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分析化学  2013 

加速溶剂萃取-气相色谱串联质谱法检测沉积物中痕量增塑剂

DOI: 10.3724/SP.J.1096.2013.30104, PP. 1315-1321

Keywords: 邻苯二甲酸酯,加速溶剂萃取,气相色谱质谱,沉积物

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Abstract:

研究了加速溶剂萃取(ASE)对沉积物中邻苯二甲酸酯类(PAEs)物质的提取效果,建立了快速溶剂萃取/气相色谱-质谱联用(GC/MS)检测沉积物中16种邻苯二甲酸酯类物质的方法。用正己烷和二氯甲烷混合溶剂作为提取溶剂,加速溶剂萃取法萃取沉积物中16种PAEs,再用Florisil层析柱净化,最后用GC/MS对净化后提取液中的PAEs进行定量分析。结果表明:当萃取剂为二氯甲烷-正己烷(1:1,V/V),萃取温度为80℃时,萃取效率最高,16种PAEs的回收率稳定在81.2%~128.5%之间,相关系数≥0.99,检出限为0.12~0.98ng/g,相对标准偏差为1.1%~10.8%。加速溶剂萃取法与传统索氏提取法相比,既提高了萃取效率同时又减少了有机萃取溶剂的用量。在检测实际样品时,同时加入3种内标指示剂对方法的性能进行了验证,3种内标的回收率分别为106.0%±18.8%,87.4%±10.8%和81.4%±14.5%,样品中16种PAEs的检出率为100%。前处理方法处理简单,定性与定量分析准确可靠。

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