Simultaneous determination of 3,3′,4′,5,7-pentamethylquercetin and its possible metabolite 3,3′,4′,7-tetramethylquercetin in dog plasma by liquid chromatography-tandem mass spectrometry and its application to preclinical pharmacokinetic study
Simultaneous determination of 3,3′,4′,5,7-pentamethylquercetin and its possible metabolite 3,3′,4′,7-tetramethylquercetin in dog plasma by liquid chromatography-tandem mass spectrometry and its application to preclinical pharmacokinetic study
复制标题
DOI：
10.1016/j.jchromb.2011.06.019
复制
发表时间：
2011-08-01
影响因子：
3
通讯作者：
Zheng, Heng
中科院分区：
文献类型：
--
作者：
Chen, Xiaomei;Li, Dongyan;Zheng, Heng
建立了以4 '，5，7-三甲基芹菜素（TMA）为内标物，同时测定犬血浆中3，3'，4 '，5，7-五甲基槲皮素（PMQ）及其代谢物3，3'，4 '，7-四甲基槲皮素（TMQ）的超快速液相色谱-电喷雾串联质谱（UFLC-ESI-MS/MS）方法。用乙腈预处理血浆样品以进行蛋白沉淀，并在Ultimate XB-CN色谱柱（5 μ m，2.1 mm x 150 mm）上分离分析物，移动的流动相由乙腈和水（2：1，v/v）组成。在三重四极杆串联质谱仪上在正多反应监测模式（MRM）下进行检测。质量跃迁离子对如下：PMQ的m/z 373.1-312.1; TMQ的m/z 359.1-344.0; TMA的m/z 313.1-298.1。PMQ的验证浓度范围为1.272 - 3060 ng/mL，TMQ的验证浓度范围为10.35 - 1725 ng/mL。PMQ和TMQ的定量下限分别为1.272 ng/mL和10.35 ng/mL。该方法已成功应用于PMQ及其代谢产物TMQ在犬体内的药代动力学研究。(C)2011 Elsevier BY. All rights reserved.
A sensitive, simple and rapid ultra fast liquid chromatography (UFLC)-ESI-MS/MS method was established for the simultaneous determination of 3,3',4',5,7-pentamethylquercetin (PMQ) and its possible metabolite 3,3',4',7-tetramethylquercetin (TMQ) in dog plasma using 4',5,7-trimethylapigenin (TMA) as the internal standard. The plasma sample was pretreated with acetonitrile for protein precipitation and the analytes were separated on an Ultimate XB-CN column (5 mu m, 2.1 mm x 150 mm) with the mobile phase consisting of acetonitrile and water (2:1, v/v). Detection was performed on a triple-quadrupole tandem mass spectrometer under a positive multiple reaction-monitoring mode (MRM). The mass transition ion-pair was followed as m/z 373.1-312.1 for PMQ 359.1-344.0 for TMQ and 313.1-298.1 for TMA. The validated concentration ranged from 1.272 to 3060 ng/mL for PMQ and from 10.35 to 1725 ng/mL for TMQ. The lower limit of quantifications for PMQ and TMQ were 1.272 ng/mL and 10.35 ng/mL, respectively. The developed-method was successfully applied for the pharmacokinetic study of PMQ and its metabolite TMQ in dogs following a single oral dose. (C) 2011 Elsevier BY. All rights reserved.