Department of Chemistry, Sapienza Università di Roma, Piazzale Aldo Moro 5, 00185 Roma, Italy.
J Chromatogr A. 2010 Sep 24;1217(39):6044-51. doi: 10.1016/j.chroma.2010.07.018. Epub 2010 Jul 17.
A sensitive and reliable liquid chromatography/photoionization (APPI) tandem mass spectrometry method has been developed for determining nine selected mycotoxins in wheat and maize samples. The analytes were chosen on the basis of the mycotoxins under EU Commission Regulation (EC) No. 1881/2006, i.e., deoxynivalenol (DON), zearalenone (ZON), aflatoxins (AFs), and ochratoxin A (OTA), and considering the possibility of a near future regulation for T-2 and HT-2 toxins. Mycotoxins were extracted from samples by means of an one-step solvent extraction without any cleanup. The developed multi-mycotoxin method permits simultaneous, simple, and rapid determination of several co-existing toxins separated in a single chromatographic run, in which AFs, T-2 and HT-2 toxin are acquired in positive, while OTA, DON and ZON in negative mode. Although a moderate signal suppression was noticeable, matrix effect did not give significant differences at p=0.05. Then, calibration in standard solution were used for quantitation. Based on the EU Commission Decision 2002/657/EC, the method was in-house validated in terms of ruggedness, specificity, linearity, trueness, within-laboratory reproducibility, decision limit (CCalpha) and detection capability (CCbeta). For all the analytes, the regression coefficient r ranged between 0.8752 (DON in wheat) and 0.9465 (ZON in maize), biases related to mean concentrations were from -13% to +12% of the nominal spiking level, and the overall within-laboratory reproducibility ranged 3-16%; finally, CCalpha values did not differ more than 20% and CCbeta not more than 42% from their respective maximum limit. Method quantification limits ranged from 1/20 (AFG1) to 1/4 (AFG2 and OTA) the maximum limit established by European Union in the Commission Regulation (EC) No. 1881/2006 and its subsequent amendments.
建立了一种灵敏可靠的液相色谱/光电离串联质谱法（APPI），用于测定小麦和玉米样品中的九种选定的霉菌毒素。分析物是根据欧盟委员会法规（EC）No.1881/2006 中规定的霉菌毒素选择的，即脱氧雪腐镰刀菌烯醇（DON）、玉米赤霉烯酮（ZON）、黄曲霉毒素（AFs）和赭曲霉毒素 A（OTA），并考虑到未来可能对 T-2 和 HT-2 毒素进行监管。通过一步溶剂萃取从样品中提取霉菌毒素，无需任何净化。开发的多霉菌毒素方法允许同时、简单和快速地测定单个色谱运行中分离的几种共存毒素，其中 AFs、T-2 和 HT-2 毒素以正模式获得，而 OTA、DON 和 ZON 以负模式获得。尽管信号抑制适中，但基质效应在 p=0.05 时没有产生显著差异。然后，使用标准溶液中的校准进行定量。根据欧盟委员会 2002/657/EC 号决定，该方法在稳健性、特异性、线性、准确度、实验室内部重现性、决策限（CCalpha）和检测能力（CCbeta）方面进行了内部验证。对于所有分析物，回归系数 r 范围为 0.8752（小麦中的 DON）至 0.9465（玉米中的 ZON），与平均浓度相关的偏差从标称加标水平的-13%至+12%，实验室内部重现性的总体范围为 3-16%；最后，CCalpha 值与各自的最大限量相差不超过 20%，CCbeta 值与各自的最大限量相差不超过 42%。方法的定量限范围为 1/20（AFG1）至 1/4（AFG2 和 OTA），低于欧盟委员会法规（EC）No.1881/2006 及其后续修正案规定的欧盟最大限量。
