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

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: 5 November 2020
Revised Date: 2 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).

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.
- Maize,
- Mycotoxins,
- Liquid chromatography-isotopic dilution mass spectrometry,
- Characterization technique
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