Sensitive profiling of phenols, bile acids, sterols, and eicosanoids in mammalian urine by large volume direct injection-online solid phase extraction-ultra high performance liquid chromatography-polarity switching tandem mass spectrometry
Sensitive profiling of phenols, bile acids, sterols, and eicosanoids in mammalian urine by large volume direct injection-online solid phase extraction-ultra high performance liquid chromatography-polarity switching tandem mass spectrometry
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通过大体积直接进样-在线固相萃取-超高效液相色谱-极性转换串联质谱法对哺乳动物尿液中的酚类、胆汁酸、甾醇和类二十烷酸进行灵敏分析
DOI：
10.1039/c6ra13272c
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发表时间：
2016-08
期刊：
影响因子：
3.9
通讯作者：
Tu Pengfei
中科院分区：
文献类型：
--
作者：
Liu Yao;Song Qingqing;Zheng Jiao;Li Jun;Zhao Yunfang;Li Chun;Song Yuelin;Tu Pengfei
胆汁酸、甾醇和类二十烷酸是哺乳动物尿液中重要的化学物质，有时也是多种疾病的主要诊断标志物，而酚类物质通常来源于饮食，在酚类衍生物的药代动力学和代谢特征分析中通常被观察到是令人讨厌的干扰物。这些物质的精确分析普遍受到不稳定性和痕量分布的影响，以及繁琐的样品制备程序导致的误差和不确定性。本文采用大体积直接进样-在线固相萃取-超高效液相色谱-极性切换串联质谱法（LVDI-online SPE-UHPLC-psMS/MS），对哺乳动物尿液中的酚类、胆汁酸类、甾醇类和类花生酸类，特别是痕量类花生酸类进行了直接同时测定。通过连续10次进样，将大体积（500 μL）液态样品直接上样到在线SPE柱上。SPE柱负责在上样阶段（−4.5至5.0 min）积累目标组分，同时在洗脱阶段（5.0-27.0 min）将这些捕获的分析物传输至沃茨HSS T3柱中。使用电子6端口/2通道阀完成相位切换。使用阳性和阴性多反应监测模式对所有分析物（共28种）进行分析物检测。各种方法验证试验证明，开发的方法具有极高的灵敏度（大多数定量限低于0.3 ng mL−1）、精密度（日内和日间变化的所有RSD均低于15%）和准确度（回收率从80.4%升至120.0%，RSD低于20%）。来自不同物种的尿液样本以及来自同一组内不同个体的尿液基质之间存在显著差异。研究结果表明，LVDI-online SPE-UHPLC-psMS/MS方法具有检测痕量组分和保护易变性物质不被降解的优点，为生物流体中物质的广泛靶向监测提供了有意义的工具。
Bile acids, sterols, and eicosanoids serve as important chemical categories in mammalian urine and, sometimes, as primary diagnostic markers for diverse diseases, whereas phenols, usually derived from the diet, are usually observed as annoying interferents in pharmacokinetic and metabolic profiling of phenolic derivatives. Precise analysis of these substances widely suffers from instability and trace distributions, as well as errors and uncertainties resulting from tedious sample preparation procedures. Herein, directly simultaneous determination of phenols, bile acids, sterols, and eicosanoids, in particular those trace ones, in mammalian urinary matrices was attempted using large volume direct injection-online solid phase extraction-ultra high performance liquid chromatography-polarity switching tandem mass spectrometry (LVDI-online SPE-UHPLC-psMS/MS). Large volumes (500 μL) of liquid-state samples were directly loaded onto an online SPE column via ten consecutive injections. The SPE column was responsible for accumulating targeted components at the loading phase (−4.5 to 5.0 min), while transmitting those trapped analytes into a Waters HSS T3 column at the elution phase (5.0–27.0 min). Phase switching was accomplished using an electronic 6-port/2-channel valve. Analyte detection of all analytes, 28 ones in total, was performed using both positive and negative multiple reaction monitoring modes. Various method validation assays demonstrated the developed method to be extremely sensitive (most limits of quantitation lower than 0.3 ng mL−1), precise (all RSDs of intra- and inter-day variations lower than 15%) and accurate (recoveries ramped from 80.4% to 120.0% with RSDs lower than 20%). Significant variations occurred for urine samples from different species, as well as amongst urinary matrices from different individuals within the same group. The findings proved that the developed LVDI-online SPE-UHPLC-psMS/MS method takes advantage of detecting the trace components and preserving those mutable substances from degradation, thus offering a meaningful tool for widely targeted monitoring substances in biofluids.
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DOI：
10.1016/j.jchromb.2016.04.017
发表时间：
2016-06
期刊：
Journal of chromatography. B, Analytical technologies in the biomedical and life sciences
影响因子：
--
作者：
Tong Zhang;D. Watson
通讯作者：
Tong Zhang;D. Watson
影响因子：
1.8
作者：
J. Boccard;F. Badoud;Nicolas Jan;R. Nicoli;C. Schweizer;F. Pralong;J. Veuthey;N. Baume;S. Rudaz;M. Saugy
通讯作者：
J. Boccard;F. Badoud;Nicolas Jan;R. Nicoli;C. Schweizer;F. Pralong;J. Veuthey;N. Baume;S. Rudaz;M. Saugy
影响因子：
3.1
作者：
Du, Gang;Zhao, Haiyu;Wang, Yitao
通讯作者：
Wang, Yitao
影响因子：
1.7
作者：
Dan Bi;Xingyun Chai;Yuelin Song;Y. Lei;P. Tu
通讯作者：
Dan Bi;Xingyun Chai;Yuelin Song;Y. Lei;P. Tu
铁载体生物合成协调调节尿路致病性大肠杆菌和人尿液的毒力相关的相互作用代谢组
影响因子：
4.6
作者：
Su Q;Guan T;Lv H
通讯作者：
Lv H