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基于氨基化多壁碳纳米管-d-SPE-LC-MS/MS测定油籽油料中的10种真菌毒素
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王思源(1999-),女,硕士,研究方向:食品、油脂方面的检测,E-mail:wsyyy0101@163.com 通讯作者:王静静(1982-),女,博士,高级工程师,研究方向:食品安全检测,E-mail:wjjyezi@163.com

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新疆维吾尔自治区自然科学基金资助项目(2021D01A34)


Determination of 10 Mycotoxins in Oilseeds by d-SPE-LC-MS/MS using Amine-functionalized Multi-walled Carbon Nanotubes
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    摘要:

    为了快速检测油籽油料中的10种真菌毒素,以氨基化多壁碳纳米管(Aminated Multi-walled Carbon Nanotubes, NH2-MWCNTs)作为分散固相萃取(Dispersive Solid Phase Extraction, d-SPE)的吸附剂,采用液相色谱串联质谱法(Liquid Chromatography-tandem Mass Spectrometry, LC-MS/MS)同时测定油籽油料中10种真菌毒素。通过X射线衍射(X-Ray Diffraction, XRD)、傅里叶红外光谱分析(Fourier Transform Infrared Spectroscopy, FTIR)、透射电子显微镜分析(Transmission Electron Microscopy, TEM)等表征方法表明了改性后的NH2-MWCNTs表面缺陷明显增多;以NH2-MWCNT作为d-SPE的吸附剂,对影响提取效率的提取液种类、净化剂类型及添加量等因素进行了优化,对所建立的检测方法进行了方法学考察。结果表明:2%体积分数的甲酸的乙腈-水(80:20)作为提取液,20 mg NH2-MWCNTs作为净化剂时为最优前处理条件;10种真菌毒素在1~20 μg/kg范围内线性关系良好,方法的检出限(Limit of Detection, LOD)在0.04~0.19 μg/kg之间,定量限(Limit of Quantitation, LOQ)在0.13~0.63 μg/kg之间,加标回收率和相对标准偏差分别为70.33%~111.67%和0.55%~9.60%。该方法操作简便快捷、大大缩短了前处理时间、有机溶剂消耗少、整个过程绿色环保,适用于油籽油料中多种类真菌毒素的测定。

    Abstract:

    Mycotoxin contamination in oilseeds is of particular concern because of their potential adverse effects, hence reliable analytical methods are required for detection and quantification. This study aims to develop a rapid method for the detection of ten mycotoxins in oilseeds using amine-functionalized multi-walled carbon nanotubes (NH2-MWCNTs) as adsorbents for dispersive solid-phase extraction (d-SPE) coupled with liquid chromatography-tandem mass spectrometry (LCMS/MS). The structural and morphological characteristics of NH2-MWCNTs were analyzed using X-ray diffraction method, fourier transform infrared spectroscopy, and transmission electron microscopy, confirming increased surface defects after modification. The optimal pretreatment conditions were identified as 2% (V/V) formic acid in acetonitrile-water (80:20) as the extraction solvent and 20 mg NH2-MWCNTs as the adsorbent. The 10 mycotoxins exhibited good linearity within 1-20 μg/kg. The detection and quantitation limits ranged from 0.04 to 0.19 μg/kg and 0.13 to 0.63 μg/kg, respectively. The spiked recovery rates were 70.33%~111.67% and 0.55%~9.60%, respectively. The proposed method is simple, rapid, and environmentally friendly, substantially reducing pre-treatment time and organic solvent consumption. Utilization of NH2-MWCNTs could be an effective approach for determining various mycotoxins in oilseeds.

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王思源,吴小勇,姚伟琴,舒圣元,巩志国,王静静.基于氨基化多壁碳纳米管-d-SPE-LC-MS/MS测定油籽油料中的10种真菌毒素[J].现代食品科技,2025,41(6):309-317.

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  • 收稿日期:2024-04-16
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  • 在线发布日期: 2025-09-17
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