REQUIMTE, Department of Bromatology, Faculty of Pharmacy, University of Porto, Porto, Portugal.
J Sep Sci. 2010 Mar;33(4-5):600-9. doi: 10.1002/jssc.200900695.
A new analytical method for the rapid and simultaneous determination of five mycotoxins (zearelenone, deoxynivalenol, Fusarenon X, 15-acetyldeoxynivalenol and nivalenol) in breakfast cereals and flours by heart-cutting GC-MS has been developed and validated. Extraction was performed with MeCN, applying a modified QuEChERS (QUick, Easy, CHeap, Effective, Rugged and Safe) procedure, and the extracts were analyzed after a silylation of the analytes under study. Careful optimization of the parameters of Deans Switch device and GC-MS was achieved in order to attain a fast separation in SIM mode, allowing a total run time of only 8 min. Acceptable recoveries for all mycotoxins at two different spiking levels (20 and 100 microg/kg) were achieved with good repeatability (from 9 to 21%). LOD ranged from 2 to 15 microg/kg and LOQ ranged from 5 to 50 microg/kg, which were lower than the maximum limit legal established by the European Union (EU). The method developed was applied to commercial breakfast cereals and flours; among the mycotoxins studied, deoxynivalenol and zearalenone were the most predominant.
建立并验证了一种用于测定谷物早餐和面粉中五种真菌毒素（玉米赤霉烯酮、脱氧雪腐镰刀菌烯醇、呋塞米酮 X、15-乙酰脱氧雪腐镰刀菌烯醇和雪腐镰刀菌烯醇）的快速、同时的新型分析方法。采用 MeCN 提取，应用改良的 QuEChERS（快速、简便、廉价、有效、坚固、安全）程序，对提取液进行衍生化后，在 SIM 模式下进行分析。仔细优化了 Dean 切换装置和 GC-MS 的参数，以实现快速分离，总运行时间仅为 8 分钟。在两个不同的添加水平（20 和 100μg/kg）下，所有真菌毒素的回收率均令人满意，重复性良好（9%至 21%）。LOD 范围为 2 至 15μg/kg，LOQ 范围为 5 至 50μg/kg，均低于欧盟规定的最大限量。所建立的方法应用于商业谷物早餐和面粉；在所研究的真菌毒素中，脱氧雪腐镰刀菌烯醇和玉米赤霉烯酮最为普遍。
