High-Throughput Determination of 30 Veterinary Drug Residues in Milk Powder by Dispersive Solid-Phase Extraction Coupled
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High-Throughput Determination of 30 Veterinary Drug Residues in Milk Powder by Dispersive Solid-Phase Extraction Coupled with Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry Ruijiao Li 1 & Moucheng Wu 1
Received: 29 March 2017 / Accepted: 14 May 2017 # Springer Science+Business Media New York 2017
Abstract A high-throughput method was established for the simultaneous determination of 30 β-agonists, fluoroquinolones, and cephalosporins in milk powder by dispersive solid-phase extraction (dSPE) and ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Samples were firstly dissolved in sodium acetate buffer, then extracted with formic acid-acetonitrile, and subsequently purified by dSPE. Thirty target analytes were separated on a C18 column by gradient elution, detected through electrospray ionization (ESI) source in the positive mode with multi-reaction monitoring (MRM) conditions. The developed method was validated in terms of linearity, accuracy, and precision. Results indicated that 30 target analytes displayed excellent linearity in their corresponding concentration ranges and that their correlation coefficients were all higher than 0.995. The limits of quantitation (LOQs) for these targets were in the range of 0.7–7.0 μg/kg. The mean recoveries for negative sample spiked at three concentration levels were calculated between 80.0 and 97.5% with the relative standard deviation (RSD, n = 6) values ranging from 2.8 to 10.8%. In addition, the inter-day precision (n = 5) of the second spiked concentration was less than 13% (4.4–12.4%). The established and validated method is accurate and rapid and suitable for the high-throughput analysis of β-agonist, fluoroquinolone, and cephalosporin multiresidues in milk powder.
* Ruijiao Li [email protected] * Moucheng Wu [email protected] 1
College of Food Science and Technology, Huazhong Agricultural University, Wuhan 430070, China
Keywords Veterinary drug residues . β-agonists . Fluoroquinolones . Cephalosporins . UPLC-MS/MS . Dispersive solid-phase extraction (dSPE)
Introduction Veterinary drugs are commonly used at therapeutic levels in livestock breeding for disease resistance and growth promotion (Chen et al. 2016; Dasenaki and Thomaidis 2015). The widespread use of drugs in animal husbandry may result in the presence of drug residues in animalderived foods as one of the key issues for food safety, which has aroused great public concern. As a consequence of the veterinary drug residues in food, the human health is highly threatened (Mauro et al. 2014; Rico and Van den Brink 2014). Therefore, sensitive and reliable analytical methods to determine the veterinary drug and pharmaceutical residues in animal’s original food are extremely needed to ensure consumers’ safety. The analytical methods of β-agonist (Chu, Zheng, Qu, Geng, and Kang 2017; Wang, Liu, Su, and Zhu 2015), fluoroquinolone (Aufartová, Brabcová, Torres-Padrón, Solich, Sosa-Ferrera, and Santana-Rodríguez 2017; de Oliveira et al. 2016; Denadai and Ca
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