唐振涛 于刚 刘菲 俞凌云 薛康

摘要 [目的]建立QuEChERS-超高效液相色谱-串联质谱法同时检测苦荞样品中10种真菌毒素。[方法]苦荞样品经水和乙腈提取后，采用QuEChERS方法净化。通过超高效液相色谱-三重四级杆质谱在多反应监测模式（MRM）下进行目标真菌毒素的分析。试验对样品前处理、仪器分析条件进行优化;考察方法的基质效应、检出限、精密度、回收率等参数。[结果]根据基质效应考察结果，50%的目标真菌毒素具有显著的信号抑制/增强效应。为了补偿基质效应的影响，选用基质配标法进行目标真菌毒素的分析。方法的线性范围为0.5～50.0 μg/L（对于黄曲霉毒素B2、G2，线性范围为0.125～12.500 μg/L），检出限和定量限分别低至0.011和0.040 μg/L，回收率为89.70%～105.83%，RSD<9%（n=6）。[结论]建立的方法简便、可靠，具有较好的灵敏度和准确性，能有效用于苦荞样品中多组分真菌毒素的检测。

关键词 苦荞;多组分真菌毒素;QuEChERS;超高效液相色谱-三重四级杆质谱

中图分类号 TS211.7 文献标识码 A

文章编号 0517-6611（2021）01-0188-06

doi：10.3969/j.issn.0517-6611.2021.01.051

Abstract [Objective]To establish an analysis method for simultaneous determination of 10 mycotoxins in buckwheat samples based on QuEChERS-ultra-high performance liquid chromatography-tandem mass spectrometry.[Method]As a typical run，mycotoxins were extracted with water and acetonitrile，followed by purification with QuEChERS procedure.The target mycotoxins were analyzed by UPLC-MS/MS in multiple reaction monitoring （MRM） mode.The sample pretreatment and instrumental analysis method were respectively optimized.Finally，matrix effect，detection limits，precision and accuracy were investigated.[Result]According to the investigation of matrix effect，50% of the target mycotoxins have encountered prominent signal suppression / enhancement.To compensate the significant matrix effect，matrix-matched calibration curves were finally employed in this study.The linear range of targets were 0.5-50.0 μg/L （0.125-12.500 μg/L for AFB2，AFG2）.Detection limits （LOD） and quantification limits （LOQ） were respectively detected down to 0.011 and 0.040 μg/L.Recoveries were obtained ranging from 89.70% to 105.83% with RSD< 9%.[Conclusion]The established method exhibits several advantages of simplicity，reliability，good sensitivity and accuracy.It is feasible and effective to apply this method for determination of multi-mycotoxins in buckwheat samples.

Key words Buckwheat;Multi-mycotoxins;QuEChERS;UPLC-MS/MS

苦蕎是蓼科荞麦属植物，在我国西南、中南、华北等地均有分布。该类植物能适应环境恶劣的生长环境，主要作为粮食和饲料供人们使用。苦荞含有优于小麦、玉米等的蛋白质及氨基酸，还含有大量维生素和多种矿质元素，具有丰富的营养价值[1]。另一方面，苦荞富含黄酮类、甾体类、多糖等生物活性成分;药理学研究表明苦荞具有降血压、降血脂、降血糖、抗氧化、预防心血管疾病等作用[2-4]。随着苦荞药理作用的研究发现，“药食同源”的苦荞及其产品迎来广阔的市场前景，有关苦荞产品的开发利用也得到越来越多的关注[5]。然而，与其他谷物一样，苦荞面临着易被真菌毒素污染的难题[6]。……