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Journal of Analytical Methods in Chemistry
Volume 2018, Article ID 2768047, 7 pages
https://doi.org/10.1155/2018/2768047
Research Article

UPLC-MS/MS Method for Simultaneous Determination of Three Major Metabolites of Mequindox in Holothurian

1Shandong Marine Resource and Environment Research Institute, Laboratory of Restoration for Marine Ecology, Yantai 264006, China
2College of Life Science, Yantai University, Yantai 264005, China

Correspondence should be addressed to Xiuzhen Zhang; moc.621@1055350zxz and Yanshen Li; moc.361@iapgnawnahziy

Received 11 October 2017; Accepted 10 January 2018; Published 1 April 2018

Academic Editor: Josep Esteve-Romero

Copyright © 2018 Huihui Liu et al. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

Abstract

This study developed an ultraperformance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method for the detection of three major metabolites of mequindox, including 3-methyl-quinoxaline-2-carboxylic acid, 1-desoxymequindox, and 1,4-bisdesoxymequindox (MQCA, 1-DMEQ, and BDMEQ), in holothurian. Target analytes were simplified with ultrasound-assisted acidolysis extracted without complicated enzymolysis steps. After that, each sample was centrifuged and purified by an Oasis MAX cartridge. Then, the processed samples were separated and monitored by UPLC-MS/MS. This developed method has been validated according to FDA criteria. At fortified levels of 2, 10, and 20 μg/kg, recoveries ranged from 82.5% to 93.5% with the intraday RSD less than 7.27% and interday RSD less than 11.8%. The limit of detection (LOD) of all the three metabolites ranged from 0.21 to 0.48 μg/kg, while the limit of quantification (LOQ) ranged from 0.79 to 1.59 μg/kg. On application to commercial samples, 14 of 20 samples were detected positive for the three target analytes, with positive rate at 70 percentage. The result indicated that this method was specific, sensitive, and suitable for the quantification and conformation of the three major metabolites of MEQ in holothurian.