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基于氨基修饰多壁碳纳米管的磁性固相萃取和手性液相色谱串联质谱法用于水体、土壤和河底沉积物中 18 种手性农药多残留对映体分析。

Multi-residue enantiomeric analysis of 18 chiral pesticides in water, soil and river sediment using magnetic solid-phase extraction based on amino modified multiwalled carbon nanotubes and chiral liquid chromatography coupled with tandem mass spectrometry.

机构信息

School of Pharmacy, Shenyang Pharmaceutical University, 103 Wenhua Road Shenhe District, 110016, Shenyang, Liaoning Province, PR China.

School of Pharmacy, Shenyang Pharmaceutical University, 103 Wenhua Road Shenhe District, 110016, Shenyang, Liaoning Province, PR China.

出版信息

J Chromatogr A. 2018 Sep 21;1568:8-21. doi: 10.1016/j.chroma.2018.07.022. Epub 2018 Jul 6.

Abstract

This manuscript describes, for the first time, the multi-residue analysis of 18 chiral pesticides at enantiomeric levels in both environmental liquid (river water, influent and effluent wastewater) and solid matrices (agricultural soil, forestal soil and river sediment) based on magnetic solid-phase extraction (MSPE) and chiral liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Magnetic amino modified multiwalled carbon nanotubes (m-MWCNTs-NH) were prepared and firstly applied to adsorb pesticides from complex matrices. Response surface methodology (RSM) was applied to assist the multivariable optimization. The simultaneous enantioseparation of the chiral pesticides was performed on a Chiralpak IG column. Under the optimum conditions, the mean recoveries for pesticides enantiomers from the water matrices ranged from 81.1 to 106.3% with intra-day RSD of 2.1-11.9% and inter-day RSD of 2.6-12.7%; the mean recoveries for all enantiomers from the solid matrices ranged from 80.3 to 105.9% with intra-day RSD of 2.3-10.9% and inter-day RSD of 4.0-13.4%. Good linearity was achieved for all enantiomers with determination coefficients (r) greater than 0.9912. Method quantification limits were below 2.04ng L in liquid matrices and below 0.50ng g in solid matrices. The developed method offered some advantages, such as simple operation, rapidity and high concentration factor. Therefore, it is suitable for monitoring the enantiomeric compositions of chiral pesticides in different environmental matrices.

摘要

本文首次描述了基于磁性固相萃取(MSPE)和手性液相色谱-串联质谱(LC-MS/MS),对手性农药在环境液体(河水、进水和出水废水)和固体基质(农业土壤、森林土壤和河底沉积物)中的 18 种手性农药进行多残留分析。制备了磁性氨基修饰多壁碳纳米管(m-MWCNTs-NH),并首次将其应用于从复杂基质中吸附农药。响应面法(RSM)用于辅助多变量优化。在最佳条件下,手性农药对映体在 Chiralpak IG 柱上同时进行对映体分离。在最优条件下,水中基质中农药对映体的平均回收率为 81.1%106.3%,日内 RSD 为 2.1%11.9%,日间 RSD 为 2.6%12.7%;所有对映体在固体基质中的平均回收率为 80.3%105.9%,日内 RSD 为 2.3%10.9%,日间 RSD 为 4.0%13.4%。所有对映体均具有良好的线性,相关系数(r)均大于 0.9912。在液体基质中,方法定量限低于 2.04ng/L,在固体基质中,方法定量限低于 0.50ng/g。所建立的方法具有操作简单、快速、浓缩倍数高等优点。因此,它适用于监测不同环境基质中手性农药的对映体组成。

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