QuEChERS sample pre-processing with UPLC-MS/MS: A method for detecting 19 quinolone-based veterinary drugs in goat's milk

Abstract

We develop and validate a method for the rapid determination and identification of 19 quinolones in goat's milk by combining the QuEChERS technique with ultra-performance liquid chromatography-tandem mass spectrometry. Plackett-Burman and Central Composite Design methods were used to select the parameters that best promote the extraction efficiency, which led to extraction with acetonitrile/5% formic acid, followed by phase separation with sodium citrate, disodium hydrogen citrate, Na₂SO₄, and NaCl as optimal. The supernatant was then extracted and cleaned by dispersive solid-phase extraction using C₁₈ and Na₂SO₄ aided by low-temperature clean-up. The method was validated, with limits of quantification (LOQs) of 5 ppb, specificities of 1/5 LOQ, linearities (R²) > 0.9853, recoveries of 73.4-114.2%, repeatabilities < 15.0%, and intermediate precisions < 13.6%. The developed method was suitable for the routine analysis of quinolone residues in goat's milk and was used to test 10 goat milk samples produced in Taiwan.

Keywords: Central composite design; Plackett–Burman; QuEChERS; Quinolones; UPLC–MS/MS; Validation.