Citation: WANG Ruiguo, GUO Lili, WANG Peilong, SU Xiao'ou, SONG Zhichao, LIN Gang, ZHU Ronghua. Simultaneous determination of 37 mycotoxins in grain and animal feed by impurity adsorption purification coupled with ultra-performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2020, 38(7): 817-825. doi: 10.3724/SP.J.1123.2019.12013 shu

Simultaneous determination of 37 mycotoxins in grain and animal feed by impurity adsorption purification coupled with ultra-performance liquid chromatography-tandem mass spectrometry

1.
Institute of Quality Standards and Testing Technology for Agricultural Products, Chinese Academy of Agricultural Science, Key Laboratory of Agrifood Safety and Quality, Ministry of Agriculture, Beijing 100081, China;
2.
Henan Institute of Veterinary Drug and Feed Control, Zhengzhou 450008, China;
3.
Alltech Biological Products(China)Co., Ltd, Beijing 100600, China

Corresponding author: SU Xiao'ou, suxiaoou@caas.cn
Received Date: 7 December 2019

Fund Project: National Key R&D Program of China (No. 2017YFC1600300)

A rapid method based on ultra-performance liquid chromatography-tandem mass spectrometry (UPLC–MS/MS) was developed for the simultaneous determination of 37 mycotoxins having various physicochemical properties in grain and animal feed samples. The 37 analytes were extracted from ground samples with acetonitrile-water-formic acid (84:15.9:0.1, v/v/v) by 20 min vibration, and purified using a commercial MLJ-1 pass-through solid-phase extraction (SPE) clean-up cartridge. The analytes were then separated on a reversed-phase BEH RP18 column by a gradient elution program with 0.1 mmol/L ammonium acetate (containing 0.1% (v/v) formic acid) aqueous solution and 0.1% (v/v) formic acid methanol solution as mobile phases. The separated analytes were detected by MS/MS in the multiple reaction monitoring (MRM) mode via ESI+/- ionization. The results showed that the purification was completed in 1 min and that the 37 analytes could be separated on the chromatographic column in 15 min. The 37 mycotoxins showed a linear relationship within their respective linear ranges, and the correlation coefficients of the matrix-matched calibration curves were greater than 0.98. The average recoveries at four spiked levels (limit of quantification (LOQ), LOQ×5, LOQ×10, LOQ×25) for all the targets except fumonisins ranged from 80% to 120%, with the relative standard deviations (RSDs) lower than 20% (n=6). The limits of quantification (LOQs) for all the analytes were between 2 and 40 μg/kg. The proposed method is simple, fast, and accurate, thus being suitable for detecting multiple mycotoxins in grain and animal feed samples.
- impurity adsorption,
- solid phase extraction (SPE),
- ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS),
- mycotoxins,
- grain,
- feed
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沈阳化工大学材料科学与工程学院沈阳 110142