Faculty of Pharmacy, University of Valencia, Av. Vicent Andrés Estellés, E-46100 Burjassot, Valencia, Spain.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2012;29(11):1727-35. doi: 10.1080/19440049.2012.702929. Epub 2012 Jul 30.
Sixty-one samples of Portuguese cereal-based foods were analysed for the occurrence of emerging mycotoxins called enniatins (A, A1, B and B1) and beauvericin. Samples were extracted with a mixture of acetonitrile/water (85/15, v/v) using an Ultra-Turrax homogeniser, and mycotoxins were detected with liquid chromatography coupled to a mass spectrometer. This method was validated and adequate values of recovery (70-103%) and relative standard deviation (<15%) were obtained. Signal suppression/enhancement was studied and matrix-matched calibration used to minimise this effect, but no additional clean-up step was necessary. The mass spectrometer was operated in selected reaction monitoring (SRM) mode and with selected transitions for each compound to quantify and to qualify them. Fifty-nine per cent of samples were contaminated. The percentages of enniatins were 53%, 49%, 44% and 16% for A1, B, B1, and A, respectively, and for beauvericin it was 1.6%. For the total samples, the mean contamination was 30, 24, 15, 2.1 and 0.1 ng g⁻¹ for enniatins A1, B, B1 and A, and beauvericin, respectively. The wheat-based samples showed higher levels and greater prevalence than any other cereals monitored. These results were used to estimate the daily intake of ENs from wheat-based cereal by the Portuguese population. At the same time, the usefulness of this method in the analysis of other important mycotoxins (aflatoxin B₁, ochratoxin A, deoxynivalenol, T-2 toxin, fumonisin B₁ and zearalenone) was evaluated.
对 61 份葡萄牙谷物食品进行了分析,以检测新型真菌毒素——恩镰孢菌素(A、A1、B 和 B1)和 beauvericin 的存在情况。采用 Ultra-Turrax 匀浆器,用乙腈/水(85/15,v/v)混合物提取样品,用液相色谱-质谱联用仪检测真菌毒素。该方法经过验证,回收率(70-103%)和相对标准偏差(<15%)均达到了良好的水平。对信号抑制/增强进行了研究,并采用基质匹配校准来最小化这种影响,但无需额外的净化步骤。质谱仪采用选择反应监测(SRM)模式,针对每种化合物选择特定的转换进行定量和定性分析。59%的样品受到了污染。A1、B、B1 和 A 的恩镰孢菌素含量分别为 53%、49%、44%和 16%,而 beauvericin 的含量为 1.6%。对于所有样品,A1、B、B1、A 和 beauvericin 的平均污染水平分别为 30、24、15、2.1 和 0.1ng/g。小麦基样品的污染水平和检出率均高于其他监测的谷物。这些结果用于估算葡萄牙人口从小麦基谷物中摄入 ENs 的情况。同时,评估了该方法在分析其他重要真菌毒素(黄曲霉毒素 B₁、赭曲霉毒素 A、脱氧雪腐镰刀菌烯醇、T-2 毒素、伏马菌素 B₁ 和玉米赤霉烯酮)中的应用价值。