QuEChERS联合UPLC-Orbitrap/MS同时测定检测坚果和干制水果中60种真菌毒素
作者:
作者单位:

1.湖北省食品质量安全监督检验研究院,湖北 武汉 430075;2.国家市场监管重点实验室 动物源性食品中重点化学危害物检测技术,湖北 武汉 430075;3.湖北省食品质量安全检测工程技术研究中心, 湖北 武汉 430075

作者简介:

汪薇 女 高级工程师 研究方向为食品中危害物分析 E-mail: wangwei_hbqt@163.com

通讯作者:

余婷婷 女 高级工程师 研究方向为食品中危害物分析 E-mail: 271377735@qq.com

中图分类号:

R155

基金项目:

国家重点研发计划(2018YFC1602302)


Sixty mycotoxins in nuts and dried fruits simultaneously detected by QuEChERS combined with UPLC-Orbitrap/MS
Author:
Affiliation:

1.Hubei Provincial Institute for Food Supervision and Test, Hubei Wuhan 430075, China;2.Key Laboratory of Detection Technology of Focus Chemical Hazards in Animal-derived Food for State Market Regulation, Hubei Wuhan 430075, China;3.Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test, Hubei Wuhan 430075, China

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    摘要:

    目的 本文针对混合坚果和干制水果类休闲食品,建立同时测定该类食品中60种真菌毒素的方法。方法 选择富含油脂和糖分的花生和葡萄干两种典型食品基质,样品经QuEChERS(900 mg MgSO4、150 mg PSA、150 mg C18)净化,采用超高效液相色谱-串联静电场轨道阱高分辨质谱的一级全扫描结合二级数据依赖扫描模式进行分析。以保留时间和母离子精确质量数定性,母离子色谱峰面积定量,同时以二级特征碎片离子进行确证。结果 提取溶液pH值会显著影响真菌毒素的解离状态,进而影响其提取回收率。通过QuEChERS净化能有效除去样品中糖类和脂类等组分的干扰,提高定性定量的准确性。采用空白基质匹配标准曲线进行校正可以减小基质效应以达到定量分析要求,真菌毒素在各自的质量浓度范围内线性关系良好(决定系数R2>0.95),回收率60%~120%,相对标准偏差小于20%,另外有7种真菌毒素线性决定系数小于0.95,进行定性分析。结论 该方法灵敏度高,结果准确、可靠,适用于坚果和干制水果60种真菌毒素的定性定量分析。

    Abstract:

    Objective A qualitative and quantitative method was established for the simultaneous detection of 60 mycotoxins in nuts and dried fruits.Methods Peanuts and raisins, two typical food substrates rich in fat and sugar, were pre-processed by QuEChERS technique (900 mg MgSO4, 150 mg PSA, 150 mg C18), and analyzed by ultra-high performance liquid chromatography-high resolution mass spectrometry (UPLC-Orbitrap/MS) with full scan and data-dependent scanning (dd-MS2) mode. It was qualitatively determined by the retention time and accurate mass of mycotoxins, the chromatographic peak area was quantified, and the fragment ion information was used for confirmation.Results The results showed that the pH value of the extraction solution significantly affected the dissociation state of mycotoxins, which in turn affected the recovery rate. The interference of components such as carbohydrates and lipids in the sample was effectively removed by QuEChERS purification, and the accuracy of qualitative and quantitative analysis was improved. A blank matrix-matched standard curve was used for calibration to reduce the matrix effect and meet the quantitative analysis requirements. The mycotoxins had a good linear relationship within their respective mass concentration ranges (correlation coefficient R2>0.95), and the recoveries were 60%-120% with relative standard deviation less than 20%. The other seven mycotoxins with R2 less than 0.95 can be qualitatively analyzed.Conclusion Compared with the detection method based on triple quadrupole mass spectrometry, the high-resolution mass spectrometry method is easier to quantify, and there is no need to optimize the parent ion, product ion and collision energy for the target one by one,which can effectively reduce the difficulty and time consuming for multi-target analysis. The method has high sensitivity, accuracy and reliable results, and is suitable for the qualitative and quantitative analysis of 60 mycotoxins in nuts and dried fruits.

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汪薇,余婷婷,张莉,范志勇,江丰,王会霞. QuEChERS联合UPLC-Orbitrap/MS同时测定检测坚果和干制水果中60种真菌毒素[J].中国食品卫生杂志,2022,34(4):707-714.

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  • 收稿日期:2021-12-30
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  • 在线发布日期: 2022-08-26
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