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首页> 外文期刊>The Journal of automatic chemistry >UPLC-MS/MS Method for Simultaneous Determination of Three Major Metabolites of Mequindox in Holothurian
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UPLC-MS/MS Method for Simultaneous Determination of Three Major Metabolites of Mequindox in Holothurian

机译：UPLC-MS / MS方法同时测定全氟尿嘧啶中三种主要代谢产物

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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.
机译：这项研究开发了一种超高效液相色谱串联质谱（UPLC-MS / MS）方法，用于检测甲喹酮的三种主要代谢物，包括3-甲基-喹喔啉-2-羧酸，1-脱氧甲喹酮和1,4-双脱氧甲喹酮（MQCA，1-DMEQ和BDMEQ），采用整型。无需复杂的酶解步骤即可通过超声辅助酸解法简化目标分析物。之后，将每个样品离心并通过Oasis MAX柱纯化。然后，将处理后的样品分离并通过UPLC-MS / MS进行监测。此开发方法已根据FDA标准进行了验证。在强化水平分别为2、10和20？g / kg时，回收率在82.5％至93.5％之间，当日RSD小于7.27％，日间RSD小于11.8％。所有三种代谢物的检出限（LOD）范围为0.21至0.48？μg/ kg，而定量限（LOQ）的范围为0.79至1.59μg/ kg。应用于商业样品时，在20个样品中有14个被检测出对三种目标分析物呈阳性，阳性率为70％。结果表明，该方法具有特异性，灵敏性，适用于定量测定和定量构筑全人类的MEQ的三种主要代谢产物。

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