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Simultaneous Determination of Fucoxanthin and Its Deacetylated Metabolite Fucoxanthinol in Rat Plasma by Liquid Chromatography-Tandem Mass Spectrometry

机译:液相色谱-串联质谱法同时测定大鼠血浆中的岩藻黄质及其脱乙酰基代谢产物岩藻黄质

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摘要

Fucoxanthin and its deacetylated metabolite fucoxanthinol are two major carotenoids that have been confirmed to possess various pharmacological properties. In the present study, fucoxanthinol was identified as the deacetylated metabolite of fucoxanthin, after intravenous (i.v.) and intragastric gavage (i.g.) administration to rats at doses of 2 and 65 mg/kg, respectively, by liquid chromatography-tandem mass spectrometric (LC-MS/MS) analysis. Next, an accurate and precise LC-MS/MS method was developed to quantitatively determine fucoxanthin and fucoxanthinol in rat plasma. Plasma samples were resolved by LC-MS/MS on a reverse-phase SB-C18 column that was equilibrated and eluted with acetonitrile (A)/aqueous 0.1% formic acid (B; 92/8, v/v) at a flow rate of 0.5 mL/min. Analytes were monitored by multiple-reaction monitoring (MRM) under positive electrospray ionization mode. The precursor/product transitions (m/z) were 659.3→109.0 for fucoxanthin, 617.2→109.0 for fucoxanthinol, and 429.4→313.2 for the internal standard (IS). Calibration curves for fucoxanthin and fucoxanthinol were linear over concentrations ranging from 1.53 to 720 and 1.17 to 600 ng/mL, respectively. The inter- and intraday accuracy and precision were within ±15%. The method was applied successfully in a pharmacokinetic study and the resulting oral fucoxanthin bioavailability calculated.
机译:岩藻黄质及其脱乙酰基代谢产物岩藻黄质是两个主要的类胡萝卜素,已被证实具有多种药理特性。在本研究中,通过液相色谱-串联质谱法(LC)分别以2 mg和65 mg / kg的剂量向大鼠静脉内(iv)和胃内灌胃(ig)给予大鼠后,岩藻黄质被鉴定为岩藻黄质的去乙酰化代谢产物-MS / MS)分析。接下来,开发了一种精确准确的LC-MS / MS方法来定量测定大鼠血浆中的岩藻黄质和岩藻黄质。血浆样品通过LC-MS / MS在反相SB-C18色谱柱上进行分离,该色谱柱用乙腈(A)/0.1%甲酸水溶液(B; 92/8,v / v)平衡并以流速洗脱0.5 mL / min。在正电喷雾电离模式下,通过多重反应监测(MRM)监测分析物。岩藻黄质的前体/产物跃迁(m / z)为659.3→109.0,岩藻黄质为617.2→109.0,内标(IS)为429.4→313.2。岩藻黄质和岩藻黄质的校准曲线在浓度分别为1.53至720和1.17至600 ng / mL时呈线性。日间和日内准确性和精确度均在±15%以内。该方法已成功地用于药代动力学研究,并计算了所得的口服岩藻黄质生物利用度。

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