<abstract xmlns="http://www.w3.org/1999/xhtml"><sec id="j_jvetres-2020-0031_s_005_w2aab3b7c28b1b6b1aab1c14b1Aa"><h3>Introduction</h3><p>The authorisation of tylosin as feed additive was withdrawn for reasons of human health concerning resistance of pathogenic bacteria. An analytical method for the identification and quantification of tylosin in animal feed was developed and validated.</p></sec><sec id="j_jvetres-2020-0031_s_006_w2aab3b7c28b1b6b1aab1c14b2Aa"><h3>Material and Methods</h3><p>The samples were extracted using an acidified methanol:water mixture and solid-phase extraction was employed for the isolation of the antibiotic from diluted feed samples. Tylosin was analysed by liquid chromatography with electrospray ionisation mass spectrometric detection. The method’s performance was evaluated in adherence to the Commission Decision 2002/657/EC.</p></sec><sec id="j_jvetres-2020-0031_s_007_w2aab3b7c28b1b6b1aab1c14b3Aa"><h3>Results</h3><p>The recovery of the analyte from spiked samples was determined to be in the range from 78.9% to 108.3% depending on tylosin concentrations. The CCα and CCβ values for tylosin in feeds were determined at 0.085 mg kg<sup>-1</sup> and 0.091 mg kg<sup>-1</sup>, respectively. The method detection limit was found to be 0.035 mg kg<sup>-1</sup> and the quantification limit 0.05 mg kg<sup>-1</sup>. The applicability of the developed method was tested by analysing real feed samples.</p></sec><sec id="j_jvetres-2020-0031_s_008_w2aab3b7c28b1b6b1aab1c14b4Aa"><h3>Conclusion</h3><p>A reliable LC-MS method was developed to identify and quantify tylosin in animal feed with a good repeatability and a high specificity and sensitivity. Because of these characteristics, the proposed method is applicable and could be deemed necessary within the field of feed control and safety.</p></sec></abstract>

IntroductionThe authorisation of tylosin as feed additive was withdrawn for reasons of human health concerning resistance of pathogenic bacteria. An analytical method for the identification and quantification of tylosin in animal feed was developed and validated.Material and MethodsThe samples were extracted using an acidified methanol:water mixture and solid-phase extraction was employed for the isolation of the antibiotic from diluted feed samples. Tylosin was analysed by liquid chromatography with electrospray ionisation mass spectrometric detection. The method’s performance was evaluated in adherence to the Commission Decision 2002/657/EC.ResultsThe recovery of the analyte from spiked samples was determined to be in the range from 78.9% to 108.3% depending on tylosin concentrations. The CCα and CCβ values for tylosin in feeds were determined at 0.085 mg kg-1 and 0.091 mg kg-1, respectively. The method detection limit was found to be 0.035 mg kg-1 and the quantification limit 0.05 mg kg-1. The applicability of the developed method was tested by analysing real feed samples.ConclusionA reliable LC-MS method was developed to identify and quantify tylosin in animal feed with a good repeatability and a high specificity and sensitivity. Because of these characteristics, the proposed method is applicable and could be deemed necessary within the field of feed control and safety.

Identification and quantification of tylosin in animal feed by liquid chromatography combined with electrospray ionisation mass spectrometry

Journal of Veterinary Research

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IntroductionThe authorisation of tylosin as feed additive was withdrawn for reasons of human health concerning resistance of pathogenic bacteria. An analytical...

Parameter	Fortification level (mg kg^-1)	Results
Correlation coefficient		0.9985
Linearity (working range), mg kg^-1		0.05-2.0
LOD, mg kg^-1		0.035
LOQ, mg kg^-1		0.05
CCα, mg kg^-1		0.085
CCβ, mg kg^-1		0.091
Recovery, %(n = 18)	0.05	88.2
	0.25	78.9
	2.0	108.3
Repeatability, CV % (n = 6)	0.05	2.4
	0.25	9.9
	2.0	3.0
Within-laboratoryreproducibility, CV %(n = 18)	0.05	6.5
	0.25	6.9
	2.0	6.5
Uncertainty (k = 2, p < 95), %	0.05	21.4
	0.25	19.7
	2.0	23.8

Identification and quantification of tylosin in animal feed by liquid chromatography combined with electrospray ionisation mass spectrometry

Published Online: May 08, 2020

Page range: 299 - 304

Received: Aug 21, 2019

Accepted: Apr 17, 2020

DOI: https://doi.org/10.2478/jvetres-2020-0031

Keywords
feed, antibiotics, tylosin, feed analysis, LC-MS

© 2020 M. Przeniosło-Siwczyńska et al. published by Sciendo

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

Results of the validation of the analytical method for the determination of tylosin in feeds

Identification and quantification of tylosin in animal feed by liquid chromatography combined with electrospray ionisation mass spectrometry

Published Online: May 08, 2020

Page range: 299 - 304

Received: Aug 21, 2019

Accepted: Apr 17, 2020

DOI: https://doi.org/10.2478/jvetres-2020-0031

Keywordsfeed, antibiotics, tylosin, feed analysis, LC-MS

© 2020 M. Przeniosło-Siwczyńska et al. published by Sciendo

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

Results of the validation of the analytical method for the determination of tylosin in feeds

Keywords
feed, antibiotics, tylosin, feed analysis, LC-MS