| 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 |
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| 基金项目: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) |
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| 中文摘要: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C18分散固相萃取净化。采用CORTECS-C18色谱柱(4.6 mm×100 mm×2.7 μm)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05~500 μg/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0.04~0.16 μg/kg和0.12~0.55 μg/kg。在5、20、50 μg/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。 |
| 中文关键词: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 |
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| 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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| 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. |
| Key Words:tetrabromobisphenol A hexabromocyclododecane QuEChERS ultra high performance liquid chromatography-tandem mass spectrometry aquatic products |
| 引用本文：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.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[J].分析测试学报,2019,38(3):301-306. |
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