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通过液相色谱-串联质谱法(LC-MS/MS)开发检测蔬菜中多种农药残留的先进分析技术。

Development of an advanced analytical technique for detecting multiple pesticide residues in vegetables through liquid chromatography tandem mass spectroscopy (LC-MS/MS).

机构信息

ICAR-Indian Institute of Vegetable Research, Varanasi, India.

Department of Chemistry, D.S.B Campus, Kumaun University, Nainital, India.

出版信息

J Environ Sci Health B. 2024;59(10):663-677. doi: 10.1080/03601234.2024.2407713. Epub 2024 Oct 2.

Abstract

A comprehensive LC-MS/MS method, which employs Positive Electrospray Ionization (PEI) and Multiple Reaction Monitoring (MRM) was developed for the simultaneous determination of 35 pesticides belonging to various chemical classes in tomato, brinjal, chili, and okra samples. Extraction was facilitated using a modified QuEChERS method, which allows efficient sample analysis in a single run. Calibration curves for each pesticide exhibited linearity within the concentration range of 0.0025 to 0.1 µg mL, with correlation coefficients ranging from 0.993 to 0.999. Mean recoveries at five fortification levels (0.01 to 0.5 µg kg) ranged from 80 to 90%, demonstrating satisfactory precision (RSD < 20%). The matrix effects, mitigated through an optimized cleanup process, were observed within the range of 6.42% to 19.52%. The developed method having the limit of quantification of 0.01 mg kg for all 35 pesticides, proved to be highly sensitive and rapid for multi-residue estimation in diverse vegetable samples. Subsequently, the method was used to analyze the market samples from Varanasi, India, which revealed the presence of pesticides like Chlorpyrifos, Chlorantraniliproleand Indoxacarb in tomato, brinjal, chili and okra. Therefore, the method could be considered as a robust tool for monitoring pesticide residues in vegetables, aiding in quality assessment and regulatory compliance in the agriculture sector.

摘要

建立了一种采用正电喷雾离子化(PEI)和多反应监测(MRM)的 LC-MS/MS 方法,用于同时测定番茄、茄子、辣椒和秋葵样品中 35 种不同化学类别的农药。采用改良的 QuEChERS 方法进行提取,可在单次运行中实现高效的样品分析。每种农药的校准曲线在 0.0025 至 0.1μg mL 的浓度范围内呈线性,相关系数范围为 0.993 至 0.999。在五个添加水平(0.01 至 0.5μg kg)下的平均回收率为 80%至 90%,表明具有令人满意的精密度(RSD < 20%)。通过优化的净化过程减轻了基质效应,其范围在 6.42%至 19.52%之间。该方法对所有 35 种农药的定量限为 0.01mg kg,对于不同蔬菜样品中的多残留估计具有高度的灵敏度和快速性。随后,该方法用于分析来自印度瓦拉纳西的市场样品,结果表明在番茄、茄子、辣椒和秋葵中存在氯吡硫磷、氯虫苯甲酰胺和茚虫威等农药。因此,该方法可以被认为是监测蔬菜中农药残留的一种强大工具,有助于农业部门的质量评估和法规遵从性。

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