Process for extracting rhynchophylline monomers from uncaria rhynchophylla
A technique for urticine and uncaria, which is applied in the field of extraction technology for extracting urticine monomer, can solve the problems of difficulty in repetition, complicated steps, complicated operation and the like, and achieves the effects of easy operation, simple preparation method and good repeatability
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Embodiment 1
[0042] Example 1 Preparation of crude extract of Uncaria chinensis
[0043] Take dry Uncaria chinensis stems and branches (Uncaria chinensis produced in Hunan), pulverize with a pulverizer and pass through a 40-mesh sieve, weigh 1kg into a large beaker, add 5L of 80% ethanol aqueous solution, mix well, seal with plastic wrap, and store in a In a refrigerator at 4°C; after 12 hours, take out the cold infusion liquid of medicinal materials, and ultrasonicate for 30 minutes at room temperature and frequency of 50 kHz. During this period, shake once every 10 minutes to ensure that the solution and medicinal powder are fully interacted; The residues of medicinal materials were filtered off, and the filtrate was collected and then filtered through filter paper to obtain a preliminary extract, which was light brown in color; the preliminary extract was evaporated to dryness under reduced pressure in a rotary evaporator three times, and the temperature was controlled at about 35 °C eac...
Embodiment 2
[0044] Embodiment 2 Uncaria crude extract is separated by column chromatography
[0045] The column chromatography eluent is acetone: petroleum ether: ammonia water (1: 2: 0.2), and a small amount of eluent is added after the installation of an atmospheric pressure chromatography column (chromatographic column size: 5 × 100 cm), and a small amount of coarse silica gel is filled at the bottom. (80-100 mesh), about 3 cm high, always keep the liquid level above the silica gel layer, settle naturally for 15 minutes, and add eluent at any time with a peristaltic pump; weigh 600 g of fine silica gel (200-300 mesh) for column chromatography , add 1500mL of eluent, and pour it into the column at one time after fully stirring, and settle for 6 hours naturally. The flow rate at the lower end is about 500mL / h. A layer of thick silica gel was placed on top as the sample layer, about 2 cm high, and continued to settle for 30 min; weigh 10 g of Uncaria crude extract extract, add 100 mL of a...
Embodiment 3
[0046] Example 3 Purification and preparation of urticine monomer
[0047] Transfer 500 mL of the rhynchophylline fraction separated by column chromatography into a 1L separatory funnel, add 4 mL of 2% HCl, shake vigorously for 3 min, let stand for 15 min, collect the lower acid solution, add 4 mL of 2% HCl again, repeat the extraction 3 times, and combine The acid solution was transferred into a 100 mL separating funnel; 2 mL of chloroform was added to the acid solution, fully shaken for 3 minutes, the impurities and organic phase in the acid solution were extracted, the lower organic phase was removed after standing for 30 minutes, 2 mL of chloroform was added again, and the extraction was repeated 3 times; Add ammonia water dropwise to the acid solution after extraction, adjust the pH to 8-9, a pale yellow precipitate can be seen, centrifuge at 3000 r / min for 10 min, discard the supernatant, add 2 mL of ultrapure water to the precipitate, vortex for 1 min, and wash out Uncar...
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