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

Inactive Publication Date: 2012-07-04
THE SECOND AFFILIATED HOSPITAL ARMY MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the methods for extracting the preliminary extract of Uncaria mainly include boiling method, alcohol-water percolation method, etc., and the total alkaloids of Uncaria have column chromatography to separate the total alkaloids of Uncaria, etc. These methods have complicated steps and low extraction rates.
The extraction and purification of rhynchophylline monomer mainly include microbial fermentation, alkalized benzene extraction, and preparative chromatography. These methods are cumbersome to operate, high in cost, and difficult to repeat

Method used

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  • Process for extracting rhynchophylline monomers from uncaria rhynchophylla
  • Process for extracting rhynchophylline monomers from uncaria rhynchophylla
  • Process for extracting rhynchophylline monomers from uncaria rhynchophylla

Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The invention relates to a process for extracting rhynchophylline monomers from uncaria rhynchophylla. The process comprises the following steps of: pretreating uncaria rhynchophylla medicinal materials by adopting a lower alcohol water quenching ultrasonic method to prepare a crude extract; separating rhynchophylline in the crude extract by adopting a silicagel column chromatography method by using two organic reagents and ammonia water according to a certain proportion as an eluent; and finally obtaining rhynchophylline monomers through steps of eluting fractions, extracting, purifying, andthe like. The method has the advantages of safety, high efficiency, low cost and high rhynchophylline monomer productivity; and per kilogram of the medicinal materials can be used for obtaining 0.27grhynchophylline monomers, and the purity is higher than 90 percent, so that the method is beneficial to industrial large-scale production and provides an approach for the further development of rhynchophylline as a new drug.

Description

technical field [0001] The invention relates to a medicine extraction process, in particular to an extraction process for extracting urticine monomers from Uncaria chinensis. Background technique [0002] Uncariar rhynchophylla (Miq.) Jacks is a traditional Chinese medicine in my country, belonging to Rubiaceae, with a wide variety of species, including Uncaria rhynchophylla (Miq.) Jacks, Uncaria macrophylla Wall, Uncaria [Uncaria rhynchophylla (Miq.) Jacks] Uncaria hirsuta Havil], Chinese Uncaria [Uncaria sinensis (Oliv.) Havil] or Uncaria sessilifructus Roxb, etc. 15 species, with hook stems and branches used as medicine, cool in nature, bitter and sweet, with heat-clearing and liver-pacifying, The effect of calming the wind. Modern research shows that Uncaria has significant antihypertensive, antiarrhythmic, sedative and treatment of Alzheimer's disease and other efficacy, and high safety. [0003] The active ingredients of Uncaria are indole alkaloids, mainly including u...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D471/20
Inventor 汤建林刘明周世文胡岚岚周吉银徐颖
Owner THE SECOND AFFILIATED HOSPITAL ARMY MEDICAL UNIV
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