Comparison of several extraction techniques for multiclass analysis of veterinary drugs in eggs using ultra-high pressure liquid chromatography–tandem mass spectrometry

• Published in: Analytica chimica acta 2010-02, Vol.661 (2), p.150-160
• Main Authors: Garrido Frenich, Antonia, Aguilera-Luiz, María del Mar, Martínez Vidal, Jose Luis, Romero-González, Roberto
• Format: Article
• Language: English
• Subjects: Analytical chemistry; Anthelmintics - analysis; Anthelmintics - chemistry; Anthelmintics - isolation & purification; Anti-Bacterial Agents - analysis; Anti-Bacterial Agents - chemistry; Anti-Bacterial Agents - isolation & purification; Chemical Fractionation - methods; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography, High Pressure Liquid; Eggs; Eggs - analysis; Exact sciences and technology; Extraction method; Food Analysis - methods; Multiclass analysis; Other chromatographic methods; Reproducibility of Results; Safety; Solid Phase Extraction; Solvents - chemistry; Spectrometric and optical methods; Tandem Mass Spectrometry; Time Factors; Ultra-high pressure liquid chromatography; Veterinary drugs; Veterinary Drugs - analysis; Veterinary Drugs - chemistry; Veterinary Drugs - isolation & purification
• ISSN: 0003-2670; 1873-4324
• DOI: 10.1016/j.aca.2009.12.016

This study compared four extraction methods for the simultaneous determination of tetracyclines, macrolides, quinolones, sulphonamides and anthelmintics (including benzimidazoles and avermectins) in eggs by ultra-high pressure liquid chromatography coupled to tandem mass spectrometry (UHPLC–MS/MS). Solvent extraction, solid-phase extraction (SPE), matrix solid-phase dispersion (MSPD) and modified QuEChERS procedure were compared in terms of recovery and number of veterinary drugs extracted. The solvent extraction procedure with a clean-up step provided better results than the other tested procedures. The QuEChERS procedure was simpler and faster, but extracted fewer compounds than solvent extraction. MSPD did not extract tetracyclines and quinolones, whereas macrolides and tetracyclines were not extracted when SPE was applied. The solvent extraction procedure was validated, obtaining recoveries ranging from 60% (sulfaquinoxaline) to 119% (levamisole) with repeatability values (expressed as relative standard deviations, RSDs) lower than 20% at two concentration levels (10 and 100 μg kg −1), except for erythromycin, emamectin and ivermectin that showed RSD values close to 25% at 10 μg kg −1. Limits of quantification (LOQs) were always equal or lower than 5 μg kg −1. Finally the method was applied to egg samples, and erythromycin, enrofloxacin, difloxacin, thiabendazole, emamectin and fenbendazole were detected in four samples.