Development and validation of a method for the determination of low-ppb levels of macrocyclic lactones in butter, using HPLC-fluorescence. (15th July 2015) - Macedo, Fabio
Highlights: Development and validation of a method to evaluate ML in butter samples. Heated liquid–liquid and ultrasonic extraction were employed. Performance parameters in accordance with international guidelines. ML residues detected in (some) real samples. First published method for this application. Abstract: An analytical method was developed and validated for the simultaneous determination of four macrocyclic lactones (ML) (abamectin, doramectin, ivermectin and moxidectin) in butter, using liquid chromatography with fluorescence detection. The method employed heated liquid–liquid extraction and a mixture of acetonitrile, ethyl acetate and water, with preconcentration and derivatization, to produce stable fluorescent derivatives. The chromatographic run time was <12.5 min, with excellent separation. The method validation followed international guidelines and employed fortified butter samples. The figures of merit obtained, e.g. recovery (72.4–106.5%), repeatability (8.8%), within-laboratory reproducibility (15.7%) and limits of quantification (0.09–0.16 μg kg −1 ) were satisfactory for the desired application. The application of the method to real samples showed that ML residues were present in six of the ten samples evaluated. The method proved to be simple, easy and appropriate for simultaneous determination of ML residues in butter. To our knowledge, this is the first method described for the evaluation of ML in butter.