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

被引:4
|
作者
Liu, Huihui [1 ]
Ren, Chuanbo [1 ]
Han, Dianfeng [1 ]
Huang, Hui [1 ]
Zou, Rongjie [1 ]
Zhang, Huawei [1 ]
Xu, Yingjiang [1 ]
Gong, Xianghong [1 ]
Zhang, Xiuzhen [1 ]
Li, Yanshen [2 ]
机构
[1] Shandong Marine Resource & Environm Res Inst, Lab Restorat Marine Ecol, Yantai 264006, Peoples R China
[2] Yantai Univ, Coll Life Sci, Yantai 264005, Peoples R China
关键词
IN-VITRO; OLAQUINDOX; CARBADOX; GENOTOXICITY; QUINOCETONE; CHICKENS; LIVER; PHARMACOKINETICS; CYADOX; TISSUE;
D O I
10.1155/2018/2768047
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
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. 0 en, the processed samples were separated and monitored by UPLC-MS/MS. 0 is developed method has been validated according to FDA criteria. At fortified levels of 2, 10, and 20 mu g/kg, recoveries ranged from 82.5% to 93.5% with the intraday RSD less than 7.27% and interday RSD less than 11.8%. 0 The limit of detection (LOD) of all the three metabolites ranged from 0.21 to 0.48 mu g/kg, while the limit of quantification (LOQ) ranged from 0.79 to 1.59 mu g/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.
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页数:7
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