关键词: 多溴联苯和多溴联苯醚, QuEChERS, 气相色谱-串联质谱, 蔬菜

Abstract: A quick, easy, cheap, effective, rugged, and safe (QuEChERS) sample pretreatment coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS) method was proposed to determine 20 polybrominated biphenyls (PBBs) and polybrominated diphenyl ethers (PBDEs) in vegetables. Samples were extracted with acidified acetonitrile, salted?out with anhydrous magnesium sulfate and sodium?chloride and cleaned with C18 modified silica gel and primary secondary amine (PSA), and the analytes were detected by GC-MS/MS under the selective reaction monitoring (SRM) mode and quantified by an external standard method. The calibration curves of monobromobiphenyl, dibromobiphenyl, tribromobiphenyl, terabromobiphenyl, pentabromobiphenyl and exabromobiphenyl as well as the corresponding PBDEs showed good linearity in the range of 0.05–5.0 mg/L, heptabromobiphenyl and octabromobiphenyl as well as the corresponding PBDEs showed good linearity in the range of 0.1–5.0 mg/L, nonabromobiphenyl and decabromobiphenyl as well as and the corresponding PBDEs showed good linearity in the range of 0.2–5.0 mg/L, with correlation coefficients of greater than 0.99. The limits of detection (LODs) were 0.30–17.67 ng/kg. With the proposed method, the recoveries in 3 different vegetables at spiked levels of 0.25, 0.5 and 2.5 mg/kg were 70.5%–118.9% with relative standard deviations (RSDs) of 1.3%–11.2%. The proposed method is simple and sensitive with good reproducibility and recovery, and thus can be suitable for the determination of PBBs and PBDEs in vegetables.

Key words: PBBs and PBDEs, QuEChERS, gas chromatography-tandem mass spectrometry, vegetables