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利用纳流液相色谱高分辨质谱法对蜂标本特定部位的农药残留进行定量测定。

Quantitative determination of pesticide residues in specific parts of bee specimens by nanoflow liquid chromatography high resolution mass spectrometry.

机构信息

University of Jaén, Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, Campus las Lagunillas s/n, 23071 Jaén, Spain.

University of Almería, Department of Physics and Chemistry, 04120 Almería, Spain.

出版信息

Sci Total Environ. 2020 May 1;715:137005. doi: 10.1016/j.scitotenv.2020.137005. Epub 2020 Jan 29.

Abstract

The presence of pesticide residues in bees is of great interest, given the central role of bees as indicators for environmental assessment. The goal of this article is to propose a method to capture enhanced chemical information for these central environmental indicators. Most of the methods rely on the analysis of pooled samples rather than individual specimens due to practical sample preparation method considerations and limitations in sensitivity. This leads to miss information on the mapping of pesticides and actual amount of pesticide per specimen. In this article, a nanoflow liquid chromatography system coupled to high resolution mass spectrometry (using a hybrid quadrupole-Orbitrap instrument) has been applied for the development of a multiresidue pesticide method for the determination of 162 multiclass pesticides in specific part of honeybee samples (ca. abdomen, head or thorax). The reduced flow rate provided an enhancement in sensitivity and a strong reduction of matrix effects, thus only a quick and simple ultrasound assisted extraction using minute amount of sample was required. Satisfactory results were obtained for all tested analytes with concentration levels detected lower than 0.5 ng g in all cases, thus being acceptable for monitoring purposes. Matrix effect was negligible for 94% of compounds. Extraction recoveries ranged from 70% to 105%, being within SANTE guidelines. Finally, the applicability of the method was demonstrated, by successful application to the analysis of contaminated honeybee samples, extracting useful information from specific bee parts of single specimens, thus, enabling pseudo spatially resolved chemical information.

摘要

鉴于蜜蜂作为环境评估指标的核心作用,其体内农药残留情况受到了广泛关注。本文旨在提出一种方法,以获取这些重要环境指示物的增强化学信息。由于实际的样品制备方法的考虑因素和灵敏度的限制,大多数方法都依赖于混合样本的分析,而不是单个样本的分析。这导致了在绘制农药图谱和实际每个样本的农药含量方面信息的缺失。在本文中,我们应用纳流液相色谱系统与高分辨质谱(使用混合四极杆-Orbitrap 仪器),开发了一种用于检测特定蜂蜜样本(约腹部、头部或胸部)中 162 种多类农药的多残留农药方法。降低的流速提高了灵敏度,并大大减少了基质效应,因此只需要使用少量样本进行快速简单的超声辅助提取。所有测试分析物的结果均令人满意,所有情况下所有检测物的浓度水平均低于 0.5ng/g,因此可用于监测目的。94%的化合物基质效应可忽略不计。萃取回收率在 70%至 105%之间,符合 SANTE 指南的要求。最后,通过成功应用于污染蜜蜂样本的分析,从单个样本的特定蜜蜂部位提取有用信息,从而实现了伪空间分辨化学信息,证明了该方法的适用性。

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