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采用“缩减规模”QuEChERS 方法和流量调制全二维气相色谱-三重四极杆质谱法测定蔬菜产品中的多种农药残留。

Determination of multi-pesticide residues in vegetable products using a "reduced-scale" Quechers method and flow-modulated comprehensive two-dimensional gas chromatography-triple quadrupole mass spectrometry.

机构信息

Department of Chemical, Biological, Pharmaceutical and Environmental Sciences, University of Messina, Messina, Italy.

Department of Mathematical and Computer Science, Physical Sciences and Earth Sciences, University of Messina, Messina, Italy.

出版信息

J Chromatogr A. 2021 May 24;1645:462126. doi: 10.1016/j.chroma.2021.462126. Epub 2021 Apr 1.

Abstract

The aim of the present research was the development of an analytical method for the determination of multi-pesticide residues (88 target analytes) in four vegetable products (tomatoes, cucumbers, sweet red peppers and iceberg lettuce) using a "reduced-scale" QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction method and flow-modulated comprehensive two-dimensional gas chromatography-triple quadrupole mass spectrometry. In particular, the suitability of flow modulation [with relatively high second-dimension gas flow conditions (8 mL min)] for trace analyte determination was evaluated. The samples were prepared according to the QuEChERS procedure as reported by the official European Union method, namely EN 15662:2018, based on the use of 3 g of vegetable product. Matrix-matched calibration processes were carried out for all the samples. The figures-of-merit determined were recovery, linearity, precision, limits of detection (LoDs), and limits of quantification (LoQs). Specifically, recoveries were in the 53-160% range, regression coefficients were between 0.9156 and 0.9999, the LoDs were in the 0.1-6.3 μg kg range, the LoQs were in the 3.0-21.0 μg kg range, and coefficients of variation were between 1 and 28% (at the 50 μg kg level).

摘要

本研究的目的是开发一种分析方法,用于检测四种蔬菜产品(西红柿、黄瓜、甜椒和冰山生菜)中的多农药残留(88 种目标分析物),使用“缩减规模”的 QuEChERS(快速、简便、廉价、有效、坚固、安全)提取方法和流调制综合二维气相色谱-三重四极杆质谱法。特别是,评估了流调制[采用相对较高的二维气流条件(8 mL min)]对痕量分析物测定的适用性。根据欧盟官方方法 EN 15662:2018 所述的 QuEChERS 程序,使用 3 克蔬菜产品制备样品。对所有样品进行基质匹配校准过程。确定的评价指标包括回收率、线性、精密度、检出限(LOD)和定量限(LOQ)。具体而言,回收率在 53-160%范围内,回归系数在 0.9156 到 0.9999 之间,LOD 在 0.1-6.3 μg kg 范围内,LOQ 在 3.0-21.0 μg kg 范围内,变异系数在 1%到 28%之间(在 50 μg kg 水平)。

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