{"title":"改进QuEChERS联合GC-MS/MS同时测定牛奶中多环芳烃和农药","authors":"Jingyin Qin , Kaixuan Tong , Qiaoying Chang , Yujie Xie , Xingqiang Wu , Chunlin Fan , Hongyi Zhang , Zhihong Shi , Hui Chen","doi":"10.1016/j.jfca.2025.107336","DOIUrl":null,"url":null,"abstract":"<div><div>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 (R<sup>2</sup>>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.</div></div>","PeriodicalId":15867,"journal":{"name":"Journal of Food Composition and Analysis","volume":"141 ","pages":"Article 107336"},"PeriodicalIF":4.6000,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Simultaneous determination of PAHs and pesticides in milk based on improved QuEChERS combined with GC-MS/MS\",\"authors\":\"Jingyin Qin , Kaixuan Tong , Qiaoying Chang , Yujie Xie , Xingqiang Wu , Chunlin Fan , Hongyi Zhang , Zhihong Shi , Hui Chen\",\"doi\":\"10.1016/j.jfca.2025.107336\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><div>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 (R<sup>2</sup>>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.</div></div>\",\"PeriodicalId\":15867,\"journal\":{\"name\":\"Journal of Food Composition and Analysis\",\"volume\":\"141 \",\"pages\":\"Article 107336\"},\"PeriodicalIF\":4.6000,\"publicationDate\":\"2025-05-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of Food Composition and Analysis\",\"FirstCategoryId\":\"97\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/S0889157525001504\",\"RegionNum\":2,\"RegionCategory\":\"农林科学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"2025/2/7 0:00:00\",\"PubModel\":\"Epub\",\"JCR\":\"Q2\",\"JCRName\":\"CHEMISTRY, APPLIED\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of Food Composition and Analysis","FirstCategoryId":"97","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S0889157525001504","RegionNum":2,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"2025/2/7 0:00:00","PubModel":"Epub","JCR":"Q2","JCRName":"CHEMISTRY, APPLIED","Score":null,"Total":0}
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.
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.