中文摘要：本研究成功开发并验证了快速准确的UPLC-MS/MS法，用于同时检测谷物和以谷物为基础的食品基质，如玉米、小麦、面食和大米中的白僵菌素、恩链孢菌素（A、A1、B、B1）和呕吐毒素。虽然这些新兴的食源性毒素源于不同的微生物，但它们具有类似的结构、毒理学及食品安全特点，因此能在相关的食品基质中进行并行测试。在电喷雾模式下，将Waters Acquit超高效液相色谱系统耦合到Waters Quattro Premier质谱仪，形成本检测法。样品预处理采用快速简便的萃取法分离目标毒素，无需洗涤。所有样品预处理都得到了可接受的毒素回收率：小麦85-105%，玉米87-106%,大米84-106%，面食85-105%。有效的提取方法，结合7分钟快速色谱分离，能节省大量的时间和费用，显示了本方法的鲁棒性和性能。方法验证按欧盟委员会第2002/657/EC号决议进行。食物基质中目标毒素的检测限为0.1-1.0μg/kg, 定量限为0.3-2.9μg/kg。该灵敏度允许检测相关的毒理学浓度。所有的重复性（日内）和精密度（日间）的相关标准差均低于20%。真实性，表现为明显的回收率为80～107%。高敏感性和重复性使本方法适用于57个自然污染的样品，能检测亚临床剂量的毒素。
外文摘要：Rapid and accurate UPLC-MS/MS methods for the simultaneous determination of beauvericin and the related enniatins (A, A1, B, B1), together with cereulide were successfully developed and validated in cereal and cereal-based food matrices such as wheat, maize, rice and pasta. Although these emerging foodborne toxins are of different microbial origin, the similar structural, toxicological and food safety features provided rationale for their concurrent detection in relevant food matrices. A Waters Acquity UPLC system coupled to a Waters Quattro Premier XE™ Mass Spectrometer operating in ESI+ mode was employed. Sample pretreatment involved a fast and simple liquid extraction of the target toxins without any further clean-up step. For all toxins the sample preparation resulted in acceptable extraction recoveries with values of 85-105% for wheat, 87-106% for maize, 84-106% for rice and 85-105% for pasta. The efficient extraction protocol, together with a fast chromatographic separation of 7min allowed substantial saving costs and time showing its robustness and performance. The validation of the developed method was performed based on Commission Decision 2002/657/EC. The obtained limits of detection ranged from 0.1 to 1.0μgkg-1 and the limits of quantification from 0.3 to 2.9μgkg-1 for the targeted toxins in the selected matrices. The obtained sensitivities allow detection of relevant toxicological concentrations. All relative standard deviations for repeatability (intra-day) and intermediate precision (inter-day) were lower than 20%. Trueness, expressed as the apparent recovery varied from 80 to 107%. The highly sensitive and repeatable validated method was applied to 57 naturally contaminated samples allowing detection of sub-clinical doses of the toxins.
外文关键词：Cyclic depsipeptides；Emerging mycotoxins；Fusarium；Cereulide；LC-MS analysis；Solvent extraction
作者：Decleer, M；Rajkovic, A；Sas, B；Madder, A；De Saeger, S
作者单位：Univ Ghent
期刊名称：JOURNAL OF CHROMATOGRAPHY A
期刊影响因子：3.926
出版年份：2016
出版刊次：11
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