Optimized liquid chromatography–tandem mass spectrometry protocol for enhanced detection of 45 pesticides in water and soil samples

IF 1.8 3区化学 Q4 BIOCHEMICAL RESEARCH METHODS Rapid Communications in Mass Spectrometry Pub Date : 2024-09-02 DOI:10.1002/rcm.9904

Lingchen Meng, Wenrui Yao, Ling Wen, Xiaoli Fu, Yulin Qi, Dietrich A. Volmer

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Abstract

Rationale

The development of analytical screening techniques for pesticides is crucial for preventing and mitigating environmental contamination. Mass spectrometry-based screening methods differ based on the complexity of the sample matrix and the diversity of the target compounds. One of the major challenges is balancing cost reduction in the extraction process with the optimization of analytical results. This protocol introduces a universal and efficient scheme for the qualitative and quantitative schemes for 45 pesticides within a single analytical run.

Methods

Water samples were extracted using an SPE column, with the pH adjusted to 7. Soil samples were processed using a modified QuEChERS method. The pretreatment for water samples emphasized selecting appropriate SPE columns and optimizing pH, while for soil samples, the focus was on choosing suitable extraction solvents and extraction salt packages. The enriched samples were then analyzed using liquid chromatography–tandem mass spectrometry (LC–MS/MS). The method was evaluated for accuracy, precision, detection limits, and matrix effects.

Results

The method enabled the simultaneous detection of 45 pesticides within a 15-minute analysis period. SPE recoveries ranged from 56.1% to 118.8%. Instrumental detection limits varied between 0.02 and 1 pg, while method detection limits extended from 0.05 to 18.47 ng/l in soil and water matrices. The approach was successfully applied to water and soil samples, with the pesticide concentration ranging from 0.1 ng/L to 38 μg/L.

Conclusions

The protocol substantially enhances the characterization and quantification of 45 pesticides in environmental samples, achieving a remarkable reduction in detection limits by an order of magnitude compared to previous research. This method enables the simultaneous detection of pesticides in both water and soil matrices using a single system, addressing the challenges of using separate systems for different environmental media. Furthermore, this protocol provides a crucial theoretical foundation for managing and safeguarding against pesticide pollution.

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优化液相色谱-串联质谱方案，增强对水和土壤样品中 45 种农药的检测。

理由：开发农药分析筛选技术对于预防和减轻环境污染至关重要。基于质谱的筛选方法因样品基质的复杂性和目标化合物的多样性而各不相同。主要挑战之一是如何在降低提取过程成本与优化分析结果之间取得平衡。本方案介绍了一种通用、高效的方案，可在一次分析运行中对 45 种农药进行定性和定量分析：水样采用 SPE 柱提取，pH 值调至 7。水样的预处理重点是选择合适的固相萃取柱和优化 pH 值，而土壤样品的预处理重点是选择合适的萃取溶剂和萃取盐包。然后使用液相色谱-串联质谱法（LC-MS/MS）对富集的样品进行分析。对该方法的准确度、精密度、检测限和基质效应进行了评估：结果：该方法可在 15 分钟的分析时间内同时检测 45 种农药。SPE 回收率为 56.1% 至 118.8%。在土壤和水基质中，仪器检测限在 0.02 至 1 pg 之间，方法检测限在 0.05 至 18.47 ng/l 之间。该方法成功应用于水和土壤样品，农药浓度范围为 0.1 ng/L 至 38 μg/L：该方法大大提高了环境样本中 45 种农药的定性和定量能力，与之前的研究相比，检测限显著降低了一个数量级。该方法可使用单一系统同时检测水和土壤基质中的农药，解决了针对不同环境介质使用不同系统的难题。此外，该方案还为管理和防范农药污染提供了重要的理论基础。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

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来源期刊

Rapid Communications in Mass Spectrometry 化学-分析化学

CiteScore

4.10

自引率

5.00%

发文量

219

审稿时长

2.6 months

期刊介绍： Rapid Communications in Mass Spectrometry is a journal whose aim is the rapid publication of original research results and ideas on all aspects of the science of gas-phase ions; it covers all the associated scientific disciplines. There is no formal limit on paper length ("rapid" is not synonymous with "brief"), but papers should be of a length that is commensurate with the importance and complexity of the results being reported. Contributions may be theoretical or practical in nature; they may deal with methods, techniques and applications, or with the interpretation of results; they may cover any area in science that depends directly on measurements made upon gaseous ions or that is associated with such measurements.