Development and validation of a solid‐phase extraction method coupled with LC–MS/MS for the simultaneous determination of 16 antibiotic residues in duck meat

• Published in: Biomedical chromatography 2019-05, Vol.33 (5), p.e4501-n/a
• Main Authors: Zheng, Weijia, Abd El‐Aty, A. M., Kim, Seong‐Kwan, Choi, Jeong‐Min, Park, Da‐Hee, Yoo, Kyung‐Hee, Kang, Young‐Sun, Jeon, Jong‐Sup, Hacımüftüoğlu, Ahmet, Shim, Jae‐Han, Shin, Ho‐Chul
• Format: Article
• Language: English
• Subjects: analysis; antibiotics; duck meat; LC–MS/MS; residues; solid‐phase extraction
• ISSN: 0269-3879; 1099-0801
• DOI: 10.1002/bmc.4501

The present study was carried out to determine 16 antibiotics belonging to seven different groups (tetracyclines, sulfonamides, penicillins, fluoroquinolones, macrolides, lincosamides and trimethoprims) in duck meat. A solid‐phase extraction method based on Oasis HLB cartridges coupled with liquid chromatography–electrospray ionization tandem mass spectrometry was developed. Solutions of 0.1 m ethylenediaminetetraacetic acid disodium salt and 2% trifluoroacetic acid were used for the preliminary extraction of the target antibiotics from duck meat and n‐hexane was used for purification prior to solid‐phase extraction. Mobile phases composed of 0.1% trifluoroacetic acid in distilled water (solvent A) and 0.1% trifluoroacetic acid in methanol (solvent B), combined with a reversed‐phase C18 analytical column, provided the optimal separation and signal intensity. The linearity of the method was assessed using six concentrations (5, 10, 20, 30, 40, and 50 μg/kg), and the recoveries, which were calculated at three spiking concentrations (5, 10 and 20 μg/kg), were in the range 69.8–103.3% with relative standard deviations (RSDs) ≤ 6.9% for the 16 tested antibiotics. Matrix effects ranging from −47.2 to −13.5% were observed for all the analytes, and the limits of quantitation (LOQ), which ranged from 4.93 to 26.21 μg/kg, were much lower than the maximum residue limits (MRLs) set by various regulatory authorities. Ten samples from a market were tested, and none of the target analytes were detected. Thus, a simple and versatile protocol has been developed to detect and quantify 16 antibiotics in duck meat samples.