A kind of dendrobium dendrobii polysaccharide and its preparation and application
A technology of Dendrobium purpurea and polysaccharide, applied in the field of medicinal chemistry, can solve the problems of unclear active ingredients and structural characteristics of Dendrobium polysaccharide, high cost of raw materials, slow growth, etc. Effect
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Embodiment 1
[0045] Preparation of Dendrobium purple polysaccharide:
[0046] (1) Dry and powder the stems of Dendrobium officinale, degrease with 80% ethanol under reflux, add water to make the ratio of solid to liquid 1:30, extract by microwave reaction, microwave power 800w, reaction time 9min.
[0047] (2) Concentrate the water extract to a certain volume, add 4 times the volume of 95% ethanol to precipitate, let stand for 30 minutes, centrifuge at 4000g for 10 minutes, retain the precipitate, add water to redissolve, freeze-dry to obtain crude polysaccharide, and the extraction rate is 28.3%. Wherein, the freeze-drying conditions are: temperature -50--70°C, absolute pressure about 4-7 Pa.
[0048] (3) Add the above crude polysaccharide and deionized water to form a solution with a concentration of 5-10mg / mL, perform ultrafiltration (molecular weight cut-off: >3kDa, Millipore, Billerica, MA, USA), discard the ultrafiltrate, and rehydrate repeatedly , ultrafiltration, adopting phenol-s...
Embodiment 2
[0050] Preparation of Dendrobium purple polysaccharide:
[0051] Properly crushed fresh or dried Dendrobium purple-skinned dendrobium is added to water for extraction, and the water extract is treated with an ultrafiltration membrane with a molecular weight cut-off of 10,000 Da; after the filtrate is discarded, water replenishment and ultrafiltration are repeated several times, and the phenol-sulfuric acid method is used to track and detect sugar content, until basically no sugar is detected in the filtrate, and the retentate is freeze-dried to obtain the purified Dendrobium polysaccharide (DDP), which is detected by iodine-potassium iodide without starch, and without uronic acid by m-hydroxybiphenyl colorimetry Check out.
Embodiment 3
[0053] Identification of polysaccharides from Dendrobium nobile:
[0054] (1) Monosaccharide composition analysis of polysaccharides from Dendrobium nobile
[0055] Gas chromatography-mass spectrometry was used to determine the monosaccharide composition of Dendrobium dendrobii polysaccharides. Take 5 mg of dendrobium dendrobium polysaccharide samples and add 1mL 2M TFA to hydrolyze them under microwave. The microwave conditions are: power 500W, microwave time 4min, after cooling, hydrolyze The solution was blown dry with nitrogen, added 0.5mL pyridine (containing 20mg hydroxylamine hydrochloride) and reacted at 90°C for 30min, then added 0.5mL acetic anhydride and heated at 90°C for 30min, blown dry with nitrogen, dissolved in 1mL methanol and determined by GC-MS.
[0056] The GC-MS analysis conditions were: Agilent 19091S-433 column, HP-5MS capillary column (30m×0.25mm×0.25μm); the inlet temperature was 250°C; the carrier gas was He gas, and the column flow rate was 1.0mL / mi...
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