Acetylation in Ionic Liquids Dramatically Increases Yield in the Glycosyl Composition and Linkage Analysis of Insoluble and Acidic Polysaccharides

Glycosyl composition and linkage analyses are important first steps toward understanding the structural diversity and biological importance of polysaccharides. Failure to fully solubilize samples prior to analysis results in the generation of incomplete and poor-quality composition and linkage data by gas chromatography–mass spectrometry (GC-MS). Acidic polysaccharides also do not give accurate linkage results, because they are poorly soluble in DMSO and tend to undergo β-elimination during permethylation. Ionic liquids can solubilize polysaccharides, improving their derivatization and extraction for analysis. We show that water-insoluble polysaccharides become much more amenable to chemical analysis by first acetylating them in an ionic liquid. Once acetylated, these polysaccharides, having been deprived of their intermolecular hydrogen bonds, are hydrolyzed more readily for glycosyl composition analysis or methylated more efficiently for glycosyl linkage analysis. Acetylation in an ionic liquid greatly improves composition analysis of insoluble polysaccharides when compared to analysis without acetylation, enabling complete composition determination of normally recalcitrant polysaccharides. We also present a protocol for uronic acid linkage analysis that incorporates this preacetylation step. This protocol produces partially methylated alditol acetate derivatives in high yield with minimal β-elimination and gives sensitive linkage results for acidic polysaccharides that more accurately reflect the structures being analyzed. We use important plant polysaccharides to show that the preacetylation step leads to superior results compared to traditional methodologies

BVRI photometric observations and light-curve analysis of GEO objects

BVRI photometric observations of Geosynchronous Earth Orbit (GEO) objects were conducted with the 1.5 m Cassini Telescope located in Loiano, Italy. The observatory is operated by the INAF (National Institute for Astrophysics) Astronomical Observatory of Bologna, Italy. The Ritchey–Chre´tien optical system is equipped with the BFOSC (Bologna Faint Object Spectrograph and Camera), a multipurpose instrument for imaging and spectroscopy, with an EEV CCD (13401300 pixel). This paper deals with the results of the photometric observations of several targets from the SSN (Space Surveillance Network) catalog that were acquired in May and December 2013