Article ID Journal Published Year Pages File Type
7609175 Journal of Chromatography A 2018 10 Pages PDF
Abstract
A multiclass method was proposed for the simultaneous determination of various classes of veterinary drugs (n = 65), mycotoxins and metabolites (n = 39) in egg and milk by ultra-high performance liquid chromatography-tandem mass spectrometry. The contaminants were extracted by QuEChERS-based strategy including salt-out partitioning and dispersive solid-phase extraction for cleanup further. With the aim of maximizing throughput and extraction efficiency, Plackett-Burman design was employed initially for screening significant variables. And response surface methodology based on central composite design was conducted to achieve optimal conditions in details: 3.35% (v/v) of formic acid in acetonitrile, 1.2 g of NaCl, 0.5 g of anhydrous NaAc, 300 mg of C18 and 140 mg of primary secondary amine. Satisfactory analytical characteristics in validation, in aspects of accuracy (70%-105% for mycotoxins and quinolones, 55%-80% for sulphonamides and 40%-105% for other veterinary drugs), precision (inter-day RSDs < 14%) and sensitivity (LOQs ranged from 0.01 μg/kg to 31 μg/kg), were achieved under the optimized conditions. The matrix effects were evaluated and compensated by the use of matrix-matched calibration curves (R2 > 0.987). In practice, 45 eggs and 30 milk samples were investigated by the established method, of which positive finding aflatoxin in milk and sterigmatocystin in eggs.
Related Topics
Physical Sciences and Engineering Chemistry Analytical Chemistry
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