Abstract

BackgroundWhen present in animal feedstuff, mycotoxins contaminants and antibiotic residues can have negative implications for animal production and Public Health, including the transmission of carcinogenic compounds and the selection of antibiotic resistant bacteria, respectively. So far there are no available methods in which both mycotoxins and antibiotic residues are analyzed using a parallel extraction approach. To address this issue, we developed a LC/MS methodology with high sensitivity (0.005 to 6.42 and 24.55 to 132.73 μg kg− 1 for mycotoxins and antimicrobials) and specificity (unique target ion mass/charge) that allows the detection of 26 mycotoxins and 23 antibiotic residues in animal feedstuff and validated it through the determination of these analytes in 294 animal feed and feed ingredient samples in the framework of a country-wide surveillance program. Two hundred and five of these samples were analyzed for mycotoxins and 89 for antibiotics.FindingsFumonisin was the most frequently toxin found, with FB1 and FB2 presenting prevalences of 50 and 52% and maximum concentrations of 14,927.61 and 8646.67 μg kg− 1, respectively. Other toxins, including diacetoxyscirpenol n = 4/101 (3.96%), fusarenon-X n = 2/101 (1.98%), citrinin n = 2 (1.98%), and patulin n = 1 (0.99%) were rarely found. Toxicologically relevant concentrations of toxin metabolites, such as HT-2 (6.38–485.49 μg kg− 1) and 3−/15-acetoxydeoxynivalenol (877.89–3236.56/5.44–1685.3 μg kg− 1), were also found. Few samples exceeded threshold mycotoxin concentrations defined in current EU guidelines. Dairy cattle and swine feeds included the higher number of samples exceeding guideline values (n = 6 and n = 5, respectively). From the total of samples analysed for antibiotics, 7.7% (n = 7/89) were classified as medicated for poultry and pigs. Unexpectedly, 57% of these medicated samples contained no detectable antibiotics (n = 4/7). The remaining 43% of the samples (n = 3/7) presented inconsistencies regarding the concentration of analytes declared on the labels or the antibiotics found. Likewise 74.6% (n = 50/67) of the non-medicated feed samples analyzed had antibiotic residues. Additionally, we analyzed commercial monensin standards for purity and evaluate batch-to-batch flushing feed industry practices.ConclusionsHerein we report the results for a year-wide analysis for mycotoxins and antibiotics in feed samples. Mycotoxins, several metabolites, and the occurrence of these emerging contaminants were evaluated and antibiotic residues in non-medicated feed samples were found using a targeted MS-based LC approach. This validated multi-analyte method is expected to facilitate the monitoring and surveillance of contaminants, from natural and anthropogenic origin, in animal feed.

Highlights

  • Mycotoxins and antibiotics represent natural and intentional contaminants of animal feed (Pinotti et al 2016; Tang et al 2017), respectively

  • We developed a Liquid chromatography (LC)/Mass spectrometry (MS)-based methodology that allows the analysis of 26 mycotoxins and 23 antibiotic residues in these matrices with high sensitivity and specificity

  • Bias, and reliability, our method only differed from those declared by the manufacturer by one standard deviation (Table 2)

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Summary

Introduction

Mycotoxins and antibiotics represent natural and intentional contaminants of animal feed (Pinotti et al 2016; Tang et al 2017), respectively. The most important mycotoxins contaminating animal feed include the aflatoxins B1, B2, G1, and G2, patulin, citrinin, ochratoxin A and B, fumonisin B1, Fumonisin B2, Type A trichothecenes, zearalenone, and emerging mycotoxins such as enniatins (Eskola et al 2018; Marín et al 2013; Wu et al 2014) Most of these substances are stable and cannot be eliminated by common feed and food production processes (Karlovsky et al 2016; Pinotti et al 2016), they can diminish animal productivity or exert toxic effects on animals (Bezerra da Rocha et al 2014; De Ruyck et al 2015; Zain 2011), such as cancer (i.e. aflatoxin B1 and fumonisin B1, Ostry et al 2017). Two hundred and five of these samples were analyzed for mycotoxins and 89 for antibiotics

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