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葡萄酒、橄榄油和血浆中羟基酪醇的高效提取及灵敏的液相色谱-质谱定量分析

Efficient extraction and sensitive LC-MS quantification of hydroxytyrosol in wine, oil and plasma.

作者信息

Wang Shao-Ting, Le Juan, Peng Rui, Li Yan

机构信息

Department of Clinical Laboratory, Renmin Hospital of Wuhan University, Wuhan 430060, China.

Department of Clinical Laboratory, Renmin Hospital of Wuhan University, Wuhan 430060, China.

出版信息

Food Chem. 2020 Apr 15;323:126803. doi: 10.1016/j.foodchem.2020.126803.

Abstract

Hydroxytyrosol (HT) possesses significant biological activity. However, the methodologies for its quantification always suffered from low sensitivity, intricate treatment and high sample consumption. Here, we presented the very first attempt for specific extraction of HT through cis-diol recognition mechanism. By using easily prepared zirconia as dispersive solid phase extraction medium, HT from small amount of wine (10 μL), oil (20 mg) and plasma (100 μL) was efficiently purified within ten minutes. Coupled with LC-MS/MS analysis, the method limit of detection (LOD) could reach 1 ng/mL in wine, 0.5 μg/kg in oil and 0.1 ng/mL in plasma. Profited by this superior method, HT analysis was successfully performed in diverse wine and oil products as well as human plasma samples after intake of extra virgin olive oil. In addition, we further confirmed the endogenous HT was undetectable from routine human plasma even after upgrading the detection sensitivity through post isonicotinoyl chloride derivatization.

摘要

羟基酪醇(HT)具有显著的生物活性。然而,其定量方法一直存在灵敏度低、处理复杂和样品消耗量大的问题。在此,我们首次尝试通过顺式二醇识别机制对HT进行特异性提取。通过使用易于制备的氧化锆作为分散固相萃取介质,可在十分钟内从少量葡萄酒(10μL)、油(20mg)和血浆(100μL)中高效纯化出HT。结合液相色谱-串联质谱(LC-MS/MS)分析,该方法在葡萄酒中的检测限(LOD)可达1ng/mL,在油中为0.5μg/kg,在血浆中为0.1ng/mL。受益于这一卓越方法,在摄入特级初榨橄榄油后,成功对多种葡萄酒和油产品以及人体血浆样本进行了HT分析。此外,我们进一步证实,即使通过异烟酰氯衍生化提高检测灵敏度后,常规人体血浆中仍未检测到内源性HT。

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