Food Technology Department, Agrotecnio Center, Escola Tècnica Superior d'Enginyeria Agrària, University of Lleida, Avda. Alcalde Rovira Roure 191, 25198 Lleida, Spain.
Department of Medicine, Facultat de Medicina, University of Lleida, Avda/Alcalde Rovira Roure 80, 25198 Lleida, Spain.
Talanta. 2016 Oct 1;159:189-193. doi: 10.1016/j.talanta.2016.06.025. Epub 2016 Jun 15.
In this study, a fast and simple blood sampling and sample pre-treatment method based on the use of the dried blood spot (DBS) cards and ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) for the quantification of olive oil phenolic metabolites in human blood was developed and validated. After validation, the method was applied to determine hydroxytyrosol metabolites in human blood samples after the acute intake of an olive oil phenolic extract. Using the FTA DMPK-A DBS card under optimum conditions, with 20µL as the blood solution volume, 100µL of methanol/Milli-Q water (50/50, v/v) as the extraction solvent and 7 disks punched out from the card, the main hydroxytyrosol metabolites (hydroxytyrosol-3-O-sulphate and hydroxytyrosol acetate sulphate) were identified and quantified. The developed methodology allowed detecting and quantifying the generated metabolites at low μM levels. The proposed method is a significant improvement over existing methods to determine phenolic metabolites circulating in blood and plasma samples, thus making blood sampling possible with the volunteer pricking their own finger, and the subsequent storage of the blood in the DBS cards prior to chromatographic analysis.
在这项研究中,开发并验证了一种基于使用干血斑 (DBS) 卡和超高效液相色谱-串联质谱 (UPLC-MS/MS) 的快速简便的血液采样和样品预处理方法,用于定量人血中的橄榄油酚代谢物。验证后,该方法应用于测定橄榄油酚提取物急性摄入后人体血液样本中羟基酪醇的代谢物。在最佳条件下使用 FTA DMPK-A DBS 卡,以 20μL 作为血液溶液体积,以 100μL 甲醇/ Milli-Q 水 (50/50,v/v) 作为提取溶剂,并从卡上冲出 7 个圆盘,鉴定并定量了主要的羟基酪醇代谢物(羟基酪醇-3-O-硫酸盐和羟基酪醇乙酸硫酸盐)。所开发的方法能够在低 μM 水平检测和定量生成的代谢物。与现有的用于测定循环在血液和血浆样品中的酚类代谢物的方法相比,该方法有了显著的改进,因此可以通过志愿者刺破自己的手指进行血液采样,然后将血液储存在 DBS 卡中,再进行色谱分析。