This is an outdated version published on 08-03-2026. Read the most recent version.

Development and validation of a simples and fast method for sulfonamides, tetracyclines and macrolides in honey using LC-MS/MS

Authors

  • Cristina Belissimo Ribeiro Laboratorio Nacional Agropecuário-LANAGRO/RS do Ministério da Agricultura Pecuéaria e Abastecimento
  • Magda Targa Martins Laboratorio Nacional Agropecuário-LANAGRO/RS do Ministério da Agricultura Pecuéaria e Abastecimento
  • Louise Jank Laboratorio Nacional Agropecuário-LANAGRO/RS do Ministério da Agricultura Pecuéaria e Abastecimento
  • Fabiano Barreto Laboratorio Nacional Agropecuário-LANAGRO/RS do Ministério da Agricultura Pecuéaria e Abastecimento
  • Rodrigo Barcellos Hoff Laboratorio Nacional Agropecuário-LANAGRO/RS do Ministério da Agricultura Pecuéaria e Abastecimento
  • Juliana Bazzan Arsand Laboratorio Nacional Agropecuário-LANAGRO/RS do Ministério da Agricultura Pecuéaria e Abastecimento

DOI:

https://doi.org/10.22456/2527-2616.84248

Keywords:

sulfonamides, tetracyclines, macrolides, validation, LC-MS/MS, residues

Abstract

Antibacterial are widely used in veterinary applications for diseases treatment and prophilatic purposes. Inadequate uses of these drugs can lead of undesirable residues in honey for consumption. In Brazil, the legal authorities set a maximum residue limit (MRL) for different compound in honey, ranging from 10 to 20 ng ml-1. The monitoring of antibacterials is a concern, since it constitutes a risk to human health and collaborates with the growth of resistant bacteria. Brazil has the National Residue Control Plan (NRCP) to ensure that the products traded are compliant with the safety and quality criteria required by consumers. The goal of this work was to develop and validate a method suitable to determine sulfonamides, tetracyclines and macrolides in honey, using liquid chromatography tandem mass spectrometry. The main objective was to develop an efficient technique, combining simplicity, speed and low cost, since the method will be employed in routine analysis. Recoveries between 36 to 139% were obtained. Good linearity (r2) above 0.95, considering three different days, for all drugs was achieved in concentrations ranging from 0 to 200% of the MRL. Intraday and inter-day precision with CV% (n=6) lower than 18%, in agreement with specifications were obtained in concentrations ranging from 0.5 to 1.5 MRL, except for erythromycin. Accuracy was between 97 to 108%. Limits of quantitation for macrolides were 2.5 ng g-1and for sulfonamides and tetracyclines were 5 ng g-1. Decision limit (CCα) was evaluated and the results obtained were between 12.9 to 28.1 ng g-1. The detection capability (CCβ) obtained was between 15.8 to 36.3 ng g-1. The proposed method demonstrated to be suitable for this intended purpose and will contribute to antibacterial honey monitoring.

Downloads

Download data is not yet available.

References

Al-Waili N, Salom K, Al-Ghandi A, Ansari JM. Antibiotic, pesticide, and microbial contaminants of honey: human health hazards. The scientific world jornal. 2012; 2012. DOI: https://doi.org/10.1100/2012/930849

Anderson CR, Rupp HS, Wu WH. Complexities in tetracyclines analysis – chemistry, matrix extraction, clenup, and liquid chromatography. Journal of chromatography A. 2005; 1075, 23-32. DOI: https://doi.org/10.1016/j.chroma.2005.04.013

Baquero F, Martínez JL, Cantón R. Antibiotics and antibiotic resistance in water environments. Current Option in biotechnology. 2008; 19(3), 260-265. DOI: https://doi.org/10.1016/j.copbio.2008.05.006

Barganska Z, Slebioda M, Namiesnik J. Determination of antibiotic residues in honey. Trends in analytical Chemistry. 2011; 30(7), 1035-1041. DOI: https://doi.org/10.1016/j.trac.2011.02.014

Benetti C, Piro R, Binato G, Angeletti R, Riancotto G. Simultaneous determination of lincomycin and five macrolide antibiotic residues in honey by liquid chromatography coupled to electrospray ionization mass spectrometry. Food additives and contaminants. 2006; 23(11), 1099-1108. DOI: https://doi.org/10.1080/02652030600699338

Berendsen BJA, Stolker LAAM, Nielen MWF. Selectivity in the sample preparation for the analysis of drug residues in products of animal origin using LC-MS/MS. Trends in analytical chemistry.2013; 43, 229-239. DOI: https://doi.org/10.1016/j.trac.2012.09.019

Boeckel TPV, Brower C, Gilbert M, Grenfell BT, Levin SA, Robinson TP, Teilland A, Laxminarayan R. Global trends in antimicrobial use in food animals. Agricultural sciences. Avalable at URL: http://www.pnas.org/cgi/doi/10.1073/pnas. 1503141112, 2015.

