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  

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

作　　者：于紫玲 左优 马瑞雪 朱晓辉 朱俊彦 陈希超 刘立婷 向明灯[1] 于云江[1] 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(State Environmental Protection Key Laboratory of Environmental Pollution Health Risk Assessment,South China Institute of Environmental Sciences,Ministry of Environmental Protection,Guangzhou 510535,China;Key Laboratory of Subsurface Hydrology and Ecological Effects in Arid Region,Ministry of Education,School of Environmental Science and Engineering,Chang an University,Xi an 710064,China;School of Public Health,Jinzhou Medical University,Jinzhou 121001,China)

机构地区：[1]环境保护部华南环境科学研究所国家环境保护环境污染健康风险评价重点实验室,广东广州510535 [2]长安大学环境科学与工程学院旱区地下水文与生态效应教育部重点实验室,陕西西安710064 [3]锦州医科大学公共卫生学院,辽宁锦州121001

出　　处：《分析测试学报》2019年第3期301-306,共6页Journal of Instrumental Analysis

基　　金：国家自然科学基金项目(21607048;21876059);广州市科技计划项目(20180410234);中央级公益性科研院所基本科研业务专项(PM-zx703-201803-068;PM-zx703-201803-071;PM-zx703-201701-030)

摘　　要：建立了同时测定水产品中四溴双酚A(TBBPA)和六溴环十二烷(HBCD)的超高效液相色谱-串联质谱方法。样品前处理采用QuEChERS方法,均质生物样品用水分散后加乙腈提取,经C_(18)分散固相萃取净化。采用CORTECS~?C_(18)色谱柱(4.6 mm×100 mm×2.7μm)分离,以甲醇-水为流动相进行梯度洗脱,流速为0.7 mL/min。采用电喷雾离子源,在负离子模式下以多反应监测(MRM)方式检测。结果表明,TBBPA和3种HBCD单体在0.5～500μg/L范围内线性良好,相关系数(r)大于0.998,检出限(LOD,S/N=3)和定量下限(LOQ,S/N=10)分别为0.04～0.16μg/kg和0.12～0.55μg/kg。在5、20、50μg/kg加标水平下的平均回收率为74.0%～121%,相对标准偏差(RSD)为0.20%～23%。该方法操作简单、快速、重现性好,适用于水产品中TBBPA和HBCD的快速检测。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.

关 键 词：四溴双酚A 六溴环十二烷 QUECHERS 超高效液相色谱-串联质谱法 水产品 

分 类 号：O657.7[理学—分析化学] S859.84[理学—化学]