超高效液相色谱-串联质谱检测燕麦中6种常见单端孢霉烯族毒素的方法研究

Detection of six common trichothecene toxins in oats by ultra-high performance liquid chromatography-tandem mass spectrometry

【目的】建立超高效液相色谱-串联质谱(UHPLC-MS/MS)检测燕麦中6种常见单端孢霉烯族毒素的方法,以监测燕麦中该毒素的含量。【方法】以燕麦为研究对象,采用响应曲面设计优化QuEChERS处理方法,并提供了一种快速、高效的样品提取净化策略,结合UHPLC-MS/MS用于同时定量分析燕麦中常见共污染的6种单端孢霉烯族毒素。【结果】该方法经验证各分析物在相应的浓度范围内具有良好的分析性能(r>0.99),准确度为87.26%~99.64%,日间和日内相对标准偏差分别小于6.8%和5.5%,具有实际应用潜力。将该方法应用于中国12份燕麦样品中真菌毒素的检测,发现1份样品呕吐毒素(DON)污染超标,同时单端孢霉烯族共污染现象普遍存在。【结论】此类毒素风险被低估,有必要开展持续广泛监测以提供污染数据从而评估消费者的风险。

[Objective]To establish a method using ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)for the detection of six common trichothecene toxins in oats.[Methods]Oats were selected as the research subject in this study.Response surface design was used to optimize the QuEChERS extraction method.Additionally,a rapid and efficient strategy for sample extraction and purification was developed.Combined with UHPLC-MS/MS,six commonly co-occurring trichothecene toxins in oats were quantitatively analyzed simultaneously.[Results]This method demonstrated good analytical performance for each analyte across the corresponding concentration ranges(r>0.99),with accuracy ranging from 87.26%to 99.64%.The inter-day and intra-day relative standard deviations were less than 6.8%and 5.5%,respectively,indicating its potential for practical application.This method was used to detect mycotoxins in 12 oat samples from China,and it was found that one sample exceeded the standard limits for deoxynivalenol(DON),and the co-contamination of trichothecene toxin was prevalent.[Conclusion]The risk posed by these toxins has been underestimated.Ongoing,extensive monitoring is necessary to provide contamination data to assess the consumer risk.