CN105037463A - Method for extracting geniposide from jasmine - Google Patents
Method for extracting geniposide from jasmine Download PDFInfo
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- CN105037463A CN105037463A CN201510541584.8A CN201510541584A CN105037463A CN 105037463 A CN105037463 A CN 105037463A CN 201510541584 A CN201510541584 A CN 201510541584A CN 105037463 A CN105037463 A CN 105037463A
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Abstract
The invention discloses a method for extracting geniposide from jasmine. The method comprises the following steps of soaking treatment, raw material treatment, first-time enzymolysis, deoiling, second-time enzymolysis, column chromatography and drying. According to the method, enzymes are adopted for extracting plant fat at first, non-oil components are utilized for separating oil and non-oil components according to the affinity difference between oil and water and the different specific gravities of oil and water, and the product yield and the extraction rate are increased.
Description
Technical field
The present invention relates to the extracting method of biological technical field, is a kind of method extracting Geniposide from cape jasmine specifically.
Background technology
Mast is the fruit of Rubiaceae (Rubiaceae) plant mast (GardeniajasminoidesEllis), oblong or ellipse, in scarlet or yellowish red color, the first batch of medicine-food two-purpose resource that the Wei Zishu Ministry of Health promulgates is traditional Chinese medicine.Mast has purging intense heat relieving restlessness, clearing heat and promoting diuresis, removing pattogenic heat from the blood and toxic material from the body, and cholagogic protects the liver, step-down, sterilizing anti-inflammatory, effect of externally used detumescence pain relieving.Tcm clinical practice is mainly used in treat pyreticosis, Jaundice Jaundice, sprain and contusion, hypertension, diabetes etc.Chemical composition in mast is a lot, and wherein mainly contain Crocin, the iridoids such as trans-crocetin (Ichietal) and Geniposide (Geniposide), its Geniposidic is its principle active component.
Geniposide is a kind of Iridoidglucoside, soluble in water.Geniposide can be hydrolyzed to genipin by R-glucosaccharase.Modern study shows, Geniposide during Digestive tract, cardiovascular system are unified general nervous system disorders all have significant curative effect, in addition, Geniposide also has the effect of certain anti-inflammatory and treatment soft tissue injury.Geniposide, except medicinal, is also widely used in other field, as can be used as plant promoter, biological detection agent etc., is a kind of important biologically active substance.Be widely used in medical treatment, field of health care products.
Geniposide is mainly present in the natural phant such as mast, the bark of eucommia, be extract the desirable feedstock of Geniposide, in domestic existing extraction process scheme, also exist that extraction yield is not high, product purity is low, energy consumption is large, in a large number with an organic solvent, the problem such as wastewater flow rate is large.
Summary of the invention
The object of this invention is to provide a kind of method extracting Geniposide from cape jasmine, there is technique simple, be applicable to producing, the advantages such as production cost is low.
The present invention is achieved through the following technical solutions, and specifically comprises the steps:
1) immersion treatment: cape jasmine is loaded woven bag, ties mouth, is placed in pond, pond topped up with water, and presses weight on pond, soaks;
2) Feedstock treating: by step 1) cape jasmine that obtains to pulverize or broken, adds the pure water being equivalent to raw material 2-3 times weight, be heated to 50-60 DEG C and maintain 5-10 minute, obtain paste serous material;
3) first time enzymolysis: by step 2) paste serous material that obtains, tunes pH is 4-5, and the N.F,USP MANNITOL of the pectin-cellulose prozyme and 0.001 weight part that add paste serous material 0.05-0.1% weight part carries out enzymolysis 40-60 minute, obtains enzymolysis solution for the first time;
4) deoil: by step 3) the first time enzymolysis solution that obtains, add the pure water of 2-3 times of weight, be heated to 60-70 DEG C of lixiviate 60-120 minute, obtain upper strata oil slick liquid and subnatant, slag mixture, be separated;
5) second time enzymolysis: by step 4) subnatant, the slag mixture that obtain, adjust pH to be 4.5, add the cellulase being equivalent to mixture 0.1-0.2% weight part and carry out enzymolysis 40-60 minute, obtain second time enzymolysis solution, repeat twice;
6) column chromatography: merge second time enzymolysis solution, filter, concentrated, by column chromatography, adsorbing with macroporous adsorbent resin, is colourless with washed with de-ionized water resin to flowing liquid, then is the ethanolic soln wash-out of 15-20% by concentration, collects elutriant;
7) dry: elutriant to be concentrated, obtains the Geniposide of paste, then obtain Geniposide by drying.
Step 1 of the present invention) described in immersion, time preferred 15-24 hour.
Step 3) described in pectin-cellulose prozyme, preferred activity is the solid-state of 1-3 ten thousand activity unit/gram (milliliter) or liquid pectin-fiber composite enzyme.
Step 6) described in the preferred D101 type of macroreticular resin, DA201 type.
