Preprint Article Version 1 NOT YET PEER-REVIEWED

A Novel Method for Multiple Mycotoxins Analysis in Feedstuffs by Flow-Through Cartridge Purification and Ultra-High-Performance Liquid Chromatography Coupled to Tandem Mass Spectrometry

Version 1 : Received: 3 December 2016 / Approved: 5 December 2016 / Online: 5 December 2016 (09:40:24 CET)

How to cite: Wang, R.; Su, X.; Wei, Z.; Wang, P.; Zhang, Z.; Wu, A.; Cheng, C.; Xue, Y.; Li, Y. A Novel Method for Multiple Mycotoxins Analysis in Feedstuffs by Flow-Through Cartridge Purification and Ultra-High-Performance Liquid Chromatography Coupled to Tandem Mass Spectrometry. Preprints 2016, 2016120023 (doi: 10.20944/preprints201612.0023.v1). Wang, R.; Su, X.; Wei, Z.; Wang, P.; Zhang, Z.; Wu, A.; Cheng, C.; Xue, Y.; Li, Y. A Novel Method for Multiple Mycotoxins Analysis in Feedstuffs by Flow-Through Cartridge Purification and Ultra-High-Performance Liquid Chromatography Coupled to Tandem Mass Spectrometry. Preprints 2016, 2016120023 (doi: 10.20944/preprints201612.0023.v1).

Abstract

A novel determination method using flow-through cartridge purification and ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) was developed for the identification and quantification of 30 mycotoxins (aflatoxin B1, B2, G1, G2, sterigmatocysin, T-2 toxin, diacetoxyscirpenol, roquefortine C, methylergonovine, ergocornine, lysergol, enniatin A, enniatin A1, enniatin B, enniatin B1, beauvericin, deoxynivalenol, 3-acetylDeoxynivalenol, 15-acetylDeoxynivalenol, patulin, verruculogen, neosolaniol, gliotoxin, HT-2 toxin, wortmannin, zearalenone, α-zearalenol, β-zearalenol, α-zearalanol, and β-zearalanol) in feedstuffs. Mycotoxins were extracted from sample by 0.1% formic acid aqueous solution/acetonitrile (16/84 v/v), then purified by a Cleanert® MC clean-up column. As a result, the pigments and other matrices were efficient removed from the sample extract solution. The purified eluate was collected, then evaporated and redissolved by 0.1% formic acid aqueous solution/acetonitrile (70:30 v/v) for UPLC-MS/MS detection. A BEH Shield RP18 chromatographic column was employed for separation of 30 mycotoxins in a total of 14 min. Multiple-reaction monitoring (MRM) mode was applied for qualitative and quantitative analysis, and matrix calibration curves obtained with the external-standard method was used for quantitation of target analytes. Under optimized conditions, the linearity range was from 2 to 1000 ng/g, and the limit of quantification of the developed method was from 2 to 50 ng/g. The recoveries of 30 mycotoxins spiked in urine samples were from 72.0% to 118.5%, and the relative standard deviation was below 20%. The method was also well approved by certified reference sample, and applied on the real feedstuff samples testing successfully.

Subject Areas

UPLC-MS/MS; mycotoxins; feedstuffs; flow-through; multiple analysis

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