Preparation method of high purity capsaicin monomer

A high-purity technology for capsaicin, applied in the separation and purification of capsaicin, the purification of natural active ingredients, and the field of dihydrocapsaicin monomer, which can solve the problems of long time consumption, low purity, and large solvent consumption

Inactive Publication Date: 2014-10-29
北京龙程菁华生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent CN102557981A uses high-speed countercurrent chromatography to separate, but only obtains capsaicin with a purity of 90.3% to 92.8%, which is relatively low in purity; patent CN101200433B uses high-speed countercurrent chromatography to obtain capsaicin, dihydrocapsaicin and nordihydrocapsaicin

Method used

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  • Preparation method of high purity capsaicin monomer
  • Preparation method of high purity capsaicin monomer
  • Preparation method of high purity capsaicin monomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Measure 100mL of capsicum essential oil into a beaker, add 300mL of 75% ethanol, stir and extract at 30°C for 12h, let it stand for 1h, filter, concentrate the filtrate under reduced pressure to remove alcohol, put the concentrate directly on the column for adsorption, and wash away impurities with 15% ethanol , Then elute with 70% ethanol, collect eluate, concentrate under reduced pressure, dry to obtain 22.73g capsaicin total alkaloids.

[0031] (2) Use Shanghai Tongtian TBE-300C semi-preparative high-speed countercurrent chromatography system for separation, the volume of the column is 300mL, the solvent system is petroleum ether-ethyl acetate-ethanol-water 5:5:5:5, column temperature: 25°C. The preparation of capsaicin and dihydrocapsaicin is carried out in two steps: 1. sherwood oil-ethyl acetate-ethanol-water with a volume ratio of 5:5:5:5 is miscible in a separatory funnel, shake up and then separate layer. Get the upper layer solution (upper phase) as the ...

Embodiment 2

[0033] Shanghai Tongtian TBE-300C semi-preparative high-speed countercurrent chromatography system was used for separation. The column volume was 300mL, the solvent system was n-hexane-ethyl acetate-methanol-water 5:5:5:5, and the column temperature was 25°C. The preparation of capsaicin and dihydrocapsaicin is carried out in two steps: 1. Mix n-hexane-ethyl acetate-methanol-water with a volume ratio of 5:5:5:5 in a separatory funnel, shake it up and then divide layer. Get the upper layer solution (upper phase) as the stationary phase, and the lower layer solution (lower phase) as the mobile phase. Before sample injection, fill the entire column with the stationary phase, adjust the speed of the main engine to 890rpm, and pump the mobile phase into the column at a flow rate of 7.0mL / min to establish a dynamic balance of the entire system. Mixed solution 4mL dissolves 300mg of total alkaloids of capsaicin obtained in Example 1 and is injected by the injection valve, and then r...

Embodiment 3

[0035] (1) Measure 200g of chili powder into a beaker, add 400mL of 75% ethanol, stir and extract at 50°C for 12h, let it stand for 1h, filter, concentrate the filtrate under reduced pressure to remove alcohol, put the concentrate directly on the column for adsorption, and wash away impurities with 15% ethanol , Then elute with 70% ethanol, collect eluate, concentrate under reduced pressure, dry to obtain 6.2g capsaicin total alkaloids.

[0036] (2) Use Shanghai Tongtian TBE-300C semi-preparative high-speed countercurrent chromatography system for separation, the volume of the column is 300mL, the solvent system is n-hexane-ethyl acetate-methanol-0.4mM hydrochloric acid 5:5:5:5, the column Temperature: 35°C. The preparation of capsaicin and dihydrocapsaicin is carried out in two steps: 1. the n-hexane-ethyl acetate-methanol-0.4mM hydrochloric acid miscibility of 5:5:5:5 by volume ratio is mixed in the separatory funnel, after shaking up Still layering. Get the upper layer so...

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Abstract

A preparation method of high purity capsaicin monomer comprises the following steps: using alcohol to extract capsaicin from pepper powder or pepper essential oil, then using macroporous resin to enrich the extract so as to obtain pepper total alkaloid; adopting a high speed counter-current chromatography method to separate the pepper total alkaloid, wherein the separating solvent system is composed of alkane, ester, alcohol, and water, and acid and alkali can be added too; adding the solvent system into a separating funnel, fully vibrating the separating funnel, allowing the separating funnel to stand still so as to divide the solution to different layers, collecting the upper-layer solvent as the stationary phase and the lower-layer solvent as the mobile phase; dissolving a sample in a mixed solvent of the upper-layer solvent and the lower-layer solvent, injecting the sample into a detector, separating, and collecting the target components according to the spectrogram on the detector so as to obtain the capsaicin monomer and dihydrocapsaicin monomer. The method has the advantages of simple technology process, low cost, high product purity, high yield, and environment-friendliness, can rapidly prepare capsaicin monomer and dihydrocapsaicin monomer with a content of more than 98%, and is suitable for industrial production of high purity capsaicin and dihydrocapsaicin.

Description

technical field [0001] The invention belongs to the field of natural product extraction, separation and purification, in particular to a method for purification of natural active ingredients, more specifically to a method for separating and purifying capsaicin and dihydrocapsaicin monomers from total alkaloids of capsicum by using high-speed countercurrent chromatography Methods. Background technique [0002] Capsaicin (also known as capsaicin, Capsaicinoids) is a class of extremely pungent vanilla amide alkaloids, and is the main spicy component in capsicum fruit, wherein capsaicin and dihydrocapsaicin account for more than 90% of the total alkaloids. At present, capsaicin is mainly used as an analgesic for external use, an analgesic for detoxification, an antipruritic, a stomach-invigorating and digestive agent, a drug for preventing heart disease, a weight-loss drug, an insecticide, and military applications. Capsaicin has complex physiological and pharmacological activi...

Claims

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Application Information

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IPC IPC(8): C07C231/24C07C233/20C07C233/18
Inventor 黄昀高春春苏士月朱金丽陈本科唐劲天张松豹张子成
Owner 北京龙程菁华生物科技有限公司
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