Determination of Hydroxylated Polybrominated Diphenyl Ethers in Soils by QuEChERS-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry / 分析化学

ABSTRACT

An QuEChERS-UPLC-MS/MS method was developed for the simultaneous determination of eight hydroxylated polybrominated diphenyl ethers( OH-PBDEs) in soil samples. After being mixed with 10 mL of water, the sample was extracted with acidified acetonitrile, cleaned up by C18 and primary secondary amine ( PSA ) . The separation of eight OH-PBDEs was performed on a C18 column using gradient elution of acetonitrile and water as mobile phase within 9 min. The OH-PBDEs were analyzed under the multiple-reaction monitoring ( MRM ) mode with negative electrospay ionization. Under the optimal conditions, the calibration curves were linear well in the range of 2-200 μg/L with correlation coefficients ranging from 0. 9936 to 0. 9990, and the limits of detection of eight OH-PBDEs were in the range of 0. 23-1. 21 ng/g. At the spiked levels of 5. 0 and 50 ng/g, the average spiked recoveries for eight OH-PBDEs were between 73. 2% and 117. 7%, with the relative standard derivations ( RSDs) from 5. 6% to 19. 7%. The developed method is simple and sensitive, and suitable for the rapid analysis of large quantities of samples.