Animal Feed Science and Technology 272 (2021) 114745
Available online 29 October 2020
0377-8401/© 2020 Elsevier B.V. All rights reserved.
Multi-detection method for mycotoxins with a modifed
QuEChERS extraction in feed and development of a simple
detoxifcation procedure
Jesús M. Gonz´ alez-Jartín
a
, Amparo Alfonso
a,
*, María J. Sainz
b
,
Mercedes R. Vieytes
c
, Luis M. Botana
a
a
Departamento de Farmacología, Facultad de Veterinaria, Universidade de Santiago de Compostela, 27002, Lugo, Spain
b
Departamento de Producci´ on Vegetal y Proyectos de Ingeniería, Facultad de Veterinaria, Universidade de Santiago de Compostela, 27002, Lugo,
Spain
c
Departamento de Fisiología, Facultad de Veterinaria, Universidade de Santiago de Compostela, 27002, Lugo, Spain
A R T I C L E INFO
Keywords:
QuEChERS
UHPLC-MS/MS
Mycotoxins
Feedstuffs
ABSTRACT
A new multi-mycotoxin analysis method was developed to identify and quantify 22 mycotoxins in
multiple feed matrices. This method is based on a QuEChERS (quick, easy, cheap, effective,
rugged and safe) extraction procedure followed by the ultra-high liquid chromatography tandem
mass spectrometry (UHPLC-MS/MS) detection. The QuEChERS extraction procedure was opti-
mized for minimizing the matrix effect of maize. Obtained recoveries ranged from 67 % to 94 %
and low LOQs (from 0.22 to 32.64 μg/kg) for regulated and emerging mycotoxins were obtained.
Then, the method was expanded to seven raw materials and eight feedstuffs. In these matrices, the
recovery for most mycotoxins was also high enough to fulfll the current legislation. The devel-
oped method was used for the analysis of 75 samples obtained from a nearby feed factory. Maize
and maize-based products showed the highest occurrence of mycotoxins, although always below
the legal limit. In addition, the ability of spheres of different composition and size to eliminate
mycotoxins from raw materials and feedstuffs was tested. Up to 28 % of the mycotoxin content
can be removed from matrices by using glass spheres of 2 mm of diameter. Therefore, a new
process for the physical removal of mycotoxins was developed.
Abbreviations: 15-AcDON, 15-acetyldeoxynivalenol; 3-AcDON, 3-acetyldeoxynivalenol; AFB
1
, afatoxin B
1
; AFB
2
, afatoxin B
2
; AFG
1
, afatoxin
G
1
; AFG
2
, afatoxin G
2
; BEA, beauvericin; CAV, cell accelerator voltage; CE, collision energy; DDGS, dried distillers grains with solubles; dMRM,
dynamic multiple reaction monitoring; DON, deoxynivalenol; DON-3Gluc, deoxynivalenol-3-glucoside; ELISA, enzyme-linked immunosorbent as-
says; ENNA, enniatin A; ENNA
1
, enniatin A
1
; ENNB, enniatin B; ENNB
1
, enniatin B
1
; ESI, electrospray ionization source; FB
1
, fumonisin B
1
; FB
2
,
fumonisin B
2
; FV, fragmentor voltage; HT-2, HT-2 toxin; LOD, limit of detection; LOQ, limit of quantifcation; MgSO
4
, magnesium sulfate; NaCl,
sodium chloride; NEO, neosolaniol; OTA, ochratoxin A; PSA, primary and secondary amine; QuEChERS, Quick, Easy, Cheap, Effective, Rugged and
Safe; R
A
, apparent recoveries; R
E
, recovery of the extraction; RSD, relative standard deviation; SSE, signal suppression/enhancement; T-2, T-2 toxin;
UHPLC-MS/MS, ultra-high liquid chromatography tandem mass spectrometry; ZEN, zearalenone; α-ZEN, α-zearalenol; β-ZEN, β-zearalenol.
* Corresponding author.
E-mail address: amparo.alfonso@usc.es (A. Alfonso).
Contents lists available at ScienceDirect
Animal Feed Science and Technology
journal homepage: www.elsevier.com/locate/anifeedsci
https://doi.org/10.1016/j.anifeedsci.2020.114745
Received 21 January 2020; Received in revised form 21 October 2020; Accepted 23 October 2020