Microextraction of tigecycline using deep eutectic solvents and its determination in milk by LC-MS/MS method

Abstract

The occurrence of tigecycline (TGC), a new first glycylcycline antibiotic residues in food products harmfully influences potential human consumers health. Therefore, analysts are forced to develop new microextraction methods connected with modern extractants for effective isolation of this compound. For this purpose, deep eutectic solvents (DES) as the extraction media were used. Liquid−liquid microextraction (LLME) of tigecycline from milk samples with application of the hydrophobic deep eutectic solvents: decanoic acid:thymol (1:1), thymol:camphor (2:1), dodecanoic acid:menthol (2:1), and dodecanoic acid:dodecanol (1:1) was developed. The studied samples were subjected to a deproteinization process using trichloroacetic acid solution and acetonitrile. The optimal microextraction parameters, molar ratio of DES components, amount of extraction solvents, pH of milk sample, shaking, and centrifugation time, were chosen. Tigecycline in the obtained microextracts of deep eutectic solvents was analyzed using a liquid chromatographic technique connected with a tandem mass spectrometry (LC-MS/MS) system. The limits of detection and quantification values for TGC determination followed by DES-LLME-LC-MS/MS method were in the 1.8 × 10−11 mol L−1 (0.01 μg kg−1) to 4.0 × 10−9 mol L−1 (2.28 μg kg−1) and 5.5 × 10−11 mol L−1 (0.03 μg kg−1) to 1.2 × 10−8 mol L−1 (6.84 μg kg−1) ranges, respectively. The RSD values of precision were in the range 1.4−7.8% (intraday) and 5.4−11.7% (interday). The developed procedures were used for the determination of tigecycline in different bovine milk samples.