CN103450322A

CN103450322A - Method for extracting ursolic acid from gardenia by using microwaves

Info

Publication number: CN103450322A
Application number: CN 201310410878
Authority: CN
Inventors: 苏刘花
Original assignee: Nanjing Zelang Agricultural Development Co Ltd
Current assignee: Nanjing Zelang Agricultural Development Co Ltd
Priority date: 2013-09-11
Filing date: 2013-09-11
Publication date: 2013-12-18

Abstract

The invention discloses a process for extracting ursolic acid from gardenia by using microwaves. According to the method, the gardenia residue obtained after the geniposide is extracted is used as the raw material, alcohol with certain concentration is used as an extracting agent, and proper solid-to-liquid ratio is regulated, and ursolic acid is extracted with microwaves. The filtering solution is filtered and extracted, and impurities are removed by using macroporous adsorption resin to realize purification; the purified eluant is condensed at reduced pressure and dried, and methanol is crystallized to obtain an ursolic acid product. The purity of the ursolic acid, measured by means of HPLC (High Performance Liquid Chromatography), is higher than 89%. By adopting the method disclosed by the invention, the ursolic acid in the gardenia residue is extracted by means of microwave technology, and the method has the advantages of high efficiency, high speed, time saving, low solvent consumption, low energy consumption and the like, compared with a traditional method.

Description

A kind of method of ursolic acid in microwave extraction cape jasmine

Technical field

The present invention relates to technical field of traditional Chinese medicines, be specifically related to the extracting method of ursolic acid in a kind of cape jasmine.

Background technology

The dry mature fruit that cape jasmine is the madder wort cape jasmine, be applied to the clinical treatment history of existing more than 1600 year in China, belongs to first medicine-food two-purpose resource that the Ministry of Health promulgates, has the function of purging intense heat relieving restlessness, clearing away heat and promoting diuresis, removing pattogenic heat from the blood and toxic material from the body.Cape jasmine fruit contains the multiple effective active compositions such as jasminoidin, ursolic acid.Ursolic acid, have another name called urson, belongs to pentacyclic triterpenoid, has multiple biological activity, comprises anti-diabetic, reducing blood-fat, antitumor, anti-oxidant, carcinogenesis etc.Its structure is as follows:

Figure 2013104108788100002DEST_PATH_IMAGE002

At present, the research of cape jasmine is mostly concentrated on to the cape jasmine glycoside, and to the refining research report of the extraction of ursolic acid in cape jasmine seldom.In Chinese medicinal materials the extracting mode of ursolic acid have multiple, as reflux extraction, percolation, supercritical extraction method, ultrasonic extraction etc.Wherein the microwave extraction technology is development in recent years a kind of technology of utilizing micro-wave energy to improve extraction yield faster, and the method extraction efficiency is high, and spent time is short.

Summary of the invention

The method that the purpose of this invention is to provide ursolic acid in a kind of microwave extraction cape jasmine residue, the method have safety non-toxic, consuming time short, extraction yield is high, the simple advantage of technique.

The present invention includes following steps:

Using the cape jasmine residue with 80 ~ 90% ethanol as extraction agent, the adjusting solid-to-liquid ratio is 1:8～12, microwave extraction 5～10min, microwave power is 150～250W, solution filter after extracting, filtrate is concentrated into to rare medicinal extract, then vacuum-drying obtains crude extract;

2. the above-mentioned crude extract made is added the sherwood oil (30 ~ 60 ℃) of 10 ~ 20 times of crude extract weight to extract 2 ~ 4 times, filter, concentrated;

3., after the medicinal extract of step 2 gained being added to the suitable quantity of water suspendible, with the upper pretreated macroporous adsorbent resin of 2～4BV/h, first with the distilled water of 2～4 times of amount of resin, be washed till colourless, use again 70%～90% ethanolic soln wash-out, collect elutriant, the concentrating under reduced pressure drying, add methanol crystallization, obtain ursolic acid.

Compared with prior art, the present invention has following characteristics:

(1) the present invention has rationally utilized the cape jasmine residue, has saved the energy, has reduced cost;

(2) the present invention adopts microwave technology to be extracted, and has solved the problem low with the traditional extraction process extraction yield, that extraction time long, energy consumption is higher;

(3) to adopt sherwood oil be solvent extraction in the present invention, avoided acetone for traditional method, the residual toxicity problem brought of ethyl acetate equal solvent;

(4) the present invention adopts polymeric adsorbent to carry out purifying, has improved significantly purity and the yield of ursolic acid.

Embodiment

Below by example, the present invention is set forth, but protection of the present invention is not limited to this.

