Departament de Química Analítica, Universitat de Barcelona, Diagonal 647, 08028 Barcelona, Spain.
Anal Bioanal Chem. 2010 Sep;398(1):357-65. doi: 10.1007/s00216-010-3898-y. Epub 2010 Jul 6.
2,5-Dihydroxybenzoic acid (DHB) has been demonstrated to be a more suitable matrix than 3,5-dimethoxy-4-hydroxycinnamic acid (sinapinic acid, SA) to obtain reliable molecular mass values of intact glycoproteins because it prevents sugar fragmentation. Lack of spot homogeneity during the crystallization step was prevented by drying the sample-matrix mixture under vacuum conditions. Nevertheless, this sample-matrix preparation procedure requires a specific experimental setup and may be time-consuming. In this work, we investigated the effectiveness of different ionic liquid matrices (ILMs) with SA and DHB on the ionization of a set of intact glycoproteins with several degrees of glycosylation. The obtained results demonstrate that some of the tested ILMs allow detection of the studied intact glycoproteins. Furthermore, the selected optimum conditions solve the reproducibility issue of using the DHB as a solid matrix without the vacuum drying method and, surprisingly, avoid sugar fragmentation when both SA and DHB were used as ILMs.
2,5-二羟基苯甲酸(DHB)已被证明比 3,5-二甲氧基-4-羟基肉桂酸(芥子酸,SA)更适合作为基质,以获得完整糖蛋白可靠的分子量值,因为它可以防止糖的碎片化。通过在真空条件下干燥样品-基质混合物,防止了结晶步骤中斑点不均匀性的产生。然而,这种样品-基质制备程序需要特定的实验设置,并且可能很耗时。在这项工作中,我们研究了不同的离子液体基质(ILM)与 SA 和 DHB 对一系列具有不同糖基化程度的完整糖蛋白的离子化效果。所得结果表明,一些测试的 ILM 允许检测研究的完整糖蛋白。此外,所选的最佳条件解决了使用 DHB 作为固体基质时的重现性问题,而无需真空干燥方法,并且令人惊讶的是,当同时使用 SA 和 DHB 作为 ILM 时,避免了糖的碎片化。