改进QuEChERS联合GC-MS/MS同时测定牛奶中多环芳烃和农药

IF 4.6 2区 农林科学 Q2 CHEMISTRY, APPLIED Journal of Food Composition and Analysis Pub Date : 2025-05-01 Epub Date: 2025-02-07 DOI:10.1016/j.jfca.2025.107336
Jingyin Qin , Kaixuan Tong , Qiaoying Chang , Yujie Xie , Xingqiang Wu , Chunlin Fan , Hongyi Zhang , Zhihong Shi , Hui Chen
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引用次数: 0

摘要

采用QuEChERS - GC-MS/MS联用技术,建立了牛奶中16种多环芳烃(PAHs)和133种农药的同时检测技术。采用1 %醋酸乙腈对样品进行提取和盐腌,并采用Box-Behnken设计优化最佳净化吸附剂用量。采用HP-5MS柱(30 m×0.25 mm×0.25 μm)分离,多反应监测(MRM)模式检测,外标法基质匹配标准曲线定量。结果表明,149个标靶在相应范围内线性良好(R2>0.997),检出限和定量限分别在0.003 ~ 1.67 μg/kg和0.01 ~ 1 μg/kg范围内。在1、2、10倍LOQ的加标水平下,平均加标回收率为72.40 % ~ 118.49 %,rsd内和rsd间的相对标准偏差(rsd)分别为0.12 ~ 15.09 %和0.07 ~ 16.04 %。该方法操作简便,灵敏度高,回收率好,精密度高,可帮助识别环境中潜在的污染源,为牛奶的调控提供一种快速简便的方法。
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Simultaneous determination of PAHs and pesticides in milk based on improved QuEChERS combined with GC-MS/MS
A simultaneous detection technique for 16 polycyclic aromatic hydrocarbons (PAHs) and 133 pesticides in milk was developed using QuEChERS combined with GC-MS/MS. The samples were extracted and salted with 1 % acetic acid acetonitrile, and the optimum amount of clean-up sorbent was optimized by Box-Behnken design. The targets were separated on an HP-5MS column (30 m×0.25 mm×0.25 μm), detected in multiple reaction monitoring (MRM) modes, and quantified by external standard method with a matrix-matched standard curve. The results showed that the 149 targets showed good linearity (R2>0.997) in the corresponding ranges, and the limits of detection (LOD) and limits of quantification (LOQ) were in the ranges of 0.003–1.67 μg/kg and 0.01–5 μg/kg, respectively. The average recoveries ranged from 72.40 % to 118.49 % at three spiked levels of 1, 2, and 10 times LOQ, and the relative standard deviations (RSDs) of Intra-RSD and Inter-RSD were 0.12∼15.09 % and 0.07∼16.04 %, respectively. The method is easy and quick to operate, with high sensitivity, good recovery, and precision, which can help to identify potential sources of contamination in the environment and provide a quick and easy method for the regulation of milk.
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来源期刊
Journal of Food Composition and Analysis
Journal of Food Composition and Analysis 工程技术-食品科技
CiteScore
6.20
自引率
11.60%
发文量
601
审稿时长
53 days
期刊介绍: The Journal of Food Composition and Analysis publishes manuscripts on scientific aspects of data on the chemical composition of human foods, with particular emphasis on actual data on composition of foods; analytical methods; studies on the manipulation, storage, distribution and use of food composition data; and studies on the statistics, use and distribution of such data and data systems. The Journal''s basis is nutrient composition, with increasing emphasis on bioactive non-nutrient and anti-nutrient components. Papers must provide sufficient description of the food samples, analytical methods, quality control procedures and statistical treatments of the data to permit the end users of the food composition data to evaluate the appropriateness of such data in their projects. The Journal does not publish papers on: microbiological compounds; sensory quality; aromatics/volatiles in food and wine; essential oils; organoleptic characteristics of food; physical properties; or clinical papers and pharmacology-related papers.
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