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使用优化的 QuEChERS 提取和 UHPLC-MS/MS 检测方法鉴定酸奶样品中的霉菌毒素。

Identification of mycotoxins in yogurt samples using an optimized QuEChERS extraction and UHPLC-MS/MS detection.

机构信息

Departamento de Farmacología, Facultad de Veterinaria, IDIS, Universidade de Santiago de Compostela, 27002, Lugo, Spain.

Departamento de Farmacología, Facultad de Farmacia, IDIS, Universidade de Santiago de Compostela, 15705, Santiago de Compostela, Spain.

出版信息

Mycotoxin Res. 2024 Nov;40(4):569-579. doi: 10.1007/s12550-024-00547-0. Epub 2024 Jul 17.

Abstract

Yogurt, a milk-derived product, is susceptible to mycotoxin contamination. While various methods have been developed for the analysis of dairy products, only a few have been specifically validated for yogurt. In addition, these methods are primarily focus on detecting aflatoxins and zearalenone. This study aimed to conduct a preliminary investigation into the presence of regulated, emerging, and modified mycotoxins in natural and oat yogurts available in the Spanish market. For this, a QuEChERS-based extraction method was optimized and then validated to detect and quantify 32 mycotoxins using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The method was in-house validated for the analysis of natural and oat yogurt in terms of linearity, matrix effect, sensitivity, accuracy, and precision. Satisfactory performance characteristics were achieved; for most of the analytes, LOQs were lower than 2 ng/g, and recoveries ranged from 60 to 110% with a precision, expressed as the relative standard deviation of the recovery, lower than 15%. Subsequently, the validated method was applied to analyze commercial yogurt samples, revealing a notable incidence of beauvericin and enniatins, with some analogues found in up to 100% of the samples. Alternariol methyl ether was also frequently found, appearing in 50% of the samples. Additionally, the study identified regulated toxins such as fumonisins, ochratoxin A , and HT-2 toxin. These results provide new incidence data in yogurt, raising concerns about potential health risks for consumers.

摘要

酸奶是一种奶制品,容易受到真菌毒素的污染。虽然已经开发了各种用于分析乳制品的方法,但只有少数方法专门针对酸奶进行了验证。此外,这些方法主要侧重于检测黄曲霉毒素和玉米赤霉烯酮。本研究旨在初步调查西班牙市场上天然和燕麦酸奶中存在的受监管、新兴和改性真菌毒素。为此,优化了基于 QuEChERS 的提取方法,并使用超高效液相色谱-串联质谱法 (UHPLC-MS/MS) 对 32 种真菌毒素进行了检测和定量。该方法在内部针对天然和燕麦酸奶进行了分析,包括线性度、基质效应、灵敏度、准确度和精密度的验证。达到了令人满意的性能特征;对于大多数分析物,LOQs 低于 2 ng/g,回收率在 60%至 110%之间,回收率的相对标准偏差(表示为回收率的相对标准偏差)低于 15%。随后,应用验证后的方法对商业酸奶样品进行分析,结果表明, beauvericin 和 enniatins 的发生率较高,某些类似物在多达 100%的样品中发现。Alternariol methyl ether 也经常出现,出现在 50%的样品中。此外,该研究还鉴定出了受监管的毒素,如伏马菌素、赭曲霉毒素 A 和 HT-2 毒素。这些结果提供了酸奶中真菌毒素的新发病数据,引起了人们对消费者潜在健康风险的关注。

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