Rapid Determination of Aminoglycosides in Milk by Exact Ion Masses Using Ultra-High-Performance Liquid Chromatography–High Resolution Quadrupole Time-of-Flight Mass Spectrometry

Abstract

A method is proposed for the rapid determination of 10 aminoglycosides (amikacin, apramycin, gentamycin, hygromycin B, dihydrostreptomycin, kanamycin A, neomycin, paromomycin, spectinomycin, and streptomycin) in milk by exact ion masses in ultra-high-performance liquid chromatography–high resolution quadrupole time-of-flight mass spectrometry. A simple method for sample preparation is proposed. The determination of aminoglycosides is possible along with other veterinary drugs in milk under the conditions of reversed-phase chromatography with an addition of an ion-pair reagent (heptafluorobutyric acid) to the sample extract being analyzed. A significant matrix effect is observed in the determination of aminoglycosides in milk (79–96%), which is reduced by diluting the extract tenfold with deionized water. Quantitative determination was performed by the method of absolute calibration. The analytical ranges for aminoglycoside were 10–1000 ng/g. The relative standard deviation of the results of analysis did not exceed 0.17. The duration of the identification of aminoglycosides in milk was 15 min; the duration of the determination of the detected analytes was 30–40 min.