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

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 holothu...

Full description

Saved in:
Bibliographic Details
Main Authors: Huihui Liu, Chuanbo Ren, Dianfeng Han, Hui Huang, Rongjie Zou, Huawei Zhang, Yingjiang Xu, Xianghong Gong, Xiuzhen Zhang, Yanshen Li
Format: Article
Language:English
Published: Wiley 2018-01-01
Series:Journal of Analytical Methods in Chemistry
Online Access:http://dx.doi.org/10.1155/2018/2768047
Tags: Add Tag
No Tags, Be the first to tag this record!
_version_ 1850230592653754368
author Huihui Liu
Chuanbo Ren
Dianfeng Han
Hui Huang
Rongjie Zou
Huawei Zhang
Yingjiang Xu
Xianghong Gong
Xiuzhen Zhang
Yanshen Li
author_facet Huihui Liu
Chuanbo Ren
Dianfeng Han
Hui Huang
Rongjie Zou
Huawei Zhang
Yingjiang Xu
Xianghong Gong
Xiuzhen Zhang
Yanshen Li
author_sort Huihui Liu
collection DOAJ
description 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.
format Article
id doaj-art-1ec1ebbb61b343938fdea154577a26d3
institution OA Journals
issn 2090-8865
2090-8873
language English
publishDate 2018-01-01
publisher Wiley
record_format Article
series Journal of Analytical Methods in Chemistry
spelling doaj-art-1ec1ebbb61b343938fdea154577a26d32025-08-20T02:03:50ZengWileyJournal of Analytical Methods in Chemistry2090-88652090-88732018-01-01201810.1155/2018/27680472768047UPLC-MS/MS Method for Simultaneous Determination of Three Major Metabolites of Mequindox in HolothurianHuihui Liu0Chuanbo Ren1Dianfeng Han2Hui Huang3Rongjie Zou4Huawei Zhang5Yingjiang Xu6Xianghong Gong7Xiuzhen Zhang8Yanshen Li9Shandong Marine Resource and Environment Research Institute, Laboratory of Restoration for Marine Ecology, Yantai 264006, ChinaShandong Marine Resource and Environment Research Institute, Laboratory of Restoration for Marine Ecology, Yantai 264006, ChinaShandong Marine Resource and Environment Research Institute, Laboratory of Restoration for Marine Ecology, Yantai 264006, ChinaShandong Marine Resource and Environment Research Institute, Laboratory of Restoration for Marine Ecology, Yantai 264006, ChinaShandong Marine Resource and Environment Research Institute, Laboratory of Restoration for Marine Ecology, Yantai 264006, ChinaShandong Marine Resource and Environment Research Institute, Laboratory of Restoration for Marine Ecology, Yantai 264006, ChinaShandong Marine Resource and Environment Research Institute, Laboratory of Restoration for Marine Ecology, Yantai 264006, ChinaShandong Marine Resource and Environment Research Institute, Laboratory of Restoration for Marine Ecology, Yantai 264006, ChinaShandong Marine Resource and Environment Research Institute, Laboratory of Restoration for Marine Ecology, Yantai 264006, ChinaCollege of Life Science, Yantai University, Yantai 264005, ChinaThis 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.http://dx.doi.org/10.1155/2018/2768047
spellingShingle Huihui Liu
Chuanbo Ren
Dianfeng Han
Hui Huang
Rongjie Zou
Huawei Zhang
Yingjiang Xu
Xianghong Gong
Xiuzhen Zhang
Yanshen Li
UPLC-MS/MS Method for Simultaneous Determination of Three Major Metabolites of Mequindox in Holothurian
Journal of Analytical Methods in Chemistry
title UPLC-MS/MS Method for Simultaneous Determination of Three Major Metabolites of Mequindox in Holothurian
title_full UPLC-MS/MS Method for Simultaneous Determination of Three Major Metabolites of Mequindox in Holothurian
title_fullStr UPLC-MS/MS Method for Simultaneous Determination of Three Major Metabolites of Mequindox in Holothurian
title_full_unstemmed UPLC-MS/MS Method for Simultaneous Determination of Three Major Metabolites of Mequindox in Holothurian
title_short UPLC-MS/MS Method for Simultaneous Determination of Three Major Metabolites of Mequindox in Holothurian
title_sort uplc ms ms method for simultaneous determination of three major metabolites of mequindox in holothurian
url http://dx.doi.org/10.1155/2018/2768047
work_keys_str_mv AT huihuiliu uplcmsmsmethodforsimultaneousdeterminationofthreemajormetabolitesofmequindoxinholothurian
AT chuanboren uplcmsmsmethodforsimultaneousdeterminationofthreemajormetabolitesofmequindoxinholothurian
AT dianfenghan uplcmsmsmethodforsimultaneousdeterminationofthreemajormetabolitesofmequindoxinholothurian
AT huihuang uplcmsmsmethodforsimultaneousdeterminationofthreemajormetabolitesofmequindoxinholothurian
AT rongjiezou uplcmsmsmethodforsimultaneousdeterminationofthreemajormetabolitesofmequindoxinholothurian
AT huaweizhang uplcmsmsmethodforsimultaneousdeterminationofthreemajormetabolitesofmequindoxinholothurian
AT yingjiangxu uplcmsmsmethodforsimultaneousdeterminationofthreemajormetabolitesofmequindoxinholothurian
AT xianghonggong uplcmsmsmethodforsimultaneousdeterminationofthreemajormetabolitesofmequindoxinholothurian
AT xiuzhenzhang uplcmsmsmethodforsimultaneousdeterminationofthreemajormetabolitesofmequindoxinholothurian
AT yanshenli uplcmsmsmethodforsimultaneousdeterminationofthreemajormetabolitesofmequindoxinholothurian