Process for extracting rhynchophylline monomers from uncaria rhynchophylla

An extraction process, the technology of rhynchophylline, applied in the field of extraction process for extracting rhynchophylline monomer, can solve the problems of difficult repetition, complicated steps, cumbersome operation, etc., and achieve the effect of easy operation, simple preparation method and good repeatability

Inactive Publication Date: 2011-06-15
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 h...

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 medicinal materials

[0043] Take dried Uncaria with hooked stems and branches (Hunan Uncaria), pulverize with a pulverizer, 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 In the refrigerator at 4℃; after 12 hours, take out the cold soaking liquid of medicinal materials, ultrasonic for 30min at room temperature and frequency of 50kHz, and shake every 10min during this period to ensure that the solution and medicinal powder are fully effected; after the end of ultrasonic, let it stand for 10min, first with gauze The medicinal residues are filtered off, the filtrate is collected and then filtered through filter paper to obtain the preliminary extract, which is light brown in color; the preliminary extract is divided into 3 times in a rotary evaporator and evaporated to dryness under reduced pressure, each time the temperature is...

Embodiment 2

[0044] Example 2 The crude extract of Uncaria is separated by column chromatography

[0045] The eluent of column chromatography is acetone: petroleum ether: ammonia (1: 2: 0.2). After installing the atmospheric chromatography column (column specification: 5×100cm), add a small amount of eluent and fill a small amount of crude silica gel at the bottom. (80~100 mesh), about 3cm high, always keep the liquid level above the silica gel layer, settling naturally for 15 minutes, add the eluent at any time with a peristaltic pump; weigh 600g of fine silica gel (200~300 mesh) for column chromatography , Add 1500mL eluent, stir well and pour it into the column at one time, settling naturally for 6 hours, the flow rate at the lower end is about 500mL / h, the eluent flowing out is reused, and the silica gel layer is about 70cm high after the sedimentation, which is higher than the fine silica gel layer. Spread a layer of crude silica gel as the sample layer, about 2cm high, and continue to s...

Embodiment 3

[0046] Example 3 Purification and preparation of rhynchophylline 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 2% HCl 4 mL again, repeat the extraction 3 times, and combine The acid solution was transferred to a 100mL separatory funnel; 2mL of chloroform was added to the acid solution and shaken well for 3 minutes to extract impurities and organic phase in the acid solution. After standing for 30 minutes, the lower organic phase was removed, and 2mL 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, and a light yellow precipitate can be seen. Centrifuge at 3000r / min for 10min, discard the supernatant, add 2mL of ultrapure water to the precipitate, mix and shake for 1min to elute Uncaria ...

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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, and the 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 0.27g rhynchophylline 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 rhynchophylline monomer from Uncaria. Background technique [0002] Uncariar rhynchophylla (Miq) Jacks is a traditional Chinese medicine in my country, belonging to the Rubiaceae plants, with a wide variety of species, including Uncaria rhynchophylla (Miq.) Jacks, Uncaria macrophylla Wall, and Uncaria macrophylla Wall. Uncaria hirsuta Havil], Uncaria sinensis (Oliv.) Havil, or Uncaria sessilifructus Roxb, and other 15 species, with hook stems and branches used as medicine, cool in nature, bitter and sweet, with heat-clearing and calming liver, The effect of calming down the wind. Modern studies have shown that Uncaria has significant effects in lowering blood pressure, anti-arrhythmia, sedation and treatment of Alzheimer's disease, and it is safe. [0003] The effective ingredients of Rhizome are indole alkaloids, mainly including rhynchophylline, iso...

Claims

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Application Information

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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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