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Method for preparing dendrobine

A technology of dendrobine and medicinal materials, which is applied in the field of preparation of dendrobine, can solve the problems of low product content, poor quality and high extraction cost, and achieves the effects of high extraction rate, small equipment investment and beneficial extraction.

Inactive Publication Date: 2012-05-30
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing process has many shortcomings such as high extraction cost, low product content, and poor quality.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Grind the medicinal material of Dendrobium nobile, take 100g, add 200ml ammonia water to infiltrate for 3 hours, then add 0.8L 80% ethanol for ultrasonic extraction for 50 minutes, the extraction temperature is 60°C, filter, add 0.5L 80% ethanol for ultrasonic extraction for 30 minutes, extract Filter at a temperature of 50°C, combine the filtrates, pressurize and pass through a hollow ultrafiltration membrane with a molecular weight cut-off of 10,000, and control the pressure to about 0.2Mpa. The extracts were combined, adjusted to pH 9.5 with 10% NaOH, and the precipitate was filtered and dried to obtain 3.2 g of dendrobine crude product; 120980 mesh silica gel was taken and 100 g of acetic acid-sodium acetate buffer (pre-saturated with chloroform) was added to the pH 4.5, Then add buffer-saturated chloroform to soak, tune into a thin paste, wet-pack the column, dissolve the crude dendrobine with 20ml of ether, mix well with 15g of silica gel, evaporate the ether, put ...

Embodiment 2

[0031] Grind the Dendrobium nobile medicinal material, take 500g, add 900ml ammonia water to infiltrate for 4 hours, then add 4L85% ethanol for ultrasonic extraction for 70 minutes, the extraction temperature is 60°C, filter, and add 3L80% ethanol for ultrasonic extraction for 40 minutes to the filter residue, the extraction temperature is Filter at 55°C, combine the filtrates, pressurize and pass through a hollow ultrafiltration membrane with a molecular weight cut-off of 8000, and control the pressure to about 0.3Mpa. Adjust the pH to 10 with 8% KOH, filter out the precipitate and dry it to obtain 11.8 g of dendrobine crude product; get 400 g of 60 mesh silica gel and add 300 g of pH 4.5 acetic acid-sodium acetate buffer solution (pre-saturated with chloroform), then add buffer saturated Soak in chloroform, adjust into a thin paste, and wet-pack the column. Dissolve the crude dendrobine in 90ml of ether, mix well with 40g of silica gel, evaporate the ether, put it on the colu...

Embodiment 3

[0033] Crush the medicinal material of Dendrobium nobile, take 1kg, add 1.5L ammonia water to infiltrate for 5 hours, then add 9L75% ethanol for ultrasonic extraction for 80 minutes, the extraction temperature is 70°C, filter, add 7L75% ethanol to the filter residue for ultrasonic extraction for 50 minutes, the extraction temperature After filtering at 50°C and combining the filtrates, pressurize them to pass through a hollow ultrafiltration membrane with a molecular weight cut-off of 7000, and control the pressure to about 0.4Mpa. , adjusted to pH 9 with 10% NaOH, filtered out the precipitate and dried to obtain 24.7 g of dendrobine crude product; get 800 g of 60 mesh silica gel and add 550 g of pH 4.5 acetic acid-sodium acetate buffer solution (pre-saturated with chloroform), then add buffer saturation soaked in chloroform, adjusted to a thin paste, packed in a column by wet method, dissolved the crude product of dendrobine with 200ml ether, mixed well with 70g silica gel, ev...

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PUM

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Abstract

The present invention relates to a method for preparing dendrobine. The method is characterized by pulverizing Herba dendrobii medicinal material, impregnating with a small amount of ammonia water, adding a high-concentration ethanol solution, ultrasonically extracting for 2-3 times, performing pressure filtration on an extractive solution with an ultrafiltration membrane, concentrating via a nanofiltration membrane, extracting a concentrated solution with acid water for 2-3 times, alkalizing an acid water layer, filtering, dissolving a precipitate in diethyl ether, mixing with a small amount of silica gel uniformly, volatizing the solvent, loading a sample, separating by partition chromatography, monitoring by thin layer chromatography, collecting an eluate, and concentrating under a reduced pressure to near dryness. The method has simple operation, low energy consumption and low investment. The product has high purity and high quality.

Description

Technical field: [0001] The invention belongs to the field of separation of natural products, and in particular relates to a preparation method of dendrobine. Background technique: [0002] Dendrobine, a tetrahydropyrrole alkaloid, is a hydrophobic weak base. [0003] Molecular formula: C 16 h 25 NO 2 . Molecular weight: 263.27. [0004] "Chinese Pharmacopoeia" records: the original plant of Chinese medicine Dendrobium is the stem of Dendrobium (Dendrobium) plant; the nature and flavor are sweet, light, slightly salty, cold; enter the stomach, lung, and kidney meridians; effects: nourishing the stomach and promoting body fluid, nourishing yin Clear heat. It is used for yin deficiency and body fluid deficiency, dry mouth, polydipsia, retching due to lack of food, asthenia heat after illness, and blurred vision. Herbal medicines of past dynasties also have detailed records on its efficacy. The "Book of Herbal Medicine" says: "In the main injury, remove numbness, lower q...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/18
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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