A selective adsorption-based separation of low-mass molecules from biological samples towards high-throughput mass spectrometry analysis in a single drop of human whole blood
A selective adsorption-based separation of low-mass molecules from biological samples towards high-throughput mass spectrometry analysis in a single drop of human whole blood
复制标题
基于选择性吸附的生物样品中低质量分子的分离，用于单滴人体全血的高通量质谱分析
DOI：
10.1016/j.talanta.2019.05.005
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发表时间：
2019
期刊：
影响因子：
6.1
通讯作者：
Jiang Guibin
中科院分区：
文献类型：
--
作者：
Wang Jing;Liang Yong;Mao Yuxiang;Liu Qian;Jiang Guibin
本文合成了一种新型多功能吸附材料十八烷基改性有序介孔碳(C18-CMK-8)，并将其用于基质辅助激光解吸电离飞行时间质谱仪(MALDI-TOF MS)同时分析多种小分子物质。通过十八烷基三甲氧基硅烷与有序介孔碳CMK-8的一步化学键合，制备了C18-CMK-8。C18-CMK-8的纳米孔结构可以选择性地富集低质量分子，同时排除全血中大分子的干扰；同时，C18链可以极大地增强对广泛小分子的亲和力。然后，将C18-CMK-8固相萃取(SPE)与MALDI-TOF MS联用技术应用于单滴人全血样品中6种兴奋剂(氨苯蝶呤、曲宁诺酮、睾酮、甲基睾酮、克伦特罗和士的宁)的快速高通量筛选。该方法具有较高的分析灵敏度(检出限为0.0 5~0.1 ng m L−1)、良好的回收率(6 7.2%~114.3%)、最低进样量(∼2 0 μL)和较强的抗干扰能力。本研究具有高通量、快速、样品用量少、灵敏度高等显著优点，不仅为复杂样品的制备提供了一种通用的富集物，而且为微量全血分析提供了一种有前景的工具。
In this work, a newly designed multifunctional adsorbent material, octadecyl-modified ordered mesoporous carbon (C18-CMK-8), was synthesized and employed for simultaneous analysis of multiple small molecules by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS). The C18-CMK-8 was facilely prepared by one-step chemical binding of octadecyltrimethoxysilane to an ordered mesoporous carbon CMK-8. The nanosized pore structure of C18-CMK-8 can selectively enrich low-mass molecules while excluding interferences from large molecules in whole blood; meanwhile, the C18chain can greatly enhance the affinity for a wide range of small molecules. Then, the C18-CMK-8-based solid-phase extraction (SPE) combined with MALDI-TOF MS measurement was applied in rapid and high-throughput screening of six doping agents (triamterene, trenbolone, testosterone, methyltestosterone, clenbuterol, and strychnine)) in single-drop human whole blood samples. The method showed high analytical sensitivity (detection limit 0.05–0.1 ng mL−1), good recoveries (67.2–114.3%), minimal sample requirement (∼20 μL), and robust anti-interference ability. With distinct advantages such as high throughput, rapidness, minimal sample requirement, and high sensitivity, this study not only offers a versatile enrichment material for complex sample preparation, but also demonstrates a promising tool for minimal whole blood analysis.