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埃及市场橄榄油中非法染料检测与定量快速液相色谱-串联质谱法的优化与验证

Optimization and validation of a rapid LC-MS/MS method for the detection and quantification of illegal dyes in olive oil from Egyptian markets.

作者信息

Ragab Menna, Khaled Omar, Eissa Fawzy, Medhat Mohamed

机构信息

Central Public Health Laboratory, Ministry of Health, 12651 Embaba, Giza, Egypt.

Agriculture Research Centre, Central Laboratory of Residue Analysis of Pesticides and Heavy Metals in Foods, Ministry of Agriculture, Giza 12311, Egypt.

出版信息

Food Chem. 2025 Oct 1;488:144924. doi: 10.1016/j.foodchem.2025.144924. Epub 2025 May 27.

Abstract

The use of banned dyes in olive oil poses a serious threat to consumer safety. This study presents a high-throughput LC-MS/MS method for the simultaneous detection and quantification of ten banned dyes. The simplified sample preparation involves dissolving the sample in n-hexane and extracting it with ACN. Method validation, performed according to CIR (EU) 2021/808, demonstrated satisfactory performance. LOD and LOQ ranged from 0.1 to 0.3 μg kg and 0.3 to 0.9 μg kg, respectively. Precision (RSDs) was below 9 % at five spiking levels (2-75 μg kg). CCα and CCβ values ranged from 14 to 15 μg kg and 12 to 13 μg kg, respectively. The method's applicability was demonstrated by analyzing 870 olive oil samples collected from local markets in Egypt, revealing the presence of Sudan Yellow (5 %), Sudan I (0.9 %), Sudan III (0.2 %), Sudan Red G (0.1 %), Sudan II (0.1 %), and Sudan Red B (0.1 %) in the tested samples.

摘要

在橄榄油中使用违禁染料对消费者安全构成严重威胁。本研究提出了一种用于同时检测和定量十种违禁染料的高通量液相色谱-串联质谱法。简化的样品制备过程包括将样品溶解在正己烷中,并用乙腈萃取。根据欧盟委员会法规(EU)2021/808进行的方法验证显示性能良好。检测限和定量限分别为0.1至0.3μg/kg和0.3至0.9μg/kg。在五个加标水平(2至75μg/kg)下,精密度(相对标准偏差)低于9%。CCα和CCβ值分别为14至15μg/kg和12至13μg/kg。通过分析从埃及当地市场收集的870个橄榄油样品,证明了该方法的适用性,结果显示在测试样品中存在苏丹黄(5%)、苏丹红I(0.9%)、苏丹红III(0.2%)、苏丹红G(0.1%)、苏丹红II(0.1%)和苏丹红B(0.1%)。

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