1. 上海大学环境与化学工程学院
2. 中国科学院上海光学精密机械研究所
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裴镜澄, 吴明红, 向甲甲, 等. 加速溶剂萃取-同步净化/气相色谱-质谱法检测沉积物中4种新型溴代阻燃剂[J]. 分析测试学报, 2014,33(7):773-779.
Determination of Four Kinds of Novel Brominated Flame Retardants in Sediments by Gas Chromatography-Mass Spectrometry Combined with Accelerated Solvent Extraction-Synchronous Purification[J]. 2014,33(7):773-779.
裴镜澄, 吴明红, 向甲甲, 等. 加速溶剂萃取-同步净化/气相色谱-质谱法检测沉积物中4种新型溴代阻燃剂[J]. 分析测试学报, 2014,33(7):773-779. DOI:
Determination of Four Kinds of Novel Brominated Flame Retardants in Sediments by Gas Chromatography-Mass Spectrometry Combined with Accelerated Solvent Extraction-Synchronous Purification[J]. 2014,33(7):773-779. DOI:
建立了同时测定沉积物中2-乙基己基 四溴苯甲酸(TBB)、1,2-二(2,4,6-三溴苯氧基)乙烷(BTBPE)、2,3,4,5-四溴-苯二羧酸双(2-乙基己基)酯(TBPH)及十溴二苯乙烷(DBDPE) 4种新型溴代阻燃剂的加速溶剂萃取-同步净化/气相色谱-质谱分析方法。冷冻干燥后的环境沉积物样品经改进后的加速溶剂萃取(ASE)并净化后,浓缩液过Florisil固相萃取小柱,用4 mL正己烷和二氯甲烷分步洗脱,氮吹定容后用气相色谱-质谱(GC-MS)检测。结果表明,4种溴代阻燃剂的线性范围为2~1 000 μg?L-1(其中DBDPE为20~10 000 μg?L-1),相关系数均大于0.995,定量下限(S/N≥10)为0.074~44.4 μg?kg-1;在2,10 μg?L-1两个加标水平下的方法回收率为79.5%~119.7%,相对标准偏差为2.6%~15.3%。采用本方法对上海市主要水体中6个河流段采样点沉积物中的4种新型溴代阻燃剂进行检测,除1个采样点未检出TBB外,其余采样点均检出4种新型溴代阻燃剂。该方法简便、快速、灵敏度高、定性定量准确,满足沉积物中新型溴代阻燃剂的检测要求。
A simple method based on accelerated solvent extraction(ASE) /solid phase extraction(SPE) coupled with gas chromatography-mass spectrometry(GC-MS) was developed for the simultaneous determination of 2-ethylhexyl-2,3,4,5-tetrabromobenzoate(TBB),1,2-bis(2,4,6-tribromophenoxy) ethane(BTBPE),bis(2-ethylhexyl) 2,3,4,5-tetrabromophthalate(TBPH) and decabromodiphenylethane(DBDPE) in sediments.Extraction and cleanup of four novel brominated flame retardants in lyophilized sediments were performed by improved accelerated solvent extraction(ASE),and the concentrated solution was cleanup using Florisil solid phase extraction cartridges with 4 mL hexane,then eluted with 4 mL dichloromethane.The eluents was concentrated under a gentle N2 stream and analyzed by GC-MS.The calibration curves were linear in the range of 20-10 000 μg?L-1 for DBDPE,and 2-1.000 μg?L-1 for the rest of compounds,with correlation coefficients more than 0.995.The instrumental limits of quantitation(S/N≥10) for target compounds were in the range of 0.074-44.4 μg?kg-1.The average recoveries of target compounds at two spiked levels(2,10 μg?L-1) were in the range of 79.5%-119.7%,with relative standard deviations(RSDs) of 2.6%-15.3%.The proposed method was applied in the determination of four novel brominated flame retardants in sediments at six different sediments sampling sites from principal watersheds of Shanghai.All samples were detected to be contain TBB,BTBPE,TBPH and DBDPE,except one sampling site without TBB.The method was simple and sensitive,and could meet the requirements for rapid and accurate determination of four novel brominated flame retardants.
加速溶剂萃取固相萃取气相色谱-质谱法沉积物溴代阻燃剂
accelerated solvent extraction(ASE)solid phase extraction(SPE)gas chromatography-mass spectrometry(GC-MS)sedimentsbrominated flame retardants
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