Yamagaki Tohru, Suzuki Hiroaki, Tachibana Kazuo
Department of Chemistry, School of Science, The University of Tokyo, Tokyo, Japan.
J Am Soc Mass Spectrom. 2007 Apr;18(4):714-23. doi: 10.1016/j.jasms.2006.12.003. Epub 2007 Jan 22.
Ammonium chloride (NH4Cl) with a beta-carboline harmine (7-methoxy-1-methyl-9H-pyrido[3,4-b]indole) Matrix promotes the generation of chloride-anionized molecules of neutral oligosaccharides in negative-ion ultraviolet matrix-assisted laser/desorption ionization mass spectrometry (MALDI MS). The relative abundances of anionized molecules and matrix ([Analyte + Cl]-/[matrix + Cl]-) correlate with the amount of NH4Cl added, and saturate at a level of NH4Cl approximately four times that of the matrix. Their solid-phase fluorescence spectra indicate that harmine and NH4Cl form a complex of the hydrochloride salt in the mixed crystal. The peak intensity at 448 nm from the harmine hydrochloride in the mixed crystal rises logarithmically with the amount of NH4Cl added, a result that quantitatively correlates with increases in the ion abundance ratios of the chloride-anionized molecules to that of harmine. The solid-phase spectroscopic method is useful for studying changes in the characteristics of the matrices and additives in the mixed crystal. Harmine hydrochloride, rather than harmine, works as an effective matrix. The attachment of the chloride to the matrix is essential for the generation of chlorinated-anionized molecules in MALDI. An N-acetyl glucosamine residue (GlcNAc) in lacto-N-tetraose promotes the generation of their chloride-anionized molecules, however, multi-GlcNAc residues in N-acetylchitooligosaccharides hinder it.
氯化铵(NH₄Cl)与β-咔啉哈尔明(7-甲氧基-1-甲基-9H-吡啶并[3,4-b]吲哚)基质在负离子紫外基质辅助激光解吸电离质谱(MALDI MS)中促进中性寡糖的氯离子化分子的生成。阴离子化分子与基质的相对丰度([分析物 + Cl]⁻/[基质 + Cl]⁻)与添加的NH₄Cl量相关,并在NH₄Cl水平约为基质的四倍时达到饱和。它们的固相荧光光谱表明,哈尔明和NH₄Cl在混合晶体中形成盐酸盐络合物。混合晶体中盐酸哈尔明在448 nm处的峰强度随添加的NH₄Cl量呈对数增加,这一结果与氯离子化分子与哈尔明的离子丰度比的增加定量相关。固相光谱法可用于研究混合晶体中基质和添加剂特性的变化。盐酸哈尔明而非哈尔明起有效基质的作用。氯离子与基质的结合对于MALDI中氯化阴离子化分子的生成至关重要。乳糖-N-四糖中的N-乙酰葡糖胺残基(GlcNAc)促进其氯离子化分子的生成,然而,N-乙酰壳寡糖中的多个GlcNAc残基则会阻碍这一过程。