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Extraction method of alkaloid

An extraction method and technology for dendrobium alkaloids, which are applied in the field of extraction and separation of natural substances, can solve the problems of cumbersome process, low efficiency, long extraction time and the like, and achieve the effect of good separation effect and improved yield.

Active Publication Date: 2019-02-01
ZHONGKAI UNIV OF AGRI & ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the above-mentioned ethanol reflux method combined with macroporous resin purification takes a long time to extract, has low efficiency, cumbersome process, and poor extraction effect

Method used

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  • Extraction method of alkaloid
  • Extraction method of alkaloid
  • Extraction method of alkaloid

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Experimental program
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Embodiment 1

[0044] A method for extracting dendrobium alkaloids, comprising the following steps:

[0045] 1) pulverizing: the dried dendrobium is pulverized through an 80-mesh sieve;

[0046] 2) Extraction: use 95% ethanol for reflux extraction, extract 3 times, use 10 times of material each time, and extract for 3 hours each time; then use 75% of 10 times of material for reflux extraction for 2 hours, centrifuge at 4000rpm for 15min, Collect the supernatant;

[0047] 3) Acidification: Concentrate under reduced pressure at 60°C, use 10 times the volume of 5% dilute hydrochloric acid to disperse the concentrate, centrifuge, and take the supernatant;

[0048] 4) Degreasing: Add 1 / 3 volume of petroleum ether to the supernatant, separate the liquid, and take the water phase;

[0049] 5) Alkalinization: add concentrated ammonia water to the water phase to pH = 9-10, concentrate under reduced pressure at 75°C to constant weight, freeze-dry at -45°C, 20Pa;

[0050] 6) Dissolving: using a mixt...

Embodiment 2

[0054] A method for extracting dendrobium alkaloids, comprising the following steps:

[0055] 1) pulverizing: the dried dendrobium is pulverized through an 80-mesh sieve;

[0056] 2) Leaching: use 95% ethanol for reflux extraction, extract 3 times, use 10 times of material each time, and extract for 3 hours each time; then use 80% ethanol for 10 times of material for reflux extraction for 2 hours, centrifuge at 4000rpm for 15min, Collect the supernatant;

[0057] 3) Acidification: Concentrate under reduced pressure at 60°C, use 10 times the volume of 5% dilute hydrochloric acid to disperse the concentrate, centrifuge, and take the supernatant;

[0058] 4) Degreasing: Add 1 / 4 volume of petroleum ether to the supernatant, separate the liquid, and take the water phase;

[0059] 5) Alkalinization: add concentrated ammonia water to the water phase to pH = 9-10, concentrate under reduced pressure at 80°C to constant weight, freeze-dry at -45°C, 20Pa;

[0060] 6) Dissolving: using...

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Abstract

The invention discloses an extraction method of dendrobium alkaloid. The method comprises the steps of: 1) crushing: crushing dried dendrobium; 2) extraction: using 95-100% ethanol and 75-80% ethanolsuccessively for reflux extraction; 3) acidification: conducting decompression concentration, using 3-8% dilute hydrochloric acid for dispersion, conducting centrifugation, and taking the supernatant;4) degreasing: adding petroleum ether into the supernatant, conducting liquid separation, and taking the water phase; 5) alkalinization: adding concentrated ammonia for alkalization, performing vacuum concentration, and conducting freeze-drying; 6) dissolution: using a mixed solution of chloroform and n-butanol in a ratio of 1:0.5-2 as the co-solvent to dissolve the freeze-dried sample; 7) chromatography: using a developing solvent composed of petroleum ether, methanol and ammonia water in a volume ratio of 5:2-3:0.5 for sample application, chromatography and color development; and 8) collection: cutting off silica gel, performing redissolving, conducting cold air circulating concentration, and recovering dendrobium alkaloid. The extraction method can selectively extract water-soluble alkaloid and oil-soluble alkaloid synchronously, reduces solvent use and improves the extraction efficiency.

Description

technical field [0001] The invention relates to an extraction and separation method of natural substances, in particular to an extraction method of alkaloids. Background technique [0002] Alkaloids are a class of nitrogen-containing basic organic compounds that exist in nature (mainly plants, but some also exist in animals). Most of them have a complex ring structure, and nitrogen is mostly contained in the ring, which has significant biological activity and is one of the important active ingredients in Chinese herbal medicine. [0003] Alkaloids are usually extracted by ethanol reflux method and then separated by macroporous resin. Wherein, the steps of extracting part include: crushing, ethanol extraction, concentration, acidification, degreasing, alkalization, extraction with chloroform and n-butanol saturated aqueous solution, concentration and freeze-drying respectively. After freeze-drying, the pure alkaloid is separated by the macroporous resin method, and the proc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/08A61K36/8984
CPCA61K36/8984A61K2236/15A61K2236/333A61K2236/35A61K2236/39A61K2236/53C07D491/08
Inventor 王琴刘袆帆梁嘉熹柳建良
Owner ZHONGKAI UNIV OF AGRI & ENG
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