高准确度液相色谱-同位素稀释质谱定值技术测定玉米粉中多种真菌毒素

引用本文: 刘栓, 冯梦雨, 李晓敏, 唐光诗, 张庆合, 李秀琴. 高准确度液相色谱-同位素稀释质谱定值技术测定玉米粉中多种真菌毒素[J]. 分析化学, 2021, 49(4): 546-553. doi: 10.19756/j.issn.0253-3820.201650 shu

Citation: LIU Shuan, FENG Meng-Yu, LI Xiao-Min, TANG Guang-Shi, ZHANG Qing-He, LI Xiu-Qin. High Accuracy Liquid Chromatography-Isotopic Dilution Mass Spectrometry Method for Determination of Multi-mycotoxins in Maize[J]. Chinese Journal of Analytical Chemistry, 2021, 49(4): 546-553. doi: 10.19756/j.issn.0253-3820.201650 shu

高准确度液相色谱-同位素稀释质谱定值技术测定玉米粉中多种真菌毒素

刘栓 ^1,2, ,
冯梦雨 ^2, ,
李晓敏 ^2, ,
唐光诗 ^1, ,
张庆合 ^2, ,
李秀琴 ^{2,
,}

1.
北京化工大学理学院, 北京 100029;
2.
中国计量科学研究院化学计量与分析科学研究所北京 100029

通讯作者: 李秀琴,E-mail:lixq@nim.ac.cn

基金项目:
国家质量基础的共性技术研究与专项课题（No.2016YFF0201106）资助。

摘要: 建立了玉米粉中黄曲霉毒素（AFB1、AFB2、AFG1、AFG2）、脱氧雪腐镰刀菌烯醇、玉米赤霉烯酮、赭曲霉毒素A和伏马毒素B1的液相色谱-同位素稀释质谱（LC-IDMS-MS）测定方法。采用阳性样品对提取溶剂进行优化，结果表明，样品经过乙腈-水-甲酸（80：19.9：0.1，V/V）浸泡12 h后进行首次提取，再采用乙腈-水-甲酸（20：79.9：0.1，V/V）进行二次提取，提取效率更高，同时也证明对阳性样品进行提取条件的优化更科学和准确。研究了样品提取前浸泡时间、取样量等对提取效率以及方法精密度的影响，结果表明，样品浸泡12 h，可更有效地提取目标物；由于真菌毒素在基体中不易分布均匀，因此取样量直接影响方法的精密度，本方法的最小取样量为10 g。研究了8种真菌毒素在玉米粉中的基质效应，结果表明，真菌毒素在玉米粉中均有很强的基质抑制现象，基质效应在22%~77%之间；而且个别毒素与其相应的同位素标记物的基质效应有较大差异，如采用溶剂校准液进行定值，基质效应会直接影响测量结果的准确性。因此，在没有空白基质情况下，可采用校正因子θ值对定量结果进行校正，以消除基质效应的影响。本方法具有简单、快速、准确度高和灵敏度高等优点，可用于真菌毒素类基体标准物质的赋值。

关键词:

English

High Accuracy Liquid Chromatography-Isotopic Dilution Mass Spectrometry Method for Determination of Multi-mycotoxins in Maize

1.
School of Science, Beijing University of Chemical Technology, Beijing 100029, China;
2.
Division of Chemical Metrology and Analytical Science, National Institute of Metrology, Beijing 100029, China

Corresponding author: LI Xiu-Qin, lixq@nim.ac.cn

Received Date: 05 November 2020
Revised Date: 02 March 2021
Fund Project:
Supported by the National Quality-based Common Technical Research and Special Project "Development of Reference Materials Such as Typical Pollutants and Element Forms in Food" (No.2016YFF0201106).

Abstract: A high accuracy liquid chromatography-isotopic dilution mass spectrometry method for determination of aflatoxins B1, B2, G1, G2, deoxynivalenol, zearalenone, ochratoxin A and fumonisin B1 in maize was developed. For the first time, a positive sample was used to optimize the extraction solvent. The sample was soaked in acetonitrile-water-formic acid (80:19.9:0.1, V/V) for 12 hours for the first extraction, and then acetonitrile-water-formic acid (20:79.9:0.1, V/V) was used for the second extraction. The results proved that the optimization of extraction conditions for positive samples was more scientific and accurate. The effects of soaking time and sampling volume before sample extraction on extraction efficiency and method precision were also investigated. The results showed that after the sample was soaked for 12 hours, the target substance could be extracted more effectively. Due to the uneven distribution of mycotoxins in the matrix, the amount of sampling directly affected the precision of the method. The minimum sampling volume of this method was 10 g. The matrix effects of 8 mycotoxins in maize were also studied in detail. The results showed that mycotoxins had strong matrix inhibition in maize, and the matrix effects were between 22% and 77%. Moreover, the matrix effects of individual toxins and their corresponding isotope markers were quite different. If a solvent calibration solution was used for the determination, the matrix effect would directly affect the accuracy of the measurement results. Therefore, in the absence of a blank matrix, the correction factor θ could be used to correct the quantitative results to eliminate the influence of matrix effects. The method was simple and fast, and had many advantages such as high accuracy and high sensitivity, and could be applied to the assignment of certified reference material.

Key words:

Maize
/ Mycotoxins
/ Liquid chromatography-isotopic dilution mass spectrometry
/ Characterization technique

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沈阳化工大学材料科学与工程学院沈阳 110142

高准确度液相色谱-同位素稀释质谱定值技术测定玉米粉中多种真菌毒素

通讯作者: 李秀琴,E-mail:lixq@nim.ac.cn

English

High Accuracy Liquid Chromatography-Isotopic Dilution Mass Spectrometry Method for Determination of Multi-mycotoxins in Maize

Corresponding author: LI Xiu-Qin, lixq@nim.ac.cn

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

高准确度液相色谱-同位素稀释质谱定值技术 测定玉米粉中多种真菌毒素

通讯作者: 李秀琴,E-mail:lixq@nim.ac.cn

English

High Accuracy Liquid Chromatography-Isotopic Dilution Mass Spectrometry Method for Determination of Multi-mycotoxins in Maize

Corresponding author: LI Xiu-Qin, lixq@nim.ac.cn

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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高准确度液相色谱-同位素稀释质谱定值技术测定玉米粉中多种真菌毒素

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