CN102432651A

CN102432651A - Preparation method of geniposide

Info

Publication number: CN102432651A
Application number: CN201110399579XA
Authority: CN
Inventors: 毕云英
Original assignee: WEIHAI TIANHONG AGRICULTURAL TECHNOLOGY CO LTD
Current assignee: WEIHAI TIANHONG AGRICULTURAL TECHNOLOGY CO LTD
Priority date: 2011-11-25
Filing date: 2011-11-25
Publication date: 2012-05-02

Abstract

The invention discloses an extracting method of geniposide. The extraction method comprises the steps: crushing gardenia, extracting, adsorbing an extract by using macroporous adsorption resin, eluting resin, collecting eluent, concentrating and drying, wherein the macroporous adsorption resin is ADS-21 type, ADS-17 type, ADS-7 type or ADS-F8 type strong-polarity macroporous adsorption resin, and decoction dregs of the gardenia after extraction can be used as feed additive or fertilizer. In the invention, a geniposide product with high purity can be obtained through only one adsorption and separation of the strong-polarity macroporous adsorption resin without the processes of decoloration or odor removal treatment, only water and ethanol are used as extracting solvent in the whole technical process, no solid dregs or technical waste water is caused by using the involving technology, the extracting method is an environment friendly process and is suitable for production and application of enterprises, and the product is good in quality and high in economic value.

Description

A kind of preparation method of jasminoidin

Technical field

The present invention relates to natural medicine field, particularly a kind of method of using cape jasmine as the feedstock production jasminoidin.

Background technology

Cape jasmine is the fruit of Gardenia Ellis Rubiaceae evergreen shrubs cape jasmine, uses and existing more than the 1600 year history of clinical treatment in China, and its bitter, cold in nature; The thoughts of returning home, liver, stomach warp have effects such as clearing away heat and promoting diuresis, water pouring relieving restlessness, removing pathogenic heat from blood and toxic substance from the body, are usually used in the pyreticosis restlessness of asrhenia type and insomnia, jaundice; Gonorrhoea is quenched one's thirst, hot eyes, pharyngalgia; Spit blood, the bloody flux eqpidemic disease is sprained disease such as swell and ache; Hepatic cholagogic arranged, promote pancreatic secretion, step-down, prevent and treat atherosclerosis and antithrombotic formation, the effect of antipyretic-antalgic, antibiotic and anti-inflammatory and treatment soft tissue injury, become active and immunity has restraining effect to fine, soft fur to mutagenic compound, and do not have carcinogenic, teratogenesis, mutagenic toxicity.

Jasminoidin is that utilization high-tech production technique is extracted the refining product that forms from the dry mature fruit of madder wort cape jasmine, is the iridoid glycoside compounds, the different name Geniposide; Molecular weight is 388, and outward appearance is a white, needle-shaped crystals, and fusing point is 148～150 ℃; Hydrophilic organic solvents such as soluble in water and methyl alcohol, ethanol; Be insoluble in hydrophobic organic solvents such as ether, chloroform, tetracol phenixin, purity is highly stable above 98% crystallization jasminoidin, and is difficult for the moisture absorption; The midbody that it is the production gardenia blue, cape jasmine is red, cape jasmine is purple and the effective monomer of crude drug article; Therefore; Separation, purifying, crystallization and assay to jasminoidin become the gordian technique to the cape jasmine deep development; Jasminoidin also has multiple pharmaceutical usage; Have the report pharmacological action to show: jasminoidin has laxative, analgesia, cholagogic, anti-inflammatory, treatment soft tissue injury and suppresses gastric secretion and reduce effect such as pancreatic amylase, also is the material medicine that is used to treat disease such as cardiovascular and cerebrovascular, liver and gall and mellitus, also can generate the increasing crop yield agent.

In China, the cape jasmine aboundresources, cheap and easy to get; Drug effect is clear and definite, and among the people being widely used in food and the medicine is rare large natural medicinal plant resource; From the sixties in 20th century begin one's study cape jasmine effective constituent utilization so far, China only possesses the ability of producing a small amount of jasminoidin product, and the supply of jasminoidin is in very well sold and in short supply state in the international market always; Simultaneously at home along with the improving constantly of modern life level and quality of life, " natural product " gains great popularity, People more and more attention natural medicine; Especially treatment by Chinese herbs; Therefore, should carry out the comprehensive utilizating research of Fructus Gardeniae extract energetically, strengthen the application and development dynamics of cape jasmine product at aspects such as medicine, food.

Summary of the invention

The present invention will disclose the process for extracting that a kind of technology is simple, with low cost, a need promptly obtain jasminoidin through a resin absorption separation.

The process for extracting of jasminoidin of the present invention comprises that cape jasmine is broken---extracts------operations such as the wash-out resin---is collected elutriant---and concentrated, drying that extracting solution is used absorption with macroporous adsorbent resin; Wherein, said macroporous adsorbent resin is the ADS-21 model, or the ADS-17 model; Or ADS-7 model; Or the strong polar macroporous adsorption resin of ADS-F8 model, the strong polar macroporous adsorption resin absorption of the general above-mentioned model of extracting solution can disposablely reach purification, decolour, takes off multiple effects such as flavor.Said wash-out resin is will adsorb good resin water earlier to clean colourlessly to clarifying, and uses ethanolic soln wash-out resin again, and the volumetric concentration of the ethanolic soln of use generally can be 70～90%; And said extraction generally is that the cape jasmine after the fragmentation is put into water or ethanolic soln heating and extracting, and it is 40～60% ethanolic soln that said ethanolic soln is preferably selected volumetric concentration for use; Its extraction time generally is advisable with 1～3 time; The time of each poach remained between 1～3 hour, and each consumption that adds entry or ethanolic soln is generally 5～8 times of cape jasmine weight, extracted temperature generally at 90～100 ℃; The gained extracting solution should be cooled to earlier below 40 ℃, uses resin absorption again.

