UPLC-MS/MS测定土壤中甲基八溴醚、十溴二苯乙烷和六溴环十二烷OA

To meet the need for the simultaneous determination of three brominated flame retardants in soil,namely tetrabromobisphenol A-bis(2,3-dibromo-2-methylpropyl ether)(TBBPA-DBMPE),decabromodiphenyl ethane(DBDPE),and hexabromocyclododecane(HBCD),this study compared the extraction efficiencies of accelerated solvent extraction and ultrasonic extraction,optimized the extraction solvent and purification conditions of the composite silica-gel column,and further opti-mized the chromatographic and mass spectrometric parameters based on the separation performance and mass spectrometric responses of the target analytes,thereby developing an ultra-performance liq-uid chromatography-tandem triple-quadrupole mass spectrometry(UPLC-MS/MS)method for the de-termination of TBBPA-DBMPE,DBDPE,and the three major diastereoisomers of HBCD in soil.In the concentration range of 2-500 ng·mL-1 for TBBPA-DBMPE and HBCD and 10-2 500 ng·mL-1 for DBDPE,the linearity exhibited correlation coefficients(r2)>0.999.When the soil sample mass was 20 g and injection volume 5 μL,the detection limits of the method were 0.004-0.02 ng·g-1,and the quantitation limits were 0.02-0.05 ng·g-1.At the spiked levels of 0.1,0.5,and 1.0 ng·g-1 for TBBPA-DBMPE and HBCD,and 1,5,and 10 ng·g-1 for DBDPE,the recoveries of TBBPA-DBMPE,DBDPE,and HBCD were 103%-114%,103%-118%,and 73.3%-118%,respectively,with relative standard deviations of 7.1%-7.9%,5.7%-9.7%,and 5.8%-16%,respectively.The proposed method was used to analyze four surface-soil samples collected around a brominated flame-retardant production enterprise in Shandong Province.The concentrations were<0.05-16 ng·g-1 for TBBPA-DBMPE,52-85 ng·g-1 for DBDPE,and 24.4-120.4 ng·g-1 for HBCD.This method is sensitive and reproducible,and suitable for the quantitative trace analysis of brominated flame retar-dants in environmental soil samples.