Analysis of (Fluoro)quinolones in Honey with Online Sample Extraction and LC-MS/MS

Importance of the Topic

Honey is a highly complex natural product prone to antibiotic contamination due to extensive use of quinolones in apiculture and animal production. Reliable screening methods are essential to protect consumer health, support regulatory compliance and maintain the integrity of the food supply.

Objectives and Study Overview

The study aimed to develop a robust LC MS MS method for simultaneous quantification of 12 fluoroquinolones and four related quinolones in honey. It replaced conventional solid phase extraction with an automated online extraction workflow to boost throughput, reduce sample handling and enhance reproducibility across multiple analytes.

Methodology and Instrumentation

Sample preparation included simple water addition to honey, homogenisation and direct filtration into HPLC vials. Automated online extraction was performed using a TurboFlow Cyclone column on the Aria TLX 1 system. Chromatographic separation utilised a Hypersil GOLD column maintained at 40 degrees Celsius. Detection was achieved on a TSQ Quantum Ultra triple quadrupole operated in positive ion mode with SRM transitions optimised for each analyte.

Main Results and Discussion

The method demonstrated detection limits between 0.5 and 2.6 micrograms per kilogram and linear response up to 100 micrograms per kilogram, with correlation coefficients exceeding 0.99. Precision assessed as relative standard deviation remained below 17 percent. Online extraction reduced sample preparation time from six hours to forty minutes for twelve samples, while also minimising matrix interferences and improving signal to noise ratios.

Benefits and Practical Applications

• High throughput analysis suitable for routine monitoring of quinolone residues in honey and other food matrices
• Significant reduction in manual sample handling and solvent consumption compared to traditional SPE workflows
• Enhanced reproducibility and sensitivity for trace level quantitation of multiple antibiotics

Future Trends and Opportunities

Advances in online sample extraction and mass spectrometry are expected to further decrease analysis time and expand the range of detectable contaminants. Integration with high resolution accurate mass screening and automation for data processing will open new possibilities for comprehensive food safety surveillance.

Conclusion

An online TurboFlow LC MS MS approach on the Aria TLX 1 and TSQ Quantum Ultra platform provides a rapid, sensitive and reliable solution for quantifying multiple quinolones in honey. This workflow offers substantial improvements in speed and data quality to support high throughput residue analysis in food safety laboratories.

References

1. Mottier P Hammel YA Gremaud E Guy PA Quantitative High Throughput Analysis of 16 Fluoroquinolones in Honey Using Automated Extraction by Turbulent Flow Chromatography Coupled to LC MS MS Journal of Agricultural and Food Chemistry 2008 56 35-43
2. Gunes N Cibik R Gunes ME Aydin L Erythromycin Residue in Honey from the Southern Marmara Region of Turkey Food Additives and Contaminants 2008 25 1313-1317
3. US Food and Drug Administration Preparation and LC MS MS Analysis of Honey for Fluoroquinolone Residues 2006
4. EU Commission Regulation No 2377/90 Laying Down a Community Procedure for the Establishment of Maximum Residue Limits of Veterinary Medicinal Products in Foodstuffs of Animal Origin Official Journal of the European Communities 1990 L224 1-8