Process for extracting of the present invention is as long as pass through strong polar macroporous adsorption resin fractionation by adsorption once; Need not warp decolouring again, take off the flavor treatment process, just can obtain the high jasminoidin product of purity, whole technological process only makes water and ethanol for extracting solvent; Production process does not have waste water, waste gas to produce; Big pore resin and ethanol reagent are all recyclable to be utilized again, is fit to suitability for industrialized production, is a kind of environment-friendly type new technology that obtains high-purity natural product jasminoidin.

Embodiment

Below in conjunction with specific embodiment the present invention is done further explain.

Embodiment one

1) gets cape jasmine 100 grams, put into 8 times of water after the fragmentation, be heated to 100 ℃ and decocted 1 hour, cross and filter water extract A to cape jasmine weight;

2) with residue put into 7 times its in the water of weight, stir, be heated to 100 ℃ and decocted 1 hour, cross and filter water extract B;

3) get residue once more and put into 6 times of water, stir, be heated to 100 ℃ and decocted 1 hour, cross and filter water extract C to its weight;

4) merge water extract A, B, C, filter postcooling to 40 ℃;

5) will cool off good filtrating adsorbs with the strong Polar Adsorbent Resin of ADS-F8 model;

6) resin that absorption is good cleans colourless to clarifying with clear water;

7) the use volumetric concentration is 70% ethanolic soln wash-out resin, collects elutriant;

8) ethanol in the recovery elutriant through vacuum concentration, spraying drying, pulverizing, obtains the jasminoidin powder, and through determined by ultraviolet spectrophotometry, wherein the jasminoidin weight content is more than 95%.

Embodiment two

1) get cape jasmine 100 gram, putting into 8 times after the fragmentation is 40% ethanolic soln to jasminoidin weight, volumetric concentration, is heated to 90 ℃ and boils 1 hour, crosses and filters alcohol extract A;

2) with residue put into 7 times its be 40% ethanolic soln in weight, volumetric concentration, stir, be heated to 90 ℃ and boiled 1 hour, cross and filter alcohol extract B;

3) getting residue once more, to put into 6 times be 40% ethanolic soln to its weight, volumetric concentration, stirs, and is heated to 90 ℃ and boiled 1 hour, crosses and filter alcohol extract C;

4) merge alcohol extract A, B, C, filter postcooling to 40 ℃;

5) will cool off good filtrating adsorbs with the strong Polar Adsorbent Resin of ADS-17 model;

7) the use volumetric concentration is 80% ethanolic soln wash-out resin, collects elutriant;

Embodiment three

1) get cape jasmine 500 gram, putting into 8 times after the fragmentation is 40% ethanolic soln to cape jasmine weight, volumetric concentration, is heated to 90 ℃ and boils 1 hour, crosses and filters alcohol extract A;

3) get once more residue put into 6 times its be 40% ethanolic soln in weight, volumetric concentration, stir, be heated to 90 ℃ and boiled 1 hour, cross and filter alcohol extract C;

4) merge alcohol extract A, B, C, filter postcooling to 40 ℃;

5) will cool off good filtrating adsorbs with the strong Polar Adsorbent Resin of ADS-7 model;

7) the use volumetric concentration is 90% ethanolic soln wash-out resin, collects elutriant;

Embodiment four

1) gets cape jasmine 500 grams, put into 8 times of water after the fragmentation, be heated to 100 ℃ and decocted 1 hour, cross and filter water extract A to cape jasmine weight;

4) merge water extract A, B, C, filter postcooling to 40 ℃;

5) will cool off good water extract adsorbs with the strong Polar Adsorbent Resin of ADS-21 model;

Claims

1. the process for extracting of a jasminoidin is characterized in that: it comprises that cape jasmine is broken---extracts that---extracting solution use absorption with macroporous adsorbent resin, and---it is concentrated, dry that the wash-out resin---is collected elutriant---; Wherein, said macroporous adsorbent resin is the ADS-21 model, or the ADS-17 model, or the ADS-7 model, or the strong polar macroporous adsorption resin of ADS-F8 model.

2. the process for extracting of jasminoidin according to claim 1 is characterized in that: said wash-out resin is will adsorb good resin water earlier to clean colourlessly to clarifying, and uses ethanolic soln wash-out resin again.

3. the process for extracting of jasminoidin according to claim 2 is characterized in that: said wash-out resin is that first water cleans resin, and using volumetric concentration again is 70～90% ethanolic soln wash-out resin.

4. according to the process for extracting of any one described jasminoidin in the claim 1～3, it is characterized in that: said extraction is that the cape jasmine after the fragmentation is put into water or ethanolic soln heating and extracting.