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印度三种土壤中农药的多残留分析:采用气相色谱串联质谱法的方法开发与验证

Multiresidue analysis of pesticides in three Indian soils: method development and validation using gas chromatography tandem mass spectrometry.

作者信息

Bhattacharyya Arijita, Pardeshi Anita, Nerpagar Apurva, Banerjee Kaushik

机构信息

National Reference Laboratory, ICAR-National Research Centre for Grapes, P.O. Manjri Farm, Pune, India.

出版信息

J Environ Sci Health B. 2023;58(2):158-194. doi: 10.1080/03601234.2023.2175578. Epub 2023 Feb 24.

Abstract

The paper reports a multiresidue method that was validated on 220 multi-class pesticides in three major Indian soils, namely, (i) new alluvial soil (NAS); (ii) red lateritic soil (RS) and (iii) black soil (BS) from three different regions. An ethyl acetate-based extraction method with a freezing-out cleanup step was employed for sample preparation, followed by gas chromatography-tandem mass spectrometric analysis. The method that was initially optimized on BS worked satisfactorily for the other two soil matrices. At the spiking level of 10 µg/kg (LOQ), the recoveries were satisfactory (within 70-120%) with precision-RSDs, ≤20% ( = 6) for 85, 88.6, and 89% of compounds in BS, RS, and NAS respectively. At 20 µg/kg, the method performance was satisfactory in each soil for all pesticides. When this validated method was applied to analyse 25 field samples, 6 pesticides were detected in them. In each case, precision (RSD) was <20%. The method sensitivity, accuracy and precision complied with the SANTE/2020/12830 guidelines. The method can be applied for environmental monitoring and risk assessment purposes, thus aiding in regulating pesticide usage in agricultural fields. The limitations and future scope of the study are also discussed.HighlightsA multiresidue method is reported for simultaneous analysis of multi-class pesticides in diverse soilsThe method was validated on 220 pesticides in new alluvial, red lateritic and black soilsSample preparation involved extraction with ethyl acetate and cleanup by a freezing stepThe residues were estimated by gas chromatography tandem mass spectrometry (GC-MS/MS)The method accuracy and precision complied with the EU's SANTE guidelines.

摘要

该论文报道了一种多残留方法,该方法在印度三种主要土壤中针对220种多类农药进行了验证,这三种土壤分别是:(i)新冲积土(NAS);(ii)红色红土(RS)和(iii)来自三个不同地区的黑土(BS)。采用基于乙酸乙酯的萃取方法并结合冷冻净化步骤进行样品制备,随后进行气相色谱 - 串联质谱分析。最初在黑土上优化的方法在其他两种土壤基质上也能令人满意地工作。在10 μg/kg(定量限)的加标水平下,回收率令人满意(在70 - 120% 范围内),黑土、红土和新冲积土中分别有85%、88.6%和89%的化合物的精密度 - 相对标准偏差(RSD)≤20%(n = 6)。在20 μg/kg时,该方法对所有农药在每种土壤中的性能均令人满意。当将这种经过验证的方法应用于分析25个田间样品时,检测到其中含有6种农药。在每种情况下,精密度(RSD)均<20%。该方法的灵敏度、准确度和精密度符合SANTE/2020/12830指南。该方法可用于环境监测和风险评估目的,从而有助于规范农业领域农药的使用。还讨论了该研究的局限性和未来发展方向。

重点内容

报道了一种用于同时分析不同土壤中多类农药的多残留方法

该方法在新冲积土、红色红土和黑土中的220种农药上进行了验证

样品制备包括用乙酸乙酯萃取和通过冷冻步骤净化

通过气相色谱串联质谱(GC - MS/MS)对残留量进行测定

该方法的准确度和精密度符合欧盟的SANTE指南

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