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基于磁性部分碳化纤维素纳米晶的磁性固相萃取法用于水中三嗪和三唑类农药的分析。

Magnetic partially carbonized cellulose nanocrystal-based magnetic solid phase extraction for the analysis of triazine and triazole pesticides in water.

机构信息

Beijing Advanced Innovation Center for Food Nutrition and Human Health, Department of Applied Chemistry, China Agricultural University, Beijing, 100193, People's Republic of China.

出版信息

Mikrochim Acta. 2019 Nov 21;186(12):825. doi: 10.1007/s00604-019-3911-x.

Abstract

Magnetic partially carbonized cellulose nanocrystals (MPC-CNC) were obtained by sulfuric acid treatment of microcrystalline cellulose (MCC) and then loaded with magnetic FeO nanoparticles. The material is shown to be a viable material for magnetic solid phase extraction of triazine and triazole pesticides from water. The pesticides (specifically: simazine, ametryn, prometryn, terbutryn, atrazine, triadimenol, epoxiconazole, myclobutanil, triadimefon and tebuconazole) were quantified by ultra HPLC in tandem with a triple quadrupole mass spectrometry (UHPLC-MS/MS). The effects of NaCl concentration, amount of adsorbent, vortex time, sample volume and pH value on extraction efficiency were optimized by Plackett-Burman design and Box-Behnken design methods. Under the optimal conditions, the method shows the following figures of merit: (a) Linear responses in the range from 0.02-10 μg L; (b) detection limits between 2.2 to 6.1 ng L (for S/N = 3); (c) recoveries from spiked samples of 73.7-117.1% with relative standard deviations (RSDs) of 2.0-15.7%; and (d) an enrichment factor of 75. The method was successfully applied to the determination of the pesticides in five environmental water samples. Graphical abstract Schematic representation of the process of magnetic solid phase extracting pesticides in water using MPC-CNC. MCC-microcrystalline cellulose; PC-CNC- partially carbonized cellulose nanocrystals; MPC-CNC-magnetic partially carbonized cellulose nanocrystals.

摘要

磁性部分碳化纤维素纳米晶(MPC-CNC)是通过微晶纤维素(MCC)的硫酸处理得到的,然后负载磁性 FeO 纳米粒子。该材料被证明是一种可行的材料,可用于从水中磁性固相萃取三嗪和三唑类农药。通过超高效液相色谱法与三重四极杆质谱联用(UHPLC-MS/MS)定量分析了这些农药(具体为:西玛津、莠去津、扑灭津、特丁津、阿特拉津、三唑酮、环丙唑醇、戊唑醇、三唑酮和戊唑醇)。通过 Plackett-Burman 设计和 Box-Behnken 设计方法优化了 NaCl 浓度、吸附剂用量、涡旋时间、样品体积和 pH 值对萃取效率的影响。在最佳条件下,该方法具有以下优点:(a)在 0.02-10μg L 范围内呈线性响应;(b)检测限在 2.2 到 6.1ng L 之间(S/N=3);(c)加标样品的回收率为 73.7-117.1%,相对标准偏差(RSD)为 2.0-15.7%;(d)富集因子为 75。该方法成功应用于五种环境水样中农药的测定。

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