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高效液相色谱-高分辨质谱联用结合QuEChERS法快速筛查水产品中192种兽药残留的方法开发与验证

Development and validation of rapid screening of 192 veterinary drug residues in aquatic products using HPLC-HRMS coupled with QuEChERS.

作者信息

Yang Guangxin, Zhang Junyu, Tang Yunyu, Kong Cong, Li Siman, Wang Shouying, Ding Shuhai, Gu Lin, Shen Xiaosheng, Martin Aka Alla, Chi Hai

机构信息

Key Laboratory of East China Sea Fishery Resources Exploitation, Ministry of Agriculture and Rural Affairs, East China Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Shanghai 200090, PR China.

School of Environment and Architecture, University of Shanghai for Science and Technology, Shanghai 200090, PR China.

出版信息

Food Chem X. 2024 May 24;22:101504. doi: 10.1016/j.fochx.2024.101504. eCollection 2024 Jun 30.

DOI:10.1016/j.fochx.2024.101504
PMID:38855097
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC11157224/
Abstract

The presence of veterinary drug residues in aquatic products represents a significant challenge to food safety. The current detection methods, limited in both scope and sensitivity, underscore the urgent need for more advanced techniques. This research introduces a swift and potent screening technique using high-performance liquid chromatography-high-resolution mass spectrometry (HPLC-HRMS) and a refined QuEChERS protocol, allowing simultaneous qualitative and semi-quantitative analysis of 192 residues. A comprehensive database, employing full scan mode and data-dependent secondary mass spectroscopy, enhances screening accuracy. The method involves efficient extraction using 90% acetonitrile, dehydration with NaSO, and acetic acid, followed by cleanup using dispersive solid-phase extract sorbent primary secondary amine. It is suitable for samples with varying fat content, offering detection limits ranging from 0.5 to 10 μg/kg, high recovery rates (60-120%), and low relative standard deviations (<20%). Practical application has validated its effectiveness for multi-residue screening, marking a significant advancement in food safety evaluation.

摘要

水产品中兽药残留的存在对食品安全构成了重大挑战。当前的检测方法在范围和灵敏度上都存在局限,凸显了对更先进技术的迫切需求。本研究引入了一种快速且高效的筛查技术,该技术采用高效液相色谱 - 高分辨率质谱联用仪(HPLC - HRMS)和优化的QuEChERS方案,可同时对192种残留进行定性和半定量分析。一个采用全扫描模式和数据依赖型二级质谱的综合数据库提高了筛查的准确性。该方法包括使用90%乙腈进行高效萃取,用无水硫酸钠和乙酸脱水,随后使用分散固相萃取吸附剂伯仲胺进行净化。它适用于不同脂肪含量的样品,检测限为0.5至10μg/kg,回收率高(60 - 120%),相对标准偏差低(<20%)。实际应用验证了其在多残留筛查方面的有效性,标志着食品安全评估取得了重大进展。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/e98f/11157224/6783ed00b725/gr4.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/e98f/11157224/1e91e41c6506/gr1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/e98f/11157224/cb48d8542d3b/gr2.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/e98f/11157224/468aa0bc6af7/gr3.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/e98f/11157224/6783ed00b725/gr4.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/e98f/11157224/1e91e41c6506/gr1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/e98f/11157224/cb48d8542d3b/gr2.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/e98f/11157224/468aa0bc6af7/gr3.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/e98f/11157224/6783ed00b725/gr4.jpg

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