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HPLC Method Validation for Simultaneous Determination of Three Mycotoxins from Corn Seeds

机译:HPLC方法验证同时测定玉米种子中三种霉菌毒素

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摘要

A new HPLC optimized method for simultaneous determination of some mycotoxins by separationand using a Dionex UltiMate3000 modular system, with multichannel UV detector was developedand validated. The method optimization was performed to determine simultaneously, several relevant mycotoxinsfrom corn seeds that were stored over 8 months. The mycotoxins selected for quantificationwere: aflatoxin B1, ochratoxin A and zearalenone. They were selected due to their high concentration inthe fodder. For the development stages of the HPLC method, it was introduced an internal standard tohave accurate results. Taking into account that the analytes should be extracted from the complex matrixthey reside, an extraction procedure was performed, using organic solvents, and the selection afterrepeated tests demonstrated the best capacity for ethyl acetate. The recovery is about 60–70 % after theextraction process also there is a good preconcentration (×2.5) of the analytes and the internal standard fortheir quantification.The limit of quantification (LOQ) obtained by chromatographic parameters optimization, for aflatoxinB1 and ochratoxin A were about 3–5 μg kg–1 and 14.4 μg kg–1 for zearalenone of raw biologicalmaterial, making these values lower than those accepted by the actual normatives and regulations.(doi: 10.5562/cca1788)
机译:开发并验证了一种新的HPLC优化方法,该方法可通过分离并使用带有多通道UV检测器的Dionex UltiMate3000模块化系统同时测定某些真菌毒素。进行了方法优化,以同时测定从玉米种子中储存的8个以上相关霉菌毒素。选择用于定量的真菌毒素为:黄曲霉毒素B1,曲霉毒素A和玉米赤霉烯酮。选择它们是因为它们在饲料中的浓度很高。在HPLC方法的开发阶段,引入了内标以达到准确的结果。考虑到应从存在的复杂基质中提取分析物,因此使用有机溶剂进行了提取程序,重复测试后的选择证明了乙酸乙酯的最佳分离能力。萃取后回收率约为60–70%,分析物和内标物的预富集程度也很好(×2.5)。通过色谱参数优化获得的黄曲霉毒素B1和och曲毒素A的定量限(LOQ)分别为玉米赤霉烯酮原料生物原料中的玉米赤霉烯酮的含量约为3–5μgkg-1和14.4μgkg-1,使这些值低于实际规范和法规所接受的值。(doi:10.5562 / cca1788)

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