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使用电喷雾辅助激光解吸/电离质谱法对在薄层色谱板上分离的有机化合物进行表征。

Using electrospray-assisted laser desorption/ionization mass spectrometry to characterize organic compounds separated on thin-layer chromatography plates.

作者信息

Lin Shu-Yao, Huang Min-Zong, Chang Hui-Chiu, Shiea Jentaie

机构信息

Department of Chemistry, National Sun Yat-Sen University, Kaohsiung, 80424, Taiwan.

出版信息

Anal Chem. 2007 Nov 15;79(22):8789-95. doi: 10.1021/ac070590k. Epub 2007 Oct 12.

Abstract

Electrospray-assisted laser desorption/ionization (ELDI), an ionization method that combines laser desorption and electrospray ionization (ESI), can be used under ambient conditions to characterize organic compounds (including FD&C dyes, amines, extracts of a drug tablet) separated in the central track on a thin-layer chromatography (TLC) plate coated with either reversed-phase C18 particles or normal-phase silica gel. After drying, the TLC plate was placed on an acrylic sample holder set in front of the sampling skimmer of an ion trap mass analyzer. The chemicals at the center of the TLC plate were analyzed by pushing the sample holder into the path of a laser beam with a syringe pump. The molecules in the sample spot were desorbed by continuously irradiating the surface of the TLC plate with a pulsed nitrogen laser. Then, the desorbed sample molecules entered an ESI plume where they were ionized through the reactions with the charged species (including protons, hydronium ions and their cluster ions, solvent ions, and charged droplets) generated by electrospraying a methanol/water solution. MS/MS analyses were also performed to further characterize the analytes. The detection limit of TLC/ELDI/MS is approximately 10(-6) M. This was evaluated by using FD&C red dye as the standard. A linear relationship was found for the calibration curve with the concentration of FD&C red dye ranged from 10(-3) to 10(-6) M.

摘要

电喷雾辅助激光解吸/电离(ELDI)是一种将激光解吸与电喷雾电离(ESI)相结合的电离方法,可在环境条件下用于表征在涂有反相C18颗粒或正相硅胶的薄层色谱(TLC)板中央通道中分离的有机化合物(包括FD&C染料、胺类、药物片剂提取物)。干燥后,将TLC板放置在离子阱质量分析仪采样撇油器前方设置的丙烯酸样品架上。通过用注射泵将样品架推到激光束路径中,对TLC板中心的化学物质进行分析。通过用脉冲氮激光连续照射TLC板表面,使样品斑点中的分子解吸。然后,解吸的样品分子进入ESI羽流,在那里它们通过与电喷雾甲醇/水溶液产生的带电物种(包括质子、水合氢离子及其簇离子、溶剂离子和带电液滴)反应而被电离。还进行了串联质谱(MS/MS)分析以进一步表征分析物。TLC/ELDI/MS的检测限约为10^(-6) M。这是通过使用FD&C红色染料作为标准进行评估的。发现校准曲线在FD&C红色染料浓度范围为10^(-3)至10^(-6) M时呈线性关系。

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