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Determination of linear alkylbenzenesulfonates in sediments using pressurized liquid extraction and ion-pair dervatization gas chromatography-mass spectrometry

机译:使用加压液萃取和离子对渗透气相色谱 - 质谱法测定沉积物中沉积物中的直链烷基苯磺酸盐

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摘要

A time and solvent saving method, called pressurized liquid extraction (PLE), was developed to extract linear alkylbenzene-sulfonate (LAS) residues from sediment samples. The analytes can be completely extracted by methanol at 100deg C and 100 atm with combined 15 min static and 20 min dynamic extraction steps. The LAS residues were then identified and quantitated by gas chromatography-mass spectrometry (GC-MS) with ion-pair derivatization in hte gas chromatography (GC) injection-port using a large volume (10-20 #mu#l) direct sample introduction (DSI) device. LAS recovery from spiked kaolin samples was 115% with 4% RSD. For lake sediment samples. LAS recovery was 110% with 2% RSD. The PLE method was also tested with recently spiked and aged samples showing its perfect applicability for LAS extraction.
机译:开发了一种被称为加压液萃取(PLE)的时间和溶剂保存方法以从沉积物样品中提取线性烷基苯 - 磺酸盐(LAS)残基。 分析物可以在100deg C和100atm中通过甲醇完全提取,其中15分钟静态和20分钟的动态提取步骤。 然后通过使用大容量的HTE气相色谱(GC)注射口中的气相色谱 - 质谱(GC-MS)鉴定并定量LAS残基并定量使用大容量(10-20#MU#L)直接样品引入 (DSI)设备。 从掺入的高岭土样品中的LAS恢复为115%,4%RSD。 用于湖泊沉积物样品。 LAS回收率为110%,2%RSD。 还使用最近的尖刺和老化样品测试了PLE方法,显示了其对LAS提取的完美适用性。

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