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Wysłany: Nie 11:00, 27 Lut 2011
Temat postu: The chemical structure of polysaccharides of _2042
The chemical structure of polysaccharides of
LNaH2t'O410, after mixing ceiling (10cm × 2ocm), activation of a dry 1o5 ℃ 2181h, point-like, the agent for the butanol ammonia. Water (6o: 40:5), glucose, galactose, mannose, xylose sugar as the control for the standard single, reagent is aniline. Phthalate. The results show that polysaccharides containing galactose, glucose and mannose 3 ingredients. 1.7.2 Gas Chromatography (GC) to take polysaccharide hydrolysis concentrated to dryness on a water bath at 9O ℃ sugar nitrile acetylation, reaction products directly by gas chromatography. Gas chromatograph for the Hp5809A gas chromatograph,
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, glass column is 2.5110. × 0.2mm fused silica capillary column, stationary phase of a 54 sE, Tam body for ChromsorbW, AWDMCS ,80-100 mesh, detector temperature 280 ℃, gasification chamber temperature 260 ℃, the column temperature was I50 ℃ I80 ℃ 21O. c/m250%, carrier gas N2, flow rate 2ml/min, the injection volume 0.6gl. Gas chromatography analysis showed that the polysaccharide contains mannose, glucose and galactose, the molar ratio of the three half: Portugal: Gan = 4:2:1, shown in Figure 1. Ⅲ blood Figure 1 polysaccharides by gas chromatography {a) sample Ib) sample + Portugal Ic) 1 sample + Portugal + Gan mannose 2. Glucose 3. Galactose glycosidic bond of 1.8 1.8. I infrared spectroscopy (IR) polysaccharides by the KBr pressed powder in NICOET170-SXFT infrared spectrometer analysis on hard times. The results showed that: in the 3200-3000CB a broad peak appears is 0. H stretching vibration; in the 3000-2800cm peak is a group of c. sugar H stretching vibration, in this region of the absorption peak is characteristic absorption peak of sugar; in the 1400 ~ 1200cm absorption peak is the CH vibration peak of variable angle; in the 890m at the absorption peak is a B-type C. pyran H angle vibration absorption peaks, shown in Figure 2. 1.8.2 H NMR ('H-NMR) to take polysaccharides on the 5O0MHzBRUKER NMR analysis, solvent D20, reference standards for the tetracarboxylic silane (TMS). The results showed that the chemical shift of hydrogen is less than 5.0ppm, indicating polysaccharides containing mouth glycosidic bond J. Nanjing University of Traditional Chinese Medicine l4 1998 No. 4 Wei shot 00) e ∞ also) 2i fine a chat nt snail eu Park Rc1 Figure 2 IR spectra of polysaccharides adjacent monosaccharide 1.9 connection base 1 .9.1 periodate oxidation take polysaccharides dissolved in dry goods 100 steep 15mmd/LNa. 104, 100 solution, in the dark (I7 ℃) interval sampling, UV spectrophotometer set at 223nnl Deputy consumption of periodic acid, when IOa-consuming to reach a stable value, use 0. O1raol/LNa0H solution of formic acid formation in the determination of the amount of the sample. The results showed that polysaccharides with periodic acid after reaction in 106h, IOg maximum consumption, consumption per mole of monosaccharide-based periodic acid 0.96, while producing 046mol formic acid. Periodate oxidation under the rules of J, that the polysaccharides and the results of periodate oxidation is consumed 2tool the proportion of high proportion of periodate and formic acid produced 1tool,
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, so we can see bits of the polysaccharide has a 1-6 glycosidic bond. 1.9.2Smith complete degradation of periodate oxidation, the reaction to take 20m1 tuck, plus 2m1 glycol overnight dialysis,
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, dialysis solution was concentrated to small volume, with sodium borohydride, acetic acid and dialysis 48h,
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, evaporated to doing polysaccharide alcohol,
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, adding pyridine and acetic anhydride, the formation of sugar acetate derivative, can be carried out by gas chromatography. Gas chromatography analysis detected a large number of monosaccharides and a small amount of glycerol. Where the product contains large amounts of simple sugars, indicating that there is a lot I molecules of a three glycosidic health, and a small amount of Ganyou Sheng Cheng, the tips are 1 - contempt and 1-2 bit glycosidic bond. 2 Physical and Chemical Properties polysaccharides pure white, powder, soluble in water, viscous solution, pH6, odorless and tasteless. Insoluble in high concentrations of ethanol, ethyl ether, acetone, ethyl acetate and other organic solvents. 1% polysaccharides solution viscosity 500cp, specific rotation of [] = 1.72, anthrone reagent was blue-green, phenol. Sulfuric acid was orange, a naphthol reagent was purple.
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