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Fabrication of benzenesulfonic acid groups modified magnetic microspheres as an MSPE adsorbent for fast determination of paraquat and diquat in human urine combined with UPLC-HRMS

化学 色谱法 季枯 甲酸铵 吸附 解吸 固相萃取 傅里叶变换红外光谱 质谱法 检出限 高效液相色谱法 百草枯 有机化学 化学工程 工程类
作者
Shengdong Pan,Jiabin Zhang,Qian He,Xiaohong Chen,Micong Jin
出处
期刊:Journal of Chromatography B [Elsevier BV]
卷期号:1136: 121880-121880 被引量:28
标识
DOI:10.1016/j.jchromb.2019.121880
摘要

In this study, novel benzenesulfonic acid groups modified magnetic microspheres (Fe3O4@SiO2@poly(4-VB)) were synthesized and characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier-transform infrared spectrometry (FTIR), and vibrating sample magnetometer (VSM). The as-prepared Fe3O4@SiO2@poly(4-VB) was employed as a magnetic-phase extraction (MSPE) adsorbent for rapid determination of paraquat (PQ) and diquat (DQ) in human urine samples coupled with ultra-high performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS). Moreover, this paper had expounded systematically the mass spectrum cracking mechanisms of PQ and DQ. And a zwitterionic functionalized SIELC Obelisc R column was employed for separation and retention of the above two polar herbicides using 50 mmol/L ammonium formate (pH = 3.7)-acetonitrile as the mobile phase. Besides, the adsorption and desorption conditions of Fe3O4@SiO2@poly(4-VB) toward PQ and DQ were optimized in spiking urine samples to obtain the best adsorption and desorption efficiencies. And the adsorption mechanisms of Fe3O4@SiO2@poly(4-VB) toward PQ and DQ referred to synergetic effect of electrostatic attraction and π-π interaction. Under the optimal conditions, the inter-day and intra-day spiking recoveries of the proposed method were in the range of 86.7-109.9% with RSDs less than 10%. The limits of detection (LODs) were obtained by spiking in blank urine samples at a series of low concentrations and were found to be 0.12 μg/L and 0.14 μg/L for PQ and DQ, respectively, which were lower than the comparing literatures. The developed analytical method was proven to be simple, rapid, sensitive, and accurate for clinical poisoning analysis.
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