Development of a semi-automated one-step purification method for determination of 63 pesticides in fish samples by HPLC-MS/MS using natural loofah sponge as a novel adsorbent

IF 9.8 1区农林科学 Q1 CHEMISTRY, APPLIED

Food Chemistry Pub Date : 2025-03-19 DOI:10.1016/j.foodchem.2025.143963

Yupeng Wen , Wendi Huo , Xinyuan Zhang , Yingchun Mu , Huan Liu , Chaoying Zhang , Lu Qiao , Jincheng Li

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Abstract

In this study, we developed a miniaturized semi-automatic purification method based on pressure-filtration purification for sensitive HPLC-MS/MS monitoring of pesticides in aquatic products. For the first time, loofah sponge was demonstrated and utilized as a novel green, low-cost, and effective one-step purification adsorbent for fish sample. The developed method consisted of two main steps: first, target analytes were extracted from fish samples using an acetonitrile-based QuEChERS extraction method. Subsequently, the extract was automatically purified through a pressure-filtration purification column in a centrifuge, followed by HPLC-MS/MS analysis. Under optimized experimental conditions, the method exhibited excellent linearity, with a range of 0.5 to 50.0 μg/L and a correlation coefficient > 0.99. The detection and quantification limits were 0.1-1.0 and 1.0–2.0 μg/kg, respectively. Recoveries at spiked levels of 2.0, 5.0 and 30.0 μg/kg ranged from 69.95 to 107.92%, with intra-day RSDs ranging from 0.58 to 15.01 % and inter-day RSDs ranging from 0.72 % to 14.32 %.

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建立了以天然丝瓜海绵为吸附剂的半自动化一步法测定鱼类样品中63种农药的高效液相色谱-质谱联用方法

在本研究中，我们开发了一种基于压力过滤净化的小型半自动净化方法，用于水产中农药的高效液相色谱-质谱联用（HPLC-MS/MS）灵敏监测。首次将丝瓜海绵作为一种新型的绿色、低成本、高效的鱼样一步净化吸附剂进行了论证和应用。该方法主要包括两个步骤：首先，使用基于乙腈的QuEChERS提取方法从鱼类样品中提取目标分析物。提取液经离心压滤纯化柱自动纯化，进行HPLC-MS/MS分析。在优化的实验条件下，该方法的线性范围为1.0 ~ 50.0 μg/kg，相关系数为 >； 0.99。检测限和定量限分别为0.5和1-2 μg/kg。在2.0、5.0和30.0 μg/kg加标水平下，加标回收率为69.95 ~ 104.88 %，日内rsd为0.58 ~ 15.01 %，日内rsd为0.72 % ~ 14.32 %。

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来源期刊

Food Chemistry 工程技术-食品科技

CiteScore

16.30

自引率

10.20%

发文量

3130

审稿时长

122 days

期刊介绍： Food Chemistry publishes original research papers dealing with the advancement of the chemistry and biochemistry of foods or the analytical methods/ approach used. All papers should focus on the novelty of the research carried out.