Solfrizzo Michele, Gambacorta Lucia, Bibi Rita, Ciriaci Martina, Paoloni Angela, Pecorelli Ivan
National Research Council of Italy, Institute of Sciences of Food Production, Via Amendola 122/O, Bari 70126, Italy.
Istituto Zooprofilattico Sperimentale dell'Umbria e delle Marche, Via Salvemini, Perugia 06126, Italy.
J AOAC Int. 2018 May 1;101(3):647-657. doi: 10.5740/jaoacint.17-0339.
Twelve different approaches commonly used for the simultaneous LC tandem MS (MS/MS) determination of mycotoxins (deoxynivalenol, aflatoxins, ochratoxin A, T-2 and HT-2 toxins, fumonisins, and zearalenone) were tested in cereals and feed materials. They comprised different extraction solvents, types of cleanup [solid-phase extraction, QuEChERS, and immunoaffinity (IMA)], and calibration approaches (external or matrix-matched). The percentage of mycotoxins with acceptable recovery, according to Regulation (EC) No. 401/2006, ranged from 9 to 100%. The approach giving the highest percentage of acceptable results was selected and further tested for corn, rice, and feed spiked at three different mycotoxin levels (low, medium, and high). The method is based on extraction with MeOH-water (70 + 30, v/v) and cleanup with two multiantibody IMA columns. For corn and rice spiked at low mycotoxin levels, a significant matrix effect was observed and was compensated by using 13C calibration. At higher mycotoxin levels (medium and high), matrix effects were negligible as no significant differences were observed for the majority of recovery results calculated by 13C calibration and external calibration. Although the proposed method still needs improvement in terms of accuracy and, to a lesser extent, precision, it was successfully tested with four proficiency tests in buckwheat, corn, rice, and feed, giving acceptable z-scores for 97% (34 out of 35) of results.
在谷物和饲料原料中测试了12种常用于同时液相色谱串联质谱（MS/MS）测定霉菌毒素（脱氧雪腐镰刀菌烯醇、黄曲霉毒素、赭曲霉毒素A、T-2和HT-2毒素、伏马菌素和玉米赤霉烯酮）的不同方法。它们包括不同的提取溶剂、净化类型[固相萃取、QuEChERS和免疫亲和（IMA）]以及校准方法（外部校准或基质匹配校准）。根据欧盟法规（EC）No. 401/2006，霉菌毒素回收率合格的百分比范围为9%至100%。选择了给出最高合格结果百分比的方法，并在添加了三种不同霉菌毒素水平（低、中、高）的玉米、大米和饲料中进一步测试。该方法基于用甲醇-水（70 + 30，v/v）提取，并用两根多抗体IMA柱净化。对于添加低水平霉菌毒素的玉米和大米，观察到显著的基质效应，并通过使用13C校准进行补偿。在较高霉菌毒素水平（中、高）下，基质效应可忽略不计，因为通过13C校准和外部校准计算的大多数回收率结果没有观察到显著差异。尽管所提出的方法在准确性方面仍需改进，在较小程度上在精密度方面也需改进，但它已在荞麦、玉米、大米和饲料的四项能力验证测试中成功测试，97%（35个结果中的34个）的结果给出了可接受的z分数。
