Extensive research on the presence of veterinary drug residues in food samples has been conducted and is still underway. The inappropriate or excessive use of veterinary drugs in food producing animals may result in trace quantities of these drugs or their metabolites in food samples. Food contamination by veterinary drug residues is one of the main challenges worldwide to public health with drug resistance being the biggest threat. One of the challenges in veterinary drug residue analysis is their occurrence in trace amounts that are normally below limits of detection of most analytical instruments. Various efficient, economical, miniaturized and environmentally friendly extraction methods have been developed in recent years to pre-concentrate these analytes before instrumental analysis to enhance their detection and also to overcome the limitations of traditional extraction methods such as liquid-liquid extraction and solid phase extraction. These methods include quick, easy, cheap, effective, rugged and safe (QuEChERS), molecularly imprinted polymers, dispersive liquid-liquid microextraction and hollow fiber liquid-phase microextraction, and they will be discussed in this chapter.

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BACKGROUND In this study, development and validation of a simple, miniaturized and, environmentally friendly carrier‐mediated three‐phase hollow‐fibre liquid‐phase micro‐extraction (HFLPME) technique was investigated for the enrichment of tetracycline residues in honey samples. The extracts were analysed using UV–visible spectrophotometry and liquid chromatography–quadrupole time‐of‐flight mass spectrometry (LC‐Q‐TOF/MS). Parameters affecting the extraction efficiency of HFLPME such as pH of the donor and acceptor solutions, salt addition, agitation speed and extraction time were optimized. RESULTS The calibration curves showed good linearity, in the range of 1–100 μg kg−1 with correlation coefficients ranging between 0.9943 and 0.9992, under the optimized conditions. Recoveries of blank honey samples at three spiking levels (1, 10 and 20 μg kg−1) ranged from 81.2% to 107.5%. Relative standard deviations for the precision of the method were less than 15.0%. Limits of detection and limits of quantification were in the range of 0.0861–0.2628 μg kg−1 and 0.2610–0.7964 μg kg−1, respectively. Finally, the proposed method was successfully applied in the extraction of five tetracyclines from honey samples. Doxycycline residue detected in one of the commercial honey samples was below the limit of quantification. CONCLUSION Because of the advantages offered by HFLPME, this method can be employed as an alternative to conventional extraction techniques for the clean‐up and pre‐concentration of antibiotics in complex matrices, including food samples. © 2021 Society of Chemical Industry

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