SEARCHCROSS-SECTIONALpublic_health, pharmacology

cross-sectional·public_health, pharmacology, toxicology, food_safety, environmental_health·PMC10014665

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

Environmental Geochemistry and Health · 3 authors, 4 centres

AI SUMMARY

FIDELITY 80%

POPULATIONHoney samples collected from 7 regions in Egypt (n=33), 8 regions in Libya (n=33), and 6 regions in Saudi Arabia (n=18)

INTERVENTIONDetection and quantification of sulfonamide (SMT, SMX, SDM) and tetracycline (OTC, TC, CTC) residues using HPLC-DAD and HPLC-MS/MS

COMPARISONComparison of antibiotic occurrence across three countries and against Swiss MRLs (50 µg/kg for SAs, 20 µg/kg for TCs)

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TL;DR

This study developed and validated multi-residue methods using HPLC-DAD and HPLC-MS/MS to detect sulfonamides (SAs) and tetracyclines (TCs) in honey from Egypt, Libya, and Saudi Arabia. SAs were dominant in Egyptian and Saudi Arabian samples, while TCs were most prevalent in Libyan samples, with some concentrations exceeding Swiss maximum residue limits. Despite elevated levels in some samples, the risk assessment indicated no significant health risk from honey consumption alone, though chronic exposure concerns remain.

Full summary

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**Background:** Honey is a complex natural food matrix containing over 300 chemical substances and is valued for its antimicrobial properties and traditional medicinal use. Contamination of honey by antibiotic residues, particularly sulfonamides (SAs) and tetracyclines (TCs), has been frequently reported due to their use in apiculture to treat bacterial infections such as American foulbrood. Chronic exposure to residual antibiotics can cause liver injury, allergic reactions, damage to bones and teeth, and contribute to antimicrobial resistance, which the WHO has classified as 'one of the greatest threats to public health.' No maximum residue limits (MRLs) for antibiotics in honey exist in Egypt, Libya, or Saudi Arabia, though Swiss authorities have set MRLs of 50 µg/kg for SAs and 20 µg/kg for TCs. This study aimed to introduce and validate multi-residue methods for determining SAs and TCs in honey, survey their occurrence across three Arabian countries, and assess potential health risks.

**Methods:** Eighty-four honey samples were collected: 33 from Egypt (7 regions), 33 from Libya (8 regions), and 18 from Saudi Arabia (6 regions). Samples were pure, unfiltered, and unprocessed. Six antibiotics were targeted: sulfamethazine (SMT), sulfamethoxazole (SMX), sulfadimethoxine (SDM), oxytetracycline (OTC), tetracycline (TC), and chlortetracycline (CTC). Two extraction methods were employed: (1) matrix solid-phase dispersion (MSPD) using diatomaceous earth for SAs, eluted with acetone and acetonitrile; (2) EDTA McIlvain's buffer (pH 4.5) with 10% TCA and SPE clean-up using Oasis HLB 200 mg cartridges for TCs. Analysis was performed using HPLC-DAD (Agilent 1100) and HPLC-MS/MS (Agilent 1260 with Thermo Finnigan LCQ Duo ion trap). Method validation assessed linearity, detection limits (DL), quantification limits (QL), accuracy, and precision. Risk assessment used estimated daily intake (EDI), source-related hazard quotient (HQ_S), source-related hazard index (HI_S), and adversity-specific hazard index (HI_A), with ADI values of 3 µg/kg bw/day for SAs and 5 µg/kg bw/day for TCs.

