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