Bonaduce Ilaria, Brecoulaki Hariclia, Colombini Maria Perla, Lluveras Anna, Restivo Vincenzo, Ribechini Erika
Dipartimento di Chimica e Chimica Industriale, Università di Pisa, via Risorgimento 35, 56126 Pisa, Italy.
J Chromatogr A. 2007 Dec 21;1175(2):275-82. doi: 10.1016/j.chroma.2007.10.056. Epub 2007 Oct 25.
This paper presents an analytical GC-MS procedure to study the chemical composition of plant gums, determining aldoses and uronic acids in one step. The procedure is based on the silylation of aldoses and uronic acids, released from plant gums by microwave assisted hydrolysis, and previously converted into the corresponding diethyl-dithioacetals and diethyl-dithioacetal lactones. Using this method only one peak for each compound is obtained, thus providing simple and highly reproducible chromatograms. The analytical procedure was optimised using reference samples of raw plant gums (arabic, karaya, ghatti, guar, locust bean and tragacanth, cherry, plum and peach gums), commercial watercolours and paint layers prepared according to ancient recipes at the Opificio delle Pietre Dure of Florence (Italy). To identify gum media in samples of unknown composition, a decisional schema for the gum identification and the principal component analysis of the relative sugar percentage contents were employed. The procedure was used to study samples collected from wall paintings from Macedonian tombs (4th-3rd centuries bc) and from the Mycenaean "Palace of Nestor" (13th century bc) in Pylos, Greece. The presence of carbohydrates was ascertained and plant gum binders (fruit and a mixture of tragacanth and fruit tree gums) were identified in some of the samples.
本文介绍了一种分析气相色谱 - 质谱联用(GC-MS)方法,用于研究植物胶的化学成分,可一步测定醛糖和糖醛酸。该方法基于对醛糖和糖醛酸的硅烷化反应,醛糖和糖醛酸通过微波辅助水解从植物胶中释放出来,并预先转化为相应的二乙二硫缩醛和二乙二硫缩醛内酯。使用这种方法,每种化合物仅获得一个峰,从而提供简单且重现性高的色谱图。使用原始植物胶(阿拉伯胶、刺梧桐胶、吉提胶、瓜尔豆胶、刺槐豆胶和黄芪胶、樱桃胶、李子胶和桃胶)的参考样品、商业水彩颜料以及按照意大利佛罗伦萨的Opificio delle Pietre Dure的古代配方制备的漆层对分析程序进行了优化。为了鉴定未知成分样品中的胶凝介质,采用了胶类鉴定的决策模式和相对糖含量的主成分分析。该方法用于研究从马其顿古墓(公元前4至3世纪)的壁画以及希腊皮洛斯的迈锡尼“内斯特宫”(公元前13世纪)采集的样品。确定了碳水化合物的存在,并在一些样品中鉴定出植物胶粘合剂(水果以及黄芪胶和果树胶的混合物)。