关键词: Matrix effect Mycotoxin UHPLC-MS/MS Validation Yogurt

来  源:   DOI:10.1007/s12550-024-00547-0

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,牛奶衍生产品,易受霉菌毒素污染。虽然已经开发了各种方法来分析乳制品,只有少数人被专门验证为酸奶。此外,这些方法主要集中于检测黄曲霉毒素和玉米赤霉烯酮。这项研究的目的是对受管制的存在进行初步调查,新兴,以及西班牙市场上天然和燕麦酸奶中的改性霉菌毒素。为此,优化了基于QuEChERS的提取方法,然后使用超高效液相色谱-串联质谱(UHPLC-MS/MS)对32种真菌毒素进行了检测和定量。该方法对天然和燕麦酸奶的线性分析进行了内部验证,基体效应,灵敏度,准确度,和精度。获得了令人满意的性能特征;对于大多数分析物,LOQs低于2ng/g,回收率从60%到110%不等,表示为回收率的相对标准偏差,低于15%。随后,将经过验证的方法应用于分析商业酸奶样品,揭示了显著的白僵素和烯尼霉素的发病率,在高达100%的样品中发现了一些类似物。交替醇甲基醚也经常被发现,出现在50%的样本中。此外,这项研究确定了受调节的毒素,如伏马菌素,曲霉毒素A,和HT-2毒素.这些结果为酸奶提供了新的发病率数据,引起人们对消费者潜在健康风险的担忧。
公众号