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超高效液相色谱-三重四极杆质谱法同时分析沉积物中6种溴代阻燃剂
Determination of 6 Brominated Flame Retardants in Sediment by Ultra-high Performance Liquid Chromatography Tandem Triple Quadruple Bar Mass Spectrometry
投稿时间:2020-02-20  修订日期:2020-04-24
DOI:10.19316/j.issn.1002-6002.2020.04.17
中文关键词:  超高效液相色谱-三重四极杆质谱  沉积物  新型溴代阻燃剂  (2,4,6-三溴苯氧基)-1,3,5-三嗪
英文关键词:ultra-high performance liquid chromatography tandem three times mass spectrometry  sediment  new brominated flame retardants  (2,4,6-tribromophenoxy)-1,3,5-triazine
基金项目:
作者单位
陈书鑫 浙江省生态环境监测中心,浙江杭州310012 
王静 浙江省生态环境监测中心,浙江杭州310012 
冯鸿儒 浙江大学化学系,浙江杭州310012 
何士冲 浙江省生态环境监测中心,浙江杭州310012 
刘铮铮 浙江省生态环境监测中心,浙江杭州310012 
穆朋倩 SCIEX公司中国亚太应用支持中心,上海200050 
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中文摘要:
      利用超高效液相色谱-三重四极杆质谱建立了沉积物中6种溴代阻燃剂的分析方法,同时进行了采样分析。以正己烷-二氯甲烷(体积比1∶9)为萃取剂,在100℃下用加速溶剂萃取仪提取沉积物样品,循环3次。萃取液浓缩至2.0 mL,转移至净化柱,用150 mL正己烷-二氯甲烷(体积比1∶2)淋洗。将淋洗液浓缩至近干,加入内标物,定容至1 mL后,用液相色谱-三重四极杆准确定量。方法干重检出限为0.01~0.1 ng/g;替代标回收率为75.6%~98.9%,相对标准偏差为12.0%~13.0%;目标物回收率为70.5%~99.2%,相对标准偏差为2.1%~17.0%。研究区域水体沉积物中的三(2,3-二溴丙基)异氰脲酸酯浓度为未检出~0.14 ng/g,(2,4,6-三溴苯氧基)-1,3,5-三嗪浓度为未检出~0.14 ng/g,十溴二苯醚浓度为0.81~4.36 ng/g,六溴苯浓度为未检出~0.08 ng/g,表明沉积物中新型溴代阻燃剂浓度处于较低水平。
英文摘要:
      A method was developed for the simultaneous analysis of 6 brominated flame retardants in sediment with ultra-high performance liquid chromatography tandem triple quadruple bar mass spectrometry.Using n-hexane/dichloromethane (1∶9) as extraction agent,the sediment samples were extracted three times by accelerated solvent extractor at 100℃.The extraction solution was concentrated to 2.0 mL,transferred to the purification column,and was washed with 150 mL n-hexane/dichloromethane (1∶2).The eluent was concentrated to near dry,and the internal standard was added.After constant volume to 1 mL,the liquid chromatogram-triple quadrupole was used for accurate quantification.The detection limit of dry weight was in range of 0.01-0.1 ng/g.Recoveries of surrogate standard and target compounds were 75.6%-98.9% and 70.5%-99.2%,with the RSD being 12.0%-13.0% and 2.1%-17.0%.The concentrations of tris-(2,3-dibromopropyl) isocyanurate,(2,4,6-tribromophenoxy)-1,3,5-triazine,decabromodiphenyl oxide and hexabromobenzene were not detected (ND)-0.14 ng/g,ND-0.14 ng/g,0.81-4.36 ng/g,ND-0.08 ng/g,which showed that new brominated flame retardants pollution was at a relative low level.
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