Guo Wenbo, Yang Junhua, Niu Xueke, Tangni Emmanuel K, Zhao Zhihui, Han Zheng
Institute for Agro-food Standards and Testing Technology, Shanghai Key Laboratory of Protected Horticultural Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201403, China.
Organic Contaminants and Additives, Sciensano, Leuvensesteenweg 17, Tervuren 3080, Belgium.
Anal Methods. 2021 Jan 21;13(2):192-201. doi: 10.1039/d0ay01787f.
An ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed for simultaneous determination of 15 mycotoxins, including aflatoxins (B1, B2, G1, and G2), ochratoxins (A, B, and C), citrinin, patulin, and emerging Alternaria toxins (alternariol, alternariol monomethyl ether, altenuene, tentoxin, tenuazonic acid, and altenusin) in orange, grape and apple juices. Different extraction approaches, sorbents, chromatographic columns and mobile phases were investigated for establishment of an optimal QuEChERS procedure and UHPLC-MS/MS conditions. Recoveries were in the range of 74-110%, and the limits of detection (LODs) and limits of quantification (LOQs) ranged from 0.05 to 0.1 ng mL-1 and from 0.1 to 5.0 ng mL-1, respectively. Matrix effects were evaluated and matrix-matched calibration curves were used to compensate for matrix effects and achieve accurate quantification. The correlation coefficients (R2) of linearity were higher than 0.99 and the relative standard deviations (RSDs) of intra- and inter-day precision were under 13%. The method was subsequently applied to 22 fruit juice samples. The high frequencies (90.9%) of mycotoxins not only proved the reliability and sensitivity of the currently established method, but also demonstrated that fruit juices are susceptible to different mycotoxins, which need to be continuously monitored in the future.
建立了一种超高效液相色谱-串联质谱（UHPLC-MS/MS）方法，用于同时测定橙汁、葡萄汁和苹果汁中的15种霉菌毒素，包括黄曲霉毒素（B1、B2、G1和G2）、赭曲霉毒素（A、B和C）、桔霉素、棒曲霉素以及新兴的链格孢菌毒素（交链孢酚、交链孢酚单甲醚、细交链孢菌酮酸、展青霉素、细交链孢菌酮酸和交链孢菌素）。研究了不同的提取方法、吸附剂、色谱柱和流动相，以建立最佳的QuEChERS程序和UHPLC-MS/MS条件。回收率在74%-110%之间，检测限（LOD）和定量限（LOQ）分别为0.05至0.1 ng mL-1和0.1至5.0 ng mL-1。评估了基质效应，并使用基质匹配校准曲线来补偿基质效应并实现准确定量。线性相关系数（R2）高于0.99，日内和日间精密度的相对标准偏差（RSD）均低于13%。该方法随后应用于22个果汁样品。霉菌毒素的高检出率（90.9%）不仅证明了当前所建立方法的可靠性和灵敏度，还表明果汁易受不同霉菌毒素污染，未来需要持续监测。
