CN105037463B - A kind of method that geniposide is extracted from cape jasmine - Google Patents
A kind of method that geniposide is extracted from cape jasmine Download PDFInfo
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- CN105037463B CN105037463B CN201510541584.8A CN201510541584A CN105037463B CN 105037463 B CN105037463 B CN 105037463B CN 201510541584 A CN201510541584 A CN 201510541584A CN 105037463 B CN105037463 B CN 105037463B
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- geniposide
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Abstract
The invention discloses a kind of method that geniposide is extracted from cape jasmine, comprise the steps:Immersion treatment, Feedstock treating, digest, deoil for the first time, second enzymolysis, column chromatography, drying.The present invention first using enzyme extraction vegetable fat, is separated with non-oil component by oily to oily different with the affinity difference and profit proportion of water using non-oil component, adds product yield and improve recovery rate.
Description
Technical field
The present invention relates to the extracting method of biological technical field, specifically a kind of side that geniposide is extracted from cape jasmine
Method.
Background technology
Mast is Rubiaceae (Rubiaceae) plant mast (Gardenia jasminoides Ellis) fruit, long
Ellipse or ellipse, in peony or yellowish red color, the first batch of medicine-food two-purpose resource of Wei Zishu Ministry of Public Health promulgation, is in tradition
Medicine.Mast has purging intense heat relieving restlessness, and clearing heat and promoting diuresis, removing pattogenic heat from the blood and toxic material from the body, lidan liver, decompression, sterilize anti-inflammatory, the work(of externally used detumescence analgesic
Effect.It is mainly used in treating pyreticosis, Jaundice Jaundice, bruise, hypertension, diabetes etc. on tcm clinical practice.Chemistry in mast
Composition is a lot, wherein mainly have crocin, the iridoids such as crocetin (Ichietal) and geniposide (Geniposide)
Compound, its Geniposidic are its principle active components.
Geniposide is a kind of Iridoidglucoside, soluble in water.Geniposide can be by R- glycoside enzyme hydrolysis
For Geniposide.Modern study shows, geniposide to digestive system, cardiovascular system and in general the nervous system disease have significantly
Curative effect, in addition, geniposide also has certain anti-inflammatory and treats the effect of soft tissue injury.Geniposide in addition to medicinal,
Also it is widely used in other fields, such as can be used as plant promoter, biological detection agent, is that a kind of important biology is living
Property material.It is widely used in medical treatment, field of health care products.
Geniposide is primarily present in the natural plants such as mast, the bark of eucommia, is the desirable feedstock for extracting geniposide, domestic
There is recovery rate is not high, product purity is low, energy resource consumption is big, largely uses organic solvent, useless in existing extraction process scheme
The problems such as water is big.
The content of the invention
It is an object of the invention to provide a kind of method that geniposide is extracted from cape jasmine, has technique simple, is adapted to life
Produce, the advantages such as production cost is low.
The present invention is achieved through the following technical solutions, and is specifically comprised the following steps：
1) immersion treatment：Cape jasmine is loaded into woven bag, ties mouth, is placed in pond, pond topped up with water, and on pond
Weight in pressure, immersion；
2) Feedstock treating：The cape jasmine that step 1) is obtained crushes or crushed, and adds pure equivalent to 2-3 times of weight of raw material
Water, 50-60 DEG C of maintenance 5-10 minute is heated to, obtains paste serous material；
3) digest for the first time：The paste serous material that step 2) is obtained, tune pH are 4-5, add paste serous material 0.05-0.1%
The pectin-cellulose complex enzyme of parts by weight and the mannitol of 0.001 parts by weight carry out digesting 40-60 minutes, obtain