Departament de Medicina Preventiva i Salut Pública, Facultat de Farmàcia, Universitat de València, Av. Vicent Andrés Estellés, 46100 Burjassot, Spain.
Food Chem Toxicol. 2012 Jun;50(6):2034-41. doi: 10.1016/j.fct.2012.03.063. Epub 2012 Mar 23.
The aim of this study was to evaluate the applicability of different calibration approaches in trichothecenes analysis from wheat flour. Concretely eight trichothecenes (five type B trichothecenes and three type A trichothecenes) were analyzed by matrix solid-phase dispersion (MSPD) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). In the first set of experiments the presence of matrix effects was evaluated; values ranged between 59% and 79%. In the second set of experiments, solutions to compensate these signal suppressions were examined. Different calibration methods showed to tackle matrix effects obtaining values between 69% and 85% for external matrix matched calibration and values from 76% to 111% and from 78% to 108% by analog and deuterated internal standard calibrations, respectively. Trueness of the method was studied using quality control material and certificated reference material (DON 1062 ± 110 μg kg(-1)). The values were compared by matrix-matched, analog internal standard (deepoxydeoxynivalenol (DOM-1)) and deuterated internal standard (DON-d(1)).
本研究旨在评估不同校准方法在小麦粉中分析曲菌烯类毒素的适用性。具体而言,通过基质固相分散(MSPD)和液相色谱-串联质谱(LC-MS/MS)分析了八种曲菌烯类毒素(五种 B 型曲菌烯类毒素和三种 A 型曲菌烯类毒素)。在第一组实验中,评估了基质效应的存在;其值在 59%至 79%之间。在第二组实验中,研究了补偿这些信号抑制的解决方案。不同的校准方法显示可以解决基质效应,外部基质匹配校准的回收率在 69%至 85%之间,模拟和氘代内标校准的回收率分别在 76%至 111%和 78%至 108%之间。通过使用质量控制材料和认证参考材料(DON 1062 ± 110 μg kg(-1)),研究了该方法的准确性。通过基质匹配、模拟内标(脱氧去氧镰刀菌烯醇(DOM-1))和氘代内标(DON-d(1))对结果进行了比较。