Determination of 7 polybrominated diphenyl ethers in serum by dispersive solid phase extraction combined with gas chromatography-tandem mass spectrometry
Objective This paper aims to develop a method for the analysis of 7 polybrominated diphenyl ethers(PBDEs)in serum by dispersive solid phase extraction(d-SPE)combined with gas chromatography-tandem mass spectrometric(GC-MS/MS).Methods The analytes in serum sample was extracted with 1％acetic acid-acetonitrile,and then 100 mg sodium chloride was added,shaken for 10 min,refrigerated and centrifuged at 8 000 r/min for 5 min.The extract was purified by adding 150 mg of anhydrous MgSO4 and 50 mg of Z-Sep dispersant and then vortexed for 5 min.1.00 ml of supernatant was dried in a nitrogen stream and redissolved in 50 μl of isooctane.The analytes in sample solution were determined by GC-MS/MS,separated with DB-5 column and detected by a mass spectrometer with electron impact ion source(EI)in multiple reac-tions monitoring(MRM)mode.The quantifications were based on matrix-matched calibration curves.Results The separa-tion effect of 7 PBDEs was good,and good linearity was obtained when the concentration of PBDEs was within 0.1 μg/L-50.0 μg/L,with correlation coefficients(r)above 0.999.The average recoveries at low,medium and high spiked levels were in the range of 88.3％-104.2％,with relative standard deviations(RSDs)of 4.8％-9.2％.The detection limits were between 0.006 ng/ml and 0.024 ng/ml,while the quantification limits were between 0.017 ng/ml and 0.072 ng/ml.Conclu-sion This method is simple,sensitive,accurate and fast,which is suitable for the rapid detection of PBDEs in serum.
Polybrominated diphenyl ethersSerumGas chromatography-tandem mass spectrometryDispersive solid phase extraction
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维普
