Solid-phase permethylation of glycans for mass spectrometric analysis

Solid-phase permethylation of glycans for mass spectrometric analysis
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DOI:
10.1002/rcm.2210
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发表时间:
2005-01-01
影响因子:
2
通讯作者:
Novotny, MV
Novotny, MV
中科院分区:
化学3区
文献类型:
--
作者:
Kang, P;Mechref, Y;Novotny, MV

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开发了一种用于寡糖定量全甲基化的小型化方法,该方法包括将氢氧化钠粉末填充在微旋柱或熔融石英毛细管(500 μ m i.d.)中,允许在小于一分钟的时间内在微尺度下有效衍生化。在质谱分析之前,分析物与碘甲烷在含有痕量水的二甲基亚砜溶液中混合,然后通过微反应器注入。该程序最大限度地减少了氧化降解和剥离反应,并避免了过度清洁的需要。皮摩尔量的线性和分支,唾液酸化和中性聚糖样品快速,有效地通过这种方法进行全甲基化,并通过基质辅助激光解吸/电离质谱分析。版权所有(c)2005年约翰威利父子有限公司。
A miniaturized approach was developed for quantitative permethylation of oligosaccharides, which involves packing of sodium hydroxide powder in microspin columns or fused-silica capillaries (500 mu m i.d.), permitting effective derivatization in less than a minute at microscale. Prior to mass spectrometry, analytes are mixed with methyl iodide in dimethyl sulfoxide solution containing traces of water before infusing through the microreactors. This procedure minimizes oxidative degradation and peeling reactions and avoids the need of excessive clean-up. Picomole amounts of linear and branched, sialylated and neutral glycan samples were rapidly and efficiently permethylated by this approach and analyzed by matrix-assisted laser desorption/ionization mass spectrometry. Copyright (c) 2005 John Wiley & Sons, Ltd.