Lee Youngsun, Kim Jung Hee, You Da-Jung, Kim Cho-Il, Lee Jee-Yeon, Park Hyun-Mee
Korea Institute of Science and Technology, Advanced Analysis Center, 5 Hwarang-ro 14-gil, Seongbuk-gu, Seoul 02792, Republic of Korea.
Korea Health Industry Development Institute, Nutrition Policy & Promotion Team, 187 Osongsaengmyeong 2-ro, Osong-eup, Heungdeok-gu, Cheongju-si, Chungcheongbuk-do 28159, Republic of Korea.
J AOAC Int. 2019 Nov 1;102(6):1657-1665. doi: 10.5740/jaoacint.19-0031. Epub 2019 Apr 19.
Determining the multi-mycotoxins present in table-ready foods is necessary for a total diet study. However, so far, most methods of analyzing multi-mycotoxins apply to raw foods. Therefore, a reliable method for analyzing multi-mycotoxins in table-ready foods is needed. We developed and validated methods of multi-mycotoxin analysis that employed stable isotope dilution with LC-tandem MS (LC-MS/MS) using two representative matrices. Samples were fortified with [C]-labeled mycotoxins as internal standards and extracted with 50% acetonitrile in water for high-carbohydrate foods and 3% formic acid in acetonitrile for high-protein and/or high-fat foods, cleaned up with -hexane and the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method, and followed up by LC-MS/MS. Validation of the methods was performed, and the results were as follows: the correlation coefficient, ², was 0.99; method detection limit, 0.01-2.4 μg/kg; recoveries, 83.6-114%; precision, 0.8-10 (intraday) and 3.1-22% (interday); interlaboratory reproducibility, ≤15%; and uncertainty, 3.5-19%. The applicability of the methods was evaluated by analyzing table-ready foods spiked with standards. These methods were successfully evaluated and deemed appropriate for determining the multi-mycotoxins in table-ready foods. This work demonstrates that stable isotope dilution with LC-MS/MS can be effectively used to analyze multi-mycotoxins simultaneously in a total diet study.
对于总膳食研究而言,确定即食食品中存在的多种霉菌毒素很有必要。然而,到目前为止,大多数分析多种霉菌毒素的方法适用于生食。因此,需要一种可靠的方法来分析即食食品中的多种霉菌毒素。我们开发并验证了多种霉菌毒素分析方法,该方法采用稳定同位素稀释结合液相色谱-串联质谱法(LC-MS/MS),使用了两种代表性基质。样品用[C]标记的霉菌毒素作为内标进行加标,对于高碳水化合物食品,用50%乙腈水溶液提取,对于高蛋白和/或高脂肪食品,用3%甲酸乙腈溶液提取,用正己烷和快速、简便、廉价、有效、耐用且安全(QuEChERS)方法进行净化,然后进行LC-MS/MS分析。对这些方法进行了验证,结果如下:相关系数r²为0.99;方法检出限为0.01 - 2.4μg/kg;回收率为83.6 - 114%;精密度为0.8 - 10%(日内)和3.1 - 22%(日间);实验室间再现性≤15%;不确定度为3.5 - 19%。通过分析加标即食食品对这些方法的适用性进行了评估。这些方法成功通过评估,被认为适用于测定即食食品中的多种霉菌毒素。这项工作表明,在总膳食研究中,稳定同位素稀释结合LC-MS/MS可有效地用于同时分析多种霉菌毒素。