**Key Results:** HPLC-MS/MS showed markedly lower DLs (0.01–0.04 ng/g) compared to HPLC-DAD (2.5–21 ng/g). The MSPD method achieved high accuracy for SAs (83.07–86.93%) but low recovery for TCs (45.48–50.20%). The EDTA buffer method achieved high accuracy for TCs (86.90–91.19%) but low recovery for SAs (57.81–65.63%). RSD values for all methods were below 15%, meeting EU directive 2002/657/EC requirements. In Egypt, 57.6% of samples (19/33) were positive for antibiotics; SMT and SMX showed 100% incidence in positive samples, while SDM was not detected. The highest average concentrations were SMX in Giza (86.9 µg/kg) and TC in Dakahlia (131.75 µg/kg). In Libya, 75% of samples (18/24) were positive, with TCs dominating; 87.5% of positive samples exceeded Swiss MRLs. CTC showed the highest average concentration (157.32 µg/kg), followed by TC (137.21 µg/kg). In Saudi Arabia, 77.7% of samples (14/18) were positive; SAs were most abundant (78.5% of positive samples), with SMT averaging 8.54 µg/kg and SMX 5.40 µg/kg. TC was detected in Abha and Al Bahah at 76.53 and 124.09 µg/kg, respectively. All HQ_S values were markedly below 1, with the highest for CTC in Libya (0.166) and TC in Libya (0.145). HI_S values for SAs were highest in Libya (0.338), followed by Saudi Arabia (0.168) and Egypt (0.156). HI_A values for both antibiotic groups were within safe ranges.

**Clinical Implications:** The study demonstrates that validated HPLC-DAD and HPLC-MS/MS methods are suitable for routine monitoring of antibiotic residues in honey. While the risk assessment indicates no immediate health threat from honey consumption alone, the detection of concentrations exceeding Swiss MRLs—particularly in Libyan samples where 87.5% of positive samples exceeded limits—highlights the need for regulatory action. The authors note that chronic exposure to antibiotics, especially from samples with the highest detected concentrations (e.g., SMX at 275.08 µg/kg in Giza, CTC at 462.48 µg/kg in Khoms), could represent a potential public health risk. The findings support calls for international bodies such as the EU and US FDA to establish MRLs for antibiotics in honey and for improved control of antibiotic use in apiculture, including natural alternatives.

PICO

PPOPULATION

Honey samples collected from 7 regions in Egypt (n=33), 8 regions in Libya (n=33), and 6 regions in Saudi Arabia (n=18)

IINTERVENTION

Detection and quantification of sulfonamide (SMT, SMX, SDM) and tetracycline (OTC, TC, CTC) residues using HPLC-DAD and HPLC-MS/MS

OOUTCOME

Occurrence rates, concentration levels, accuracy/precision of extraction methods, and risk characterization parameters (HQ_S, HI_S, HI_A)

STUDY TYPE

cross-sectional

SPECIALTY

public_health

SUMMARISED BY

AI pipeline

FIDELITY CHECK

80% · B

ORIGINAL PAPER

PMC10014665

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

Environmental Geochemistry and Health

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ABSTRACT

Abstract 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. Supplementary Information The online version contains supplementary material available at 10.1007/s10653-022-01258-0. Keywords: Bee’s honey, Contamination, Sulfonamides, Tetracyclines, Chromatographic analysis, Method validation, Risk assessment

CITATION EXPORT

Mohamed Bedair M Ahmed, Amro Ahmed Taha, Fathy Mohamed Saber Mehaya. Method validation and risk assessment for sulfonamides and tetracyclines in bees’ honey from Egypt, Libya and Saudi Arabia. Environmental Geochemistry and Health. (2022). https://doi.org/10.1007/s10653-022-01258-0

AUTHORS

3 · 4 CENTRES

Mohamed Bedair M Ahmed, Amro Ahmed Taha, Fathy Mohamed Saber Mehaya

1Department of Food Toxicology and Contaminants, National Research Centre, 33 El-Bohouth Street, P. O. box: 12622, Dokki Cairo, Egypt
2Beekeeping Research Department, Plant Protection Research Institute, Agricultural Research Center, Dokki Giza, Egypt
3Department of Food Technology, National Research Centre, 33 El-Bohouth Street, P. O. box: 12622, Dokki Cairo, Egypt
4Research and Training Station, King Faisal University, Al-Ahsa, Saudi Arabia