Brasil. MAPA. Ministry of agricultural, livestock and supply. Manual of analytical quality assurance.1st ed., MAPA/ACS, Brasília, 2011.

Commission Decision 2002/657/EC. Implementing Council Directive 96/23/EC concerning the performance of analytical methods and interpretation of results. Official jornal of Europeam communities. 2002; L239, 66-98.

Galarini R, Saluti G, Giusepponi D, Rossi R, Monetti S. Multiclass determination of 27 antibioticas in honey. Food control. 2015; 48, 12-24. DOI: https://doi.org/10.1016/j.foodcont.2014.03.048

Hammel Y, Mohamed R, Gremaud E, LeBreton M, Guy PA. Multiscreening approach to monitor and quantify 42 antibiotic residues in honey by liquid chromatography-tandem mass spectrometry. Journal of Chromatography. A. (2008); 1177(1), 58-76. DOI: https://doi.org/10.1016/j.chroma.2007.10.112

Kaufmann A, Roth S, Ryser B, Widmer M, Guggisberg D. Quantitative LC/MSMS determination of sulfonamides and some other antibiotics in honey. Journal of AOAC International. 2002; 85(4), 853- 860. DOI: https://doi.org/10.1093/jaoac/85.4.853

Kivrak I, Kivrak S, Harmandar. Development of a rapid method for the determination of antibiotic residues in honey using UPLC-ESI-MS/MS. Food Science and Technology. 2016; 36(1), 90- 96. DOI: https://doi.org/10.1590/1678-457X.0037

Kibroyesfa B and Haile N. Review on antibiotic residues in food of animal origin: economic and public health impacts. Applied jornal of hygiene. 2017; 6(1), 01-08.

Kümmerer K. Antibiotics in the aquatic environment – A review – Part I. Chemosphere. (2009). 75(4), 417-434. DOI: https://doi.org/10.1016/j.chemosphere.2008.11.086

Lee MH, Lee HJ, Ryu PD. Public health risks: chemical and antibiotic residuesreview. Asian-Australasian journal of animal sciences. 2001; 14(3), 402-413. DOI: https://doi.org/10.5713/ajas.2001.402

Lehotay SJ, Lightfield AR, HarmamFetcho JA, Donogue DJ. Analysis of pesticide residues in eggs by direct sample introduction/gas chromatography/tandem mass spectrometry. Journal of agricultural and food chemistry. 2001; 49, 4589-4596. DOI: https://doi.org/10.1021/jf0104836

Lopez MI, Pettis JS, Smith IB, Chu PS. Multiclass determination and confirmation of antibiotic residues in honey using LCMS/MS. Journal of Agricultural and Food Chemistry. 2008; 56(5), 1553-1559. DOI: https://doi.org/10.1021/jf073236w

Martinez-Vidal J L, Aguilera-Luiz MM, Romero-González R, Frenich AG. Multiclass analysis of antibiotic residues in honey by ultraperformance liquid chromatography-tandem mass spectrometry. Journal of Agricultural and Food Chemistry. (2009); 57(5), 1760- 1767. DOI: https://doi.org/10.1021/jf8034572

Normative Instruction (NI). Ministry of agricultural, livestock and supply. IN/09/2017.

Pan C, Zhang H, Chen S, Xuy Y, Jiang S. Determination of chloramphenicol residues in honey by monolithic column liquid chromatography-mass spectrometry after use of quechers clean up. Acta chromatographica. 2006; 17(17), 320-327.

Prestes OD, Friggi CA, Adaime MB, Zanella R. Um método moderno de preparo de amostra para determinação multirresídue de pesticidas por métodos cromatográficos acoplados à espectrometria de massas. Química nova. 2009; 32(6), 1620-1634. DOI: https://doi.org/10.1590/S0100-40422009000600046

Sheridan R, Policastro B, Thomas S, Rice D. Analysis and occurence of 14 sulfonamide antibacterials and chloramphenicol in honey by solid-phase extraction followed by LC-MS/MS analysis. Journal of agricultural and food chemistry. 2008; 56, 3509-3516. DOI: https://doi.org/10.1021/jf800293m

Sttubings G & Bigwood T. The development and validation of a multiclass liquid chromatography tandem mass spectrometry (LC-MS/MS) procedure for the determination of veterinary drug residues in animal tissue using a QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) approach. Analytica Chimica Acta, 2009; 57, 1467- 1480.

Downloads

Published

14-09-2018 — Updated on 08-03-2026

Versions

How to Cite

Ribeiro, C. B., Martins, M. T., Jank, L., Barreto, F., Hoff, R. B., & Arsand, J. B. (2026). Development and validation of a simples and fast method for sulfonamides, tetracyclines and macrolides in honey using LC-MS/MS . Drug Analytical Research, 2(1), 21–28. https://doi.org/10.22456/2527-2616.84248 (Original work published September 14, 2018)

Issue

Section

ORIGINAL ARTICLES