Method validation and risk assessment for sulfonamides and tetracyclines in bees' honey from Egypt, Libya and Saudi Arabia

Environ Geochem Health. 2023 Mar;45(3):997-1011. doi: 10.1007/s10653-022-01258-0. Epub 2022 Apr 13.


Several studies worldwide have reported contamination of bees' honey by antibiotics, which may pose a hazard to consumers' health. The present study was thus established to: (1) introduce a validated multi-residue method for determining sulfonamides (SAs) and tetracyclines (TCs) in honey; and (2) characterize the potential risk due to the exposure to SAs and TCs in honey samples from Egypt, Libya, and Saudi Arabia. SAs and TCs were simultaneously extracted using solid-phase extraction and matrix solid phase dispersion methods. SAs and TCs were screened using HPLC-MS/MS and HPLC-DAD. The results confirmed detection limits for SAs and TCs by HPLC-MS/MS of 0.01 and 0.02-0.04 (ng g-1), respectively. The limits were 2.5-5.6 and 12.0-21.0 (ng g-1) for SAs and TCs by HPLC-DAD, respectively. The obtained accuracy rates were in the ranges of 83.07-86.93% and 86.90-91.19%, respectively, for SAs and TCs, with precision rates lower than 9.54%. Concerning the occurrence of antibiotics, the positive samples constituted 57.6%, 75%, and 77.7% of the Egyptian, Saudi Arabian, and Libyan samples, respectively. Notably, SAs antibiotics were the most prevalent in the Egyptian and Saudi Arabian samples; in contrast, TCs were the most dominant in Libya. Calculated parameters of risk assessment, concerning the aggregated exposure to SAs and TCs, showed no potential adverse effects from the exposure to contaminated honey in studied countries.

Keywords: Bee’s honey; Chromatographic analysis; Contamination; Method validation; Risk assessment; Sulfonamides; Tetracyclines.

MeSH terms

  • Animals
  • Anti-Bacterial Agents
  • Bees
  • Egypt
  • Honey* / analysis
  • Libya
  • Risk Assessment
  • Saudi Arabia
  • Sulfanilamide
  • Sulfonamides
  • Tandem Mass Spectrometry / methods
  • Tetracyclines* / analysis


  • Tetracyclines
  • Sulfonamides
  • Anti-Bacterial Agents
  • Sulfanilamide