QuEChERS sample pre-processing with UPLC-MS/MS: A method for detecting 19 quinolone-based veterinary drugs in goat's
Siou Bang Ye1, Ying Huang2, Ding-Yan Lin3
1Chiayi County Health Bureau Laboratory Section, No. 3, E. Sec., Sianghe 2nd Rd., Taibao City, Chiayi County 61249, Taiwan, ROC; Institute of Food Safety Management, National Pingtung University of Science and Technology, 1, Shuefu Road, Neipu, Pingtung 912301, Taiwan, ROC.
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.
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