Determination of Aminoglycosides Residues in Milk by Microwave-assisted Derivatization and Ionic Liquid-based Dispersive Liquid-liquid Microextraction Coupled with HPLC
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Abstract:
A new method based on simultaneous microwave-assisted derivatization and ionic liquid-based dispersive liquid-liquid microextraction was developed for the derivatization and extraction of aminoglycosides (AGs) including streptomycin (STR), gentamicin (GEN), kanamycin (KAN), tobramycin (TOB), micronomicin (MIC), amikacin (AMI) and neomycin (NEO) in milk samples. In the experiment, 9-fluorenylmethyl chloroformate (FMOC-Cl), 1-octyl-3- methylimidazolium hexafluorophosphate ([Omim]PF6) and methanol were used as derivatization reagent, extraction solvent and disperser, respectively. Aminoglycosides were simultaneously derivatized and extracted into ionic liquid phase by this method in a single step. Derivatives of the aminoglycosides were then determined by high-performance liquid chromatography coupled with fluorescence detection. The calibration curve had good linear relationship (r＞0.9989). The limits of detection (LODs) of analytes were in range of 0.11~0.57 μg/L. The recoveries were between 91.95% and 106.33% with the relative standard deviations of 1.39~5.92%. The proposed method has the advantages of simple operation, high sensitivity and reliable results and should be extensively applied for determination of aminoglycosides in milk samples.
