Development and validation of a high-throughput micro solid-phase extraction method coupled with ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry for rapid identification and quantification of phenolic metabolites in human plasma and urine
Development and validation of a high-throughput micro solid-phase extraction method coupled with ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry for rapid identification and quantification of phenolic metabolites in human plasma and urine
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DOI：
10.1016/j.chroma.2016.08.027
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发表时间：
2016-09-16
影响因子：
4.1
通讯作者：
Rodriguez-Mateos, Ana
中科院分区：
文献类型：
--
作者：
Feliciano, Rodrigo P.;Mecha, Elsa;Rodriguez-Mateos, Ana
优化并验证了一种快速、高通量的微固相萃取（mu-SPE）-超高效液相色谱-四极杆飞行时间质谱（UHPLC Q-TOF MS）联用方法，用于使用真实标准品定量测定人血浆和尿液中的67种多酚代谢物。在专属性、线性、方法检测限（MDL）、方法定量限（MQL）、重复性、日内和日间精密度、准确度和基质效应方面对该方法进行了充分验证。该方法被证明具有专属性，结果显示所有化合物的响应呈线性，血浆中的MDL范围为0.04 nM至86 nM，尿液中的MDL范围为0.01 nM至136 nM。血浆中的MQL范围为0.14 nM至286 nM，尿液中的MQL范围为0.03 nM至465 nM。血浆和尿液中的重复性分别为1.7%和9.2%，2.2%和10.4%。血浆和尿液中的中位精密度值分别为8.7%和11.5%（日内）以及10.8%和10.0%（日间）。两种生物基质中的中位回收率均为89%。测定基质效应，血浆和尿液中的中位值分别为-1.2%和-6.8%。方法验证后，49和57种化合物，包括第二阶段和肠道微生物代谢产物，分别在血浆和尿液中定量，蔓越莓汁消费后。这种方法可以应用于大规模的人类饮食干预试验，允许高样品通量。(C)2016由Elsevier B. V.出版
A rapid and high-throughput micro-solid phase extraction (mu-SPE) method coupled with ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC Q-TOF MS) analysis was optimized and validated for the quantification of 67 (poly)phenol metabolites in human plasma and urine using authentic standards. The method was fully validated in terms of specificity, linearity, method detection limit (MDL), method quantification limit (MQL), repeatability, intra- and inter-day precision, accuracy and matrix effects. The method proved to be specific and results showed linearity of responses for all compounds, with MDL ranging between 0.04 nM and 86 nM in plasma and between 0.01 nM and 136 nM in urine. MQL ranged between 0.14 nM and 286 nM in plasma and between 0.03 nM and 465 nM in urine. Repeatability varied between 1.7 and 9.2% in plasma and between 2.2% and 10.4% in urine. Median precision values of 8.7 and 11.5% (intra-day), and 10.8% and 10.0% (inter-day) were obtained in plasma and urine, respectively. The median recovery was 89% in both biological matrices. Matrix effects were determined and median values of -1.2% and -6.8% in plasma and urine were obtained. After method validation, 49 and 57 compounds, including phase II and gut microbial metabolites, were quantified in plasma and urine, respectively, following cranberry juice consumption. This methodology can be applied to large-scale human dietary intervention trials allowing for high sample throughput. (C) 2016 Published by Elsevier B.V.