PMID- 28941404 OWN - NLM STAT- MEDLINE DCOM- 20171030 LR - 20171030 IS - 1873-376X (Electronic) IS - 1570-0232 (Linking) VI - 1065-1066 DP - 2017 Oct 15 TI - Development of a simple multi-residue determination method of 80 veterinary drugs in Oplegnathus punctatus by liquid chromatography coupled to quadrupole Orbitrap mass spectrometry. PG - 20-28 LID - S1570-0232(17)31272-2 [pii] LID - 10.1016/j.jchromb.2017.09.013 [doi] AB - A simple, rapid and sensitive multi-residue analytical method was developed and validated for 80 veterinary drugs in Oplegnathus punctatus using ultrahigh performance liquid chromatography-Orbitrap high resolution mass spectrometry (LC-HRMS). The analytes belong to 12 different families include benzimidazoles, beta-lactams, lincosamides, macrolides, nitromidazoles, quinolones, sulfonamides and trimethoprim, tetracyclines, triphenylmethane dyes, amphenicols, nonsteroidal estrogens and steroid hormones. The sample preparation was optimized base on QuEChERS (quick, easy, cheap, effective, rugged and safe) procedure. A very simple and sufficient preparation procedure without salting-out and complex clean-up process was studied. It had been proved that water in the extract was helpful for extracting hydrophilic compounds and precipitating the lipids during the subsequent cleaning process. In addition, an appropriate percent of methanol was necessary to some analytes. Finally, a mixture of acetonitrile, methanol and water (3:1:1, v/v/v) which include 1% acetic acid and 10mM ethylenediaminetetraacetic acid disodium salt 2-hydrate was selected as the extraction solvent, and the clean-up step consisted of a low temperature procedure and two times of high-speed centrifugation to deproteinize and remove lipids. The detection and quantification of all compounds were performed by ultrahigh performance liquid chromatography coupled with electrospray ionization quadrupole Orbitrap high resolution mass spectrometry in positive and negative ion mode. This methodology was validated according to the Commission Decision 2002/657/EC and SANTE/11945/2015. The recoveries ranged from 60.74%-109.85% with relative standard deviations (RSDs)<20%. The limits of quantification (LOQs) were 0.25-25ug/kg, for the analytes which the MRL or MRPL had been established in fish tissue, the LOQs were all lower than their own legal tolerances. The values of decision limit (CCalpha) and detection capability (CCbeta) were in the range of 1.91-1001.13ug/kg and 3.52-1002.26ug/kg, respectively. This validated method has been successfully applied on the determination of veterinary drugs in real commercial oplegnathus punctatus samples. CI - Copyright (c) 2017 Elsevier B.V. All rights reserved. FAU - Zhao, Fei AU - Zhao F AD - College of Food Science and Engineering, Ocean University of China, 5 Yushan Road, Qingdao 266003, China; Shandong Entry-Exit Inspection and Quarantine Bureau, 70 Qutangxia Road, Qingdao 266002, China. FAU - Gao, Xin AU - Gao X AD - College of Food Science and Engineering, Ocean University of China, 5 Yushan Road, Qingdao 266003, China. Electronic address: xingao@ouc.edu.cn. FAU - Tang, Zhixu AU - Tang Z AD - Shandong Entry-Exit Inspection and Quarantine Bureau, 70 Qutangxia Road, Qingdao 266002, China. Electronic address: zhixutang@126.com. FAU - Luo, Xin AU - Luo X AD - Shandong Entry-Exit Inspection and Quarantine Bureau, 70 Qutangxia Road, Qingdao 266002, China. FAU - Wu, Miaomiao AU - Wu M AD - College of Food Science and Engineering, Ocean University of China, 5 Yushan Road, Qingdao 266003, China. FAU - Xu, Jiachao AU - Xu J AD - College of Food Science and Engineering, Ocean University of China, 5 Yushan Road, Qingdao 266003, China. FAU - Fu, Xiaoting AU - Fu X AD - College of Food Science and Engineering, Ocean University of China, 5 Yushan Road, Qingdao 266003, China. LA - eng PT - Journal Article DEP - 20170918 PL - Netherlands TA - J Chromatogr B Analyt Technol Biomed Life Sci JT - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JID - 101139554 RN - 0 (Veterinary Drugs) SB - IM MH - Animals MH - Chromatography, High Pressure Liquid/*methods MH - *Fishes MH - Limit of Detection MH - Linear Models MH - Mass Spectrometry/*methods MH - Reproducibility of Results MH - Seafood/*analysis MH - Veterinary Drugs/*analysis/isolation & purification OTO - NOTNLM OT - Extraction optimization OT - Fish tissues OT - Multi-residue OT - Orbitrap OT - Veterinary drugs EDAT- 2017/09/25 06:00 MHDA- 2017/10/31 06:00 CRDT- 2017/09/24 06:00 PHST- 2017/07/24 00:00 [received] PHST- 2017/09/01 00:00 [revised] PHST- 2017/09/07 00:00 [accepted] PHST- 2017/09/25 06:00 [pubmed] PHST- 2017/10/31 06:00 [medline] PHST- 2017/09/24 06:00 [entrez] AID - S1570-0232(17)31272-2 [pii] AID - 10.1016/j.jchromb.2017.09.013 [doi] PST - ppublish SO - J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Oct 15;1065-1066:20-28. doi: 10.1016/j.jchromb.2017.09.013. Epub 2017 Sep 18.