Determination of macrolide antibiotics in meat and fish using pressurized liquid extraction and liquid chromatography-mass spectrometry

We developed a method for determining the quantities of seven macrolide antibiotics in meat and fish by using pressurized liquid extraction (PLE) and liquid chromatography-mass spectrometry with electrospray ionization (LC-(ESI)MS). The PLE was optimized with regard to solvents, temperature, pressure, extraction time and number of cycles. The optimum conditions were: methanol as the extraction solvent: a temperature of 80 degrees C; a pressure of 1500 psi: an extraction time of 15 min; 2 cycles; a flush volume of 150% and a purge time of 300s. All recoveries for macrolide antibiotics were over 77% at 200 mu g/kg, except for erythromycin, which was 58%. The repeatability and reproducibility on days in between, expressed as %RSD (n = 12), were lower than 10% and 12%, respectively. The quantification limits of all compounds were 25 mu g/kg of dry weight of animal muscle except for troleandomycin (50 mu g/kg). The method was applied to determine the pharmaceuticals in real samples taken from 18 meat and fish samples. The results showed that PLE is quantitative short time consuming technique, with use of smaller initial sample sizes. Greater specificity and selectivity in extraction and increased potential for automation were shown. (C) 2008 Elsevier B.V. All rights reserved.