Compared with prior art, advantage of the present invention:
1, the vegetable cell of cape jasmine is interior containing a large amount of greases, be the mixture of the compound composition of triglyceride level primarily of composition, these greases with elaioleucite and oil body protoplastis form, the existence form such as to be irregularly dispersed in cell in discontinuous particulate state, together with granule protein body and to exist.Existing extracting method, all by mode extracting directly such as water extraction/alcohol extracting, enzymolysis or microwave extraction after directly the raw materials such as cape jasmine being smashed or pulverized, when extraction, grease in cell together with time isolate, the compositions such as the group containing grease and Geniposide, genipic acid, pigment mix, thus affect the separation of follow-up effective constituent, add the intractability of operation.The present invention first adopts enzyme extraction Vegetable oil lipoprotein, utilizes non-oil component different with the avidity difference of water and profit proportion and by oil and non-oil component separating, add product yield and improve extraction yield to oil.
2, the present invention adopts cape jasmine pond to soak, and cape jasmine is immersed in water, and cape jasmine is softened gradually, and moisture enters into inside naturally, is beneficial to the separation of Vegetable oil lipoprotein, is beneficial to follow-up enzymolysis, deoils; Meanwhile, cape jasmine is immersed in water, anaerobic bacterium amount reproduction, and particularly when summer, meeting souring, pH value can drop to about 4, the adjustment pH of convenient operation below.
3, the present invention first adopts pectin-cellulose prozyme to remove cell walls, and the grease in release vegetable cell, adds N.F,USP MANNITOL, can keep osmotic pressure, be beneficial to the release of grease.
4, the Geniposide that obtains of the present invention, detects through HPLC, and content is more than 98.5%, and yield improves 25% than prior art.
Embodiment
With embodiment, the invention will be further described below, but the present invention is not limited to these embodiments.
Embodiment 1:
From cape jasmine, extract a method for Geniposide, specifically comprise the steps:
1) immersion treatment: cape jasmine is loaded woven bag, ties mouth, is placed in pond, pond topped up with water, and presses weight on pond, soaks 15 hours;
2) Feedstock treating: by step 1) cape jasmine that obtains pulverizes, adds the pure water being equivalent to raw material 2-3 times weight, be heated to 50 DEG C and maintain 5 minutes, obtain paste serous material;
3) first time enzymolysis: by step 2) paste serous material that obtains, pH is adjusted to be 4, add paste serous material 0.05% parts by weight of activated be 10,000 activity units/gram pectin-cellulose prozyme and the N.F,USP MANNITOL of 0.001 weight part carry out enzymolysis 40 minutes, obtain first time enzymolysis solution;
4) deoil: by step 3) the first time enzymolysis solution that obtains, add the pure water of 2 times of weight, be heated to 60 DEG C of lixiviates 120 minutes, obtain upper strata oil slick liquid and subnatant, slag mixture, be separated;
5) second time enzymolysis: by step 4) subnatant, the slag mixture that obtain, adjust pH to be 4.5, add the cellulase being equivalent to mixture 0.1% weight part and carry out enzymolysis 60 minutes, obtain second time enzymolysis solution, repeat twice;
6) column chromatography: merge second time enzymolysis solution, filter, concentrated, by column chromatography, adsorbing with D101 type macroporous adsorbent resin, is colourless with washed with de-ionized water resin to flowing liquid, then is the ethanolic soln wash-out of 20% by concentration, collects elutriant;
7) dry: elutriant to be concentrated, obtains the Geniposide of paste, then obtain Geniposide by drying, detect through HPLC, content 99.1%.
Embodiment 2:
From cape jasmine, extract a method for Geniposide, specifically comprise the steps:
1) immersion treatment: cape jasmine is loaded woven bag, ties mouth, is placed in pond, pond topped up with water, and presses weight on pond, soaks 24 hours;
2) Feedstock treating: by step 1) cape jasmine that obtains is broken, and add the pure water being equivalent to raw material 2-3 times weight, be heated to 60 DEG C and maintain 8 minutes, obtain paste serous material;
3) first time enzymolysis: by step 2) paste serous material that obtains, pH is adjusted to be 4.5, adding paste serous material 0.1% parts by weight of activated is that the pectin-cellulose prozyme of 20,000 activity units/milliliter and the N.F,USP MANNITOL of 0.001 weight part carry out enzymolysis 50 minutes, obtains first time enzymolysis solution;
4) deoil: by step 3) the first time enzymolysis solution that obtains, add the pure water of 3 times of weight, be heated to 70 DEG C of lixiviates 60 minutes, obtain upper strata oil slick liquid and subnatant, slag mixture, be separated;
5) second time enzymolysis: by step 4) subnatant, the slag mixture that obtain, adjust pH to be 4.5, add the cellulase being equivalent to mixture 0.15% weight part and carry out enzymolysis 50 minutes, obtain second time enzymolysis solution, repeat twice;
6) column chromatography: merge second time enzymolysis solution, filter, concentrated, by column chromatography, adsorbing with DA201 type macroporous adsorbent resin, is colourless with washed with de-ionized water resin to flowing liquid, then is the ethanolic soln wash-out of 15% by concentration, collects elutriant;
7) dry: elutriant to be concentrated, obtains the Geniposide of paste, then obtain Geniposide by drying, detect through HPLC, content 99.3%.
