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Physicochemical characterization of silicon-containing glycolipids by DSC,FT-Raman spectroscopy and X-ray diffraction
Authors:Uhr M  Wartewig S  Unruh T  Richter H
Affiliation:Department of Pharmacy, Institute of Pharmaceutical Chemistry, Martin-Luther-Universit?t Halle/Wittenberg, Wolfgang-Langenbeck-Str. 4, 06120 Halle, Germany.
Abstract:Derivatives of dimethylalkylchlorosilanes are novel substances which may be used in formulations for drug targeting. In order to design their properties it is essential to perform physicochemical characterization. For this purpose, a combination of differential scanning calorimetry (DSC), FT-Raman spectroscopy and X-ray diffraction is well suited. For the starting material dimethyloctadecylchlorosilane (DMOC), the assignment of Raman bands is discussed. The influence of sugar-containing head groups on the structures of the hydrocarbon chains of 1-O-(dimethyldodecylsilyl)-[2,3,4,6-tetra-O-acetyl-beta-D-glucopyranoside] and 1-O-(dimethyloctadecylsilyl)-[2,3,4,6-tetra-O-acetyl-beta-D-glucopyranoside] was investigated using the band position of the symmetric methylene mode. The temperature dependence of conformationally sensitive bands in the CH(2)-stretching region (2800-2900 cm(-1)), C-C-stretching region (1000-1150 cm(-1)) and CH(3)-rocking region (830-900 cm(-1)) was studied to characterize the state of order of the alkyl chains. Using X-ray diffraction, the repeating distances of layered structures was determined. The phase transitions occurring were found to be completely reversible. The subcell of DMOC shows an orthorhombic perpendicular packing structure in the crystalline state.
Keywords:Dimethyloctadecylchlorosilane   FT-Raman spectroscopy   X-ray diffraction   Differential scanning calorimetry
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