Wood is thermally modified by heating and steaming in order to change its properties, e.g., to improve the biological resistance and to increase the hardness of wood. The structure of thermally modified Scots pine (Pinus sylvestris) was studied using wide-angle, small-angle and ultra-small-angle X-ray scattering methods. Modification temperatures varied from 100 to 240°C. No marked changes in the microfibril angle distribution were observed. The mass fraction of crystalline cellulose in wood (the crystallinity of wood) and the size of cellulose crystallites increased above 150°C. After modification at 230°C for 4 h the thickness of the cellulose crystallites increased from 3.1 to 3.4 nm. Thermal modification had no effect on the orientation of the voids, but an increase in the porosity of the cell wall was observed. The distance between cellulose crystallites was approximately 4.7 nm in hydrated wood and a decrease in order between microfibrils was observed at 160–200°C.
A combined derivatization method for gas chromatographic/mass spectrometric (GC/MS) analysis of steroidal glycoalkaloid (SGA) aglycons was developed using both trimethylsilylation and pentafluoropropionylation. In comparison with underivatized or only silylated aglycons, the new technique produces more specific and abundant fragmentation for compounds with a tomatidine-type structure. For example, the difference between solasodine and tomatidine, the former containing a double bond at position 5,6 in the steroidal skeleton, can be observed by their base peak fragments at m/z 417 (C(24)H(41)O(2)Si(2)) and m/z 419 (C(24)H(43)O(2)Si(2)). The method is well suited for the simultaneous determination of both solanidane- and spirosolane-type SGA aglycons from Solanum species and hybrids. The reproducibility of the method, including SGA extraction, hydrolysis, derivatization, and quantitative GC/MS analysis, was <6% (CV) for the principal aglycons determined from a hybrid between a wild potato species, Solanum brevidens Phil., and a cultivated potato, S. tuberosum L. A single ion monitoring technique using specific fragments m/z 419 and 417 could be applied for the determination of minor stereoisomers, which are often overlapped by large amounts of tomatidine.
Interspecific somatic hybrids produced by protoplast fusion between two wild Solanum species (S. acaule, acl; S. brevidens, brd) and cultivated potato Solanum tuberosum (tbr) were analyzed in terms of the starch nanometer-range structure and glycoalkaloid (GA) contents. The crystallinity of starch granules, the average size of starch crystallites, and the lamellar distances were obtained from tuber samples using wide-angle and small-angle X-ray scattering methods. These measurements showed that incorporation of wild genomes from either nontuberous (brd) or tuberous (acl) Solanum species caused no significant modifications of the nanostructure of potato starch. In contrast, the GA profiles of the hybrids, which were analyzed by LC-ESI-MS in both tuber and foliage samples, differed considerably from those of cultivated potato. Regardless of the low total tuber GA concentrations (approximately 9 mg/100 g of fresh weight), the somatic hybrids contained GAs not detected in the parental species. A high proportion of spirotype GAs consisting of 5,6-dihydrogenated aglycons, for example, alpha-tomatine and tomatidine bound with solatriose, and chacotriose were found in the hybrids. In conclusion, the foliage of interspecific hybrids contained a higher variation in the structures of GAs than did the tubers.
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