Embodiment 3:
1) immersion treatment: cape jasmine is loaded woven bag, ties mouth, is placed in pond, pond topped up with water, and presses weight on pond, soaks 18 hours;
2) Feedstock treating: by step 1) cape jasmine that obtains pulverizes, adds the pure water being equivalent to raw material 2-3 times weight, be heated to 55 DEG C and maintain 10 minutes, obtain paste serous material;
3) first time enzymolysis: by step 2) paste serous material that obtains, pH is adjusted to be 5, add paste serous material 0.08% parts by weight of activated be 30,000 activity units/gram pectin-cellulose prozyme and the N.F,USP MANNITOL of 0.001 weight part carry out enzymolysis 60 minutes, obtain first time enzymolysis solution;
4) deoil: by step 3) the first time enzymolysis solution that obtains, add the pure water of 2 times of weight, be heated to 65 DEG C of lixiviates 100 minutes, obtain upper strata oil slick liquid and subnatant, slag mixture, be separated;
5) second time enzymolysis: by step 4) subnatant, the slag mixture that obtain, adjust pH to be 4.5, add the cellulase being equivalent to mixture 0.2% weight part and carry out enzymolysis 40 minutes, obtain second time enzymolysis solution, repeat twice;
6) column chromatography: merge second time enzymolysis solution, filter, concentrated, by column chromatography, adsorbing with D101 type macroporous adsorbent resin, is colourless with washed with de-ionized water resin to flowing liquid, then is the ethanolic soln wash-out of 20% by concentration, collects elutriant;
7) dry: elutriant to be concentrated, obtains the Geniposide of paste, then obtain Geniposide by drying, detect through HPLC, content 98.9%.
Claims (4)
1. from cape jasmine, extract a method for Geniposide, it is characterized in that, comprise the steps:
1) immersion treatment: cape jasmine is loaded woven bag, ties mouth, is placed in pond, pond topped up with water, and presses weight on pond, soaks;
2) Feedstock treating: by step 1) cape jasmine that obtains to pulverize or broken, adds the pure water being equivalent to raw material 2-3 times weight, be heated to 50-60 DEG C and maintain 5-10 minute, obtain paste serous material;
3) first time enzymolysis: by step 2) paste serous material that obtains, tunes pH is 4-5, and the N.F,USP MANNITOL of the pectin-cellulose prozyme and 0.001 weight part that add paste serous material 0.05-0.1% weight part carries out enzymolysis 40-60 minute, obtains enzymolysis solution for the first time;
4) deoil: by step 3) the first time enzymolysis solution that obtains, add the pure water of 2-3 times of weight, be heated to 60-70 DEG C of lixiviate 60-120 minute, obtain upper strata oil slick liquid and subnatant, slag mixture, be separated;
5) second time enzymolysis: by step 4) subnatant, the slag mixture that obtain, adjust pH to be 4.5, add the cellulase being equivalent to mixture 0.1-0.2% weight part and carry out enzymolysis 40-60 minute, obtain second time enzymolysis solution, repeat twice;
6) column chromatography: merge second time enzymolysis solution, filter, concentrated, by column chromatography, adsorbing with macroporous adsorbent resin, is colourless with washed with de-ionized water resin to flowing liquid, then is the ethanolic soln wash-out of 15-20% by concentration, collects elutriant;
7) dry: elutriant to be concentrated, obtains the Geniposide of paste, then obtain Geniposide by drying.
2. a kind of method extracting Geniposide from cape jasmine according to claim 1, is characterized in that: step 1) described in immersion, the time is 15-24 hour.
3. a kind of method extracting Geniposide from cape jasmine according to claim 1, it is characterized in that: step 3) described in pectin-cellulose prozyme, for activity be 1-3 ten thousand activity unit/gram the liquid pectin-fiber composite enzyme of solid-state or 1-3 ten thousand activity units/milliliter.
4. a kind of method extracting Geniposide from cape jasmine according to claim 1, is characterized in that: step 6) described in macroreticular resin be D101 type, DA201 type.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101029066A (en) * | 2007-04-13 | 2007-09-05 | 桂林莱茵生物科技股份有限公司 | Method for extracting genipin and geniposide from gardenia jasminoides |
| CN102432651A (en) * | 2011-11-25 | 2012-05-02 | 威海天泓农业科技有限公司 | Preparation method of geniposide |
| CN103788152A (en) * | 2012-10-26 | 2014-05-14 | 湖北老龙洞杜仲开发有限公司 | Method for preparing geniposide in eucommia leaf |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101029066A (en) * | 2007-04-13 | 2007-09-05 | 桂林莱茵生物科技股份有限公司 | Method for extracting genipin and geniposide from gardenia jasminoides |
| CN102432651A (en) * | 2011-11-25 | 2012-05-02 | 威海天泓农业科技有限公司 | Preparation method of geniposide |
| CN103788152A (en) * | 2012-10-26 | 2014-05-14 | 湖北老龙洞杜仲开发有限公司 | Method for preparing geniposide in eucommia leaf |
Non-Patent Citations (1)
| Title |
|---|
| 赵超 等: "栀子中栀子甙的提取工艺研究", 《河南大学学报（医学版）》 * |
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