of three kinds of different polarity pollutants through one-time solid phase extraction and improved the efficiency of utilization of limited serum samples.The work could s provide a technical basis for further on-line SPE technology development and environmental exposure assessment. |