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A new application of acetylation for analysis of acidic heteropolysaccharides by liquid chromatography-electrospray mass spectrometry

机译:乙酰化乙酰化液相色谱 - 电喷雾质谱法分析乙酰化

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摘要

A novel ultra-high-performance liquid chromatography-electrospray mass spectrometry (UHPLC-ESI-MS) method was proposed for simultaneous determination of neutral and acidic monosaccharaides by employing acetylation derivatization that is specialized for gas chromatography-mass spectrometry (GC-MS) analyses. The UHPLC-ESI-MS was carried out in a positive ionization mode with selective ion monitoring (SIM) of sodium adducts at m/z 385 (Ara, Xyl and Rib), 399 (Rha and Fuc), 443 (Glc, Gal and Man) and 457 (GlcA and GalA). The separation was achieved on a Cortecs C18(+) (2.1 mm x 150 mm, 1.6 mu m) within 8 min using acetonitrile water as the mobile phase without additional buffer salt added. Furthermore, quantitative analysis of the multi-monosaccharaides by single marker (QAMS) was developed and validated using a relative correction factor. The UHPLC-ESI-MS and QAMS were compared and successfully applied to analyze the monosaccharide contents of a purified acidic heteropolysaccharide previously isolated from Ephedra sinica. The established UHPLC-ESI-MS and QAMS approach possesses high precision, stability and repeatability, and can be widely used for high-throughput analysis of the monosaccharide compositions of plant polysaccharides.
机译:提出了一种新型的超高效液相色谱 - 电喷雾质谱(UHPLC-ESI-MS)方法,用于通过采用专门用于气相色谱 - 质谱(GC-MS)分析的乙酰化衍生化来同时测定中性和酸性单变量。在阳性电离模式下进行UHPLC-ESI-MS,在M / Z 385(ARA,XYL和RIB),399(RHA和FUC),443(GLC,GAL和男人)和457(Glca和Gala)。在8分钟内使用乙腈水在8分钟内在Cortcs C18(+)(2.1mm×150mm,1.6μm)上进行分离,作为流动相,没有加入另外的缓冲盐。此外,使用相对校正因子开发和验证单个标记(QAM)对多单次糖的定量分析。比较UHPLC-ESI-MS和QAM,并成功地应用于分析预先从Ephedra Sinica中分离的纯化的酸性杂多糖的单糖含量。已建立的UHPLC-ESI-MS和QAMS方法具有高精度,稳定性和可重复性,并且可以广泛用于植物多糖的单糖组合物的高通量分析。

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