QuEChERS/超高效液相色谱-串联质谱法同时测定水产品中四溴双酚A与六溴环十二烷

于紫玲; 左优; 马瑞雪; 朱晓辉; 朱俊彦; 陈希超; 刘立婷; 向明灯; 于云江

Simultaneous Determination of Tetrabromobisphenol A and Hexabromocyclododecane in Aquatic Products by QuEChERS Extraction/Ultra high Performance Liquid Chromatography-Tandem Mass Spectrometry

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KeyWord:tetrabromobisphenol A hexabromocyclododecane QuEChERS ultra high performance liquid chromatography-tandem mass spectrometry aquatic products

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YU Zi-ling,ZUO You，MA Rui-xue,ZHU Xiao-hui,ZHU Jun-yan，CHEN Xi-chao,LIU Li-ting，XIANG Ming-deng，YU Yun-jiang

1.State Environmental Protection Key Laboratory of Environmental Pollution Health Risk Assessment，South China Institute of Environmental Sciences，Ministry of Environmental Protection;2.Key Laboratory of Subsurface Hydrology and Ecological Effects in Arid Region，Ministry of Education，School of Environmental Science and Engineering，Chang'an University;3.School of Public Health，Jinzhou Medical University

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Abstract:

An ultra high performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was developed for the simultaneous determination of tetrabromobisphenol A(TBBPA) and hexabromocyclododecane(HBCD) in aquatic products.Sample preparation was based on QuEChERS procedure.The target analytes in samples were extracted with acetonitrile，followed by a dispersive solid phase extraction clean up procedure using C18.Separation of TBBPA and HBCD isomers was achieved on a CORTECS- C18(4.6 mm×100 mm×2.7 μm) column with gradient elution using water-methanol as mobile phase at a flow rate of 0.7 mL/min.The MS/MS analysis was performed with electrospray ion source in negative mode under multiple reaction monitoring(MRM) mode.Good linearities for TBBPA and three HBCD isomers were achieved in the concentration range of 0.5-500 μg/L，with their correlation coefficients(r) above 0.998.The limits of detection(LOD) and the limits of quantitation(LOQ) were in the ranges of 0.04-0.16 μg/kg and 0.12-0.55 μg/kg，respectively. Recoveries at three spiked levels of 5，20 and 50 μg/kg ranged from 74.0% to 121%，with relative standard deviations(RSDs) of 0.20%-23%.The developed method was simple，rapid and reliable，and was suitable for the rapid determination of TBBPA and HBCD in aquatic products.