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将薄层色谱与振动冷却基质辅助激光解吸/电离傅里叶变换质谱联用用于神经节苷脂混合物的分析。

Coupling thin-layer chromatography with vibrational cooling matrix-assisted laser desorption/ionization Fourier transform mass spectrometry for the analysis of ganglioside mixtures.

作者信息

Ivleva Vera B, Elkin Yuri N, Budnik Bogdan A, Moyer Susanne C, O'Connor Peter B, Costello Catherine E

机构信息

Mass Spectrometry Resource, Cardiovascular Proteomics Center, and Department of Biochemistry, Boston University School of Medicine, 715 Albany Street R-806, Boston, Massachusetts 02118-2526, USA.

出版信息

Anal Chem. 2004 Nov 1;76(21):6484-91. doi: 10.1021/ac0491556.

DOI:10.1021/ac0491556
PMID:15516145
Abstract

Thin-layer chromatography (TLC), which is widely used for separation of glycolipids, oligosaccharides, lipids, and compounds of environmental and pharmaceutical interest, can be readily coupled to matrix-assisted laser desorption/ionization (MALDI) time-of-flight mass spectrometers, but this arrangement usually compromises mass spectral resolution due to the irregularity of the TLC surface. However, TLC can be coupled to an external ion source MALDI-Fourier transform (FT) MS instrument without compromising mass accuracy and resolution of the spectra. Furthermore, when the FTMS has a vibrationally cooled MALDI ion source, fragile glycolipids can be desorbed from TLC plates without fragmentation, even to the point that desorption of intact molecules from "hot"matrixes such as alpha-cyano-4-hydroxycinnamic acid is possible. In this work, whole brain gangliosides are separated using TLC; the TLC plates are attached directly to the MALDI target, where the gangliosides are desorbed, ionized, and detected in the FTMS with >70 000 resolving power.

摘要

薄层色谱法(TLC)广泛用于分离糖脂、寡糖、脂质以及环境和制药领域感兴趣的化合物,它可以很容易地与基质辅助激光解吸/电离(MALDI)飞行时间质谱仪联用,但由于TLC表面的不规则性,这种联用方式通常会影响质谱分辨率。然而,TLC可以与外部离子源MALDI-傅里叶变换(FT)质谱仪联用,而不会影响质谱的准确性和分辨率。此外,当傅里叶变换质谱仪具有振动冷却的MALDI离子源时,脆弱的糖脂可以从TLC板上解吸而不发生碎片化,甚至可以从诸如α-氰基-4-羟基肉桂酸等“热”基质上解吸出完整分子。在这项工作中,使用TLC分离全脑神经节苷脂;将TLC板直接连接到MALDI靶上,在那里神经节苷脂被解吸、电离,并在分辨率大于70000的傅里叶变换质谱仪中进行检测。

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