Embodiment 1:

Claim the dry cape jasmine residue 1kg of obtaining, the ethanol that adds 8L 80%, microwave extraction 10min, the power of microwave is 200 watts, solution filter after extracting, filtrate is concentrated into rare medicinal extract, then vacuum-drying obtains jasminoidin fruit crude extract, and crude extract is extracted 3 times with the sherwood oil (30 ~ 60 ℃) of 10 times of amounts, combining extraction liquid, filter, concentrated, obtain medicinal extract; After again medicinal extract being added to the suitable quantity of water suspendible, pass through pretreated AB-8 macroporous adsorbent resin with 2BV/h, first use the distilled water wash-out of 4 times of amounts, discard elutriant, then use 80% ethanol elution, collect elutriant, the concentrating under reduced pressure drying, add methanol crystallization, obtain 4.21g ursolic acid product, it is 89.5% that the HPLC method records ursolic acid purity.

Embodiment 2:

Claim the dry cape jasmine residue 1kg of obtaining, the ethanol that adds 10L 90%, microwave extraction 8min, the power of microwave is 150 watts, solution filter after extracting, filtrate is concentrated into rare medicinal extract, then vacuum-drying obtains jasminoidin fruit crude extract, and crude extract is extracted 2 times with the sherwood oil (30 ~ 60 ℃) of 15 times of amounts, combining extraction liquid, filter, concentrated, obtain medicinal extract; After again medicinal extract being added to the suitable quantity of water suspendible, pass through pretreated NKA macroporous adsorbent resin with 3BV/h, first use the distilled water wash-out of 2 times of amounts, discard elutriant, then use 70% ethanol elution, collect elutriant, the concentrating under reduced pressure drying, add methanol crystallization, obtain 4.12g ursolic acid product, it is 89.1% that the HPLC method records ursolic acid purity.

Embodiment 3:

Claim the dry cape jasmine residue 1kg of obtaining, the ethanol that adds 12L 90%, microwave extraction 5min, the power of microwave is 250 watts, solution filter after extracting, filtrate is concentrated into rare medicinal extract, then vacuum-drying obtains jasminoidin fruit crude extract, and crude extract is extracted 4 times with the sherwood oil (30 ~ 60 ℃) of 20 times of amounts, combining extraction liquid, filter, concentrated, obtain medicinal extract; After again medicinal extract being added to the suitable quantity of water suspendible, pass through pretreated X-5 macroporous adsorbent resin with 4BV/h, first use the distilled water wash-out of 2 times of amounts, discard elutriant, then use 90% ethanol elution, collect elutriant, the concentrating under reduced pressure drying, add methanol crystallization, obtain 4.16g ursolic acid product, it is 89.3% that the HPLC method records ursolic acid purity.

Claims

1. the microwave extraction technique of ursolic acid in a cape jasmine, is characterized in that, the cape jasmine residue extracted after jasminoidin of take is raw material, add certain density ethanol, regulate suitable solid-to-liquid ratio, the microwave extraction ursolic acid, filter, filtrate is concentrated into to rare medicinal extract, then vacuum-drying obtains the cape jasmine fruit crude extract; The sherwood oil of 10 ~ 20 times of crude extract weight (30 ~ 60 ℃) extracts 2 ~ 4 times, filters, concentrated; Then, after the crude extract of gained being added to the suitable quantity of water suspendible, with the upper pretreated macroporous adsorbent resin of 2 ~ 4BV/h, first with the distilled water of 2～4 times of amount of resin, be washed till colourless, use again 70%～90% ethanolic soln wash-out, collect elutriant, the concentrating under reduced pressure drying, add methanol crystallization, obtain ursolic acid.

2. the method for ursolic acid in microwave extraction cape jasmine residue according to claim 1, is characterized in that, in leaching process, the alcohol concn added is 80%～90%, and described suitable solid-to-liquid ratio is 1:8～12.

3. the method for ursolic acid in microwave extraction cape jasmine residue according to claim 1, is characterized in that, described microwave extraction condition is microwave power 150～250W, extraction time 5～10min.

4. the method for ursolic acid in microwave extraction cape jasmine residue according to claim 1, it is characterized in that, the preprocessing process of macroporous adsorbent resin is soaked in absolute ethyl alcohol 24h, from the micropore of resin, drives bubble out of, allow rear water repeatedly rinse, until the liquid eluted is not in muddiness.

5. the method for ursolic acid in microwave extraction cape jasmine according to claim 1, is characterized in that, described macroreticular resin is AB-8, NKA, X-5.