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Determination of hydroxylated polychlorinated biphenyls by offline solid-phase extraction-liquid chromatography-tandem mass spectrometry using a molecularly imprinted polymer as a sorbent for sample preconcentration

机译:脱模固相萃取-液相色谱-串联质谱法以分子印迹聚合物为吸附剂进行样品预浓缩,测定羟基化多氯联苯

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摘要

Hydroxylated polychlorinated biphenyls (OH-PCBs) can be detected by liquid chromatography-mass spectrometry coupled to solid-phase extraction (SPE) using a dummy molecularly imprinted polymer (DMIP) as a sorbent. The DMIP is prepared by using an analogue of OH-PCBs (i.e., 4, 4-dihydroxybiphenyl) as a dummy template, to avoid the leakage of the target molecules. The DMIP-SPE sorbent shows good recoveries for OH-PCBs at pH 11 due to the charge-assisted hydrogen bondings between OH-PCBs and the DMIP. It has been found that the DMIP is much more effective and selective than the traditional C-18-SPE method. The sample pH, polymer dosage, elution solvent and volume have been optimized for higher recoveries. Under the optimum experimental conditions, OH-PCBs can be detected in the linear concentration range of 0.05-1.0 pM, with the detection limits ranging from 11 fM to 82 fM for 4'-OH-CB 9, 4'-OH-CB 30, 4'-OH-CB 61, 4'-OH-CB 106 and 4'-OH-CB 112. The proposed system has been successfully applied to the determination of trace OH-PCBs in spiked water samples with recoveries in the range of 89-110%. (C) 2015 Elsevier B.V. All rights reserved.
机译:羟基化多氯联苯(OH-PCBs)可以通过液相色谱-质谱联用固相萃取(SPE),使用虚拟分子印迹聚合物(DMIP)作为吸附剂进行检测。通过使用OH-PCBs的类似物(即4,4,4-二羟基联苯)作为虚拟模板来制备DMIP,以避免目标分子的泄漏。 DMIP-SPE吸附剂由于在OH-PCBs和DMIP之间的电荷辅助氢键作用而在pH 11下显示出对OH-PCBs的良好回收率。已经发现,DMIP比传统的C-18-SPE方法更加有效和选择性。样品的pH,聚合物用量,洗脱溶剂和体积均经过优化,可实现更高的回收率。在最佳实验条件下,可以在0.05-1.0 pM的线性浓度范围内检测OH-PCBs,对于4'-OH-CB 9、4'-OH-CB 30的检测限范围为11 fM至82 fM。 ,4'-OH-CB 61、4'-OH-CB 106和4'-OH-CB112。该提议的系统已成功用于测定加标水样中加标水样品中的痕量OH-PCBs。 89-110%。 (C)2015 Elsevier B.V.保留所有权利。

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