Evaluation of hydrophilic interaction liquid chromatography–tandem mass spectrometry and extraction with molecularly imprinted polymers for determination of aminoglycosides in milk and milk-based functional foods

Abstract

An analytical method for the determination of eleven aminoglycosides in different types of milk and milk-based functional products has been optimized and validated. A hydrophilic interaction chromatography (HILIC) column was proposed for the separation of analytes by ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS). A commercially molecularly imprinted polymer has been used for the solid phase extraction of the analytes, in order to achieve high selectivity in the sample treatment. The proposed method was characterized for different types of milk (whole cow milk, skimmed cow milk, whole goat milk) and functional dairy products, such as follow-on milk, Omega 3-enriched milk and isoflavones-enriched milk. Matrix effect was studied in the different matrices, being lower than │15│% in all cases, showing that the proposed procedure provided very clean extracts. Limits of quantification in the range 4.2–49µgkg−1 were estimated, well below the maximum residue limits established by the European Union. Recoveries ranged from 70% to 106% with RSD lower than 13%, in compliance with the current legislation. The combination of HILIC to solve the difficulties of the separation of these very polar compounds in reverse phase with the use of MISPE for sample treatment and MS/MS detection provided a very sensitive, highly selective, robust and useful method for identification and quantification of aminoglycoside residues in different types of milk and milk-based products.