Characterization of the vulcanization products of squalene by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry:: model studies on the vulcanization of natural rubber
Characterization of the vulcanization products of squalene by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry:: model studies on the vulcanization of natural rubber
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DOI：
10.1002/jms.130
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发表时间：
2001-03-01
影响因子：
2.3
通讯作者：
Folch, I
中科院分区：
文献类型：
--
作者：
Gros, M;Borr贸s, S;Folch, I
开发了一种使用基质辅助激光解吸/电离夜间质谱 (MALDI-TOFMS) 表征角鲨烯硫化反应产物的方法。角鲨烯被选为天然橡胶的模型分子。使用线性模式下的光谱仪、正/负高电压和不同的激光功率来评估不同的基质-溶剂对。该研究得出以下重要结论。角鲨烯的鉴定需要阳离子化剂，而所用的两类固化体系（次磺酰胺和秋兰姆）的鉴定仅需要使用基质（分别为地蒽酚和二羟基苯甲酸）。首次鉴定了中间体化合物，例如带有含硫侧基并与锌相互作用的角鲨烯衍生物以及交联角鲨烯。仅需要基质，并且溶剂乙腈比 THF（在样品制备过程中低聚）产生更好的光谱。充分的样品处理对于该方法的成功至关重要。找到了表征硫化反应的合适条件。 MALDI-TOFMS 似乎是天然橡胶硫化机理分析和解卷积的重要工具。版权所有 (C) 2001 John Wiley & Sons, Ltd.
A method for the characterization of the vulcanization reaction products of squalene using matrix-assisted laser desorption/ionization time-of-night mass spectrometry (MALDI-TOFMS) was developed. Squalene was chosen as a model molecule for natural rubber. Different matrix-solvent pairs were evaluated with the spectrometer functioning in the linear mode, working with positive/negative high voltages and different laser powers. The study led to the following important conclusions. The identification of squalene requires a cationizing agent whereas the identification of the two families of curing systems used, a sulfenamide and a thiuram, requires only the use of a matrix (dithranol and dihydroxybenzoic acid, respectively). For the first time, the intermediate compounds such as squalene derivatives with pendant sulfur-containing groups and interacting with zinc as well as cross-linked squalene were identified. Only a matrix is required and the solvent acetonitrile leads to better spectra than THF (which oligomerizes during sample preparation). Adequate sample treatment is critical to the success of the method. Suitable conditions were found for the characterization of the vulcanization reaction. MALDI-TOFMS appears to be an important tool for the analysis and deconvolution of the mechanisms of the vulcanization of natural rubber. Copyright (C) 2001 John Wiley & Sons, Ltd.