Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Campus Fuentenueva s/n, E-18071 Granada, Spain.
Talanta. 2013 Oct 15;115:61-7. doi: 10.1016/j.talanta.2013.04.024. Epub 2013 Apr 19.
A sensitive, simple and rapid method for the determination of fourteen mycotoxins in nuts and seeds (including almonds, peanuts, sunflower seeds, pumpkin seeds, walnuts, macadamia nuts, pistachios, hazelnuts and pine nuts) has been developed using ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS). The sample treatment comprises a first step based on QuEChERS procedure for the determination of fumonisin B1, fumonisin B2, deoxynivalenol, fusarenon-X, T-2 and HT-2 toxin, citrinin, sterigmatocystin, zearalenone and ochratoxin A. A subsequent clean-up step based on the dispersive liquid-liquid microextraction (DLLME) was necessary for the determination of aflatoxins (B1, B2, G1 and G2), since their determination was not possible applying only the QuEChERS-based extraction. The method was validated for peanuts as representative matrix and was subsequently evaluated for the other eight matrices. Quantification limits obtained for aflatoxins, the unique mycotoxins legislated on these matrices, were lower than the maximum levels allowed by the current legislation, while quantification limits obtained for the other mycotoxins were lower than the limits usually permitted by the legislation in other food matrices. Precision of the method was always lower than 11%, and recoveries ranged between 60.7% and 104.3%.
已开发出一种灵敏、简单、快速的方法,用于测定坚果和种子中的 14 种真菌毒素(包括杏仁、花生、葵花籽、南瓜籽、核桃、澳洲坚果、开心果、榛子和松子),该方法采用超高效液相色谱-串联质谱法(UHPLC-MS/MS)。样品处理包括基于 QuEChERS 程序的第一步,用于测定伏马菌素 B1、伏马菌素 B2、脱氧雪腐镰刀菌烯醇、玉米赤霉烯酮、T-2 和 HT-2 毒素、桔青霉素、桔霉素、玉米赤霉烯酮和赭曲霉毒素 A。由于仅使用基于 QuEChERS 的提取方法无法测定黄曲霉毒素(B1、B2、G1 和 G2),因此需要进行基于分散液-液微萃取(DLLME)的后续净化步骤。该方法已针对代表性基质花生进行了验证,随后对其他八种基质进行了评估。在这些基质中,唯一规定的真菌毒素黄曲霉毒素的定量限低于现行法规允许的最大水平,而其他真菌毒素的定量限低于其他食品基质法规通常允许的限量。方法的精密度始终低于 11%,回收率在 60.7%至 104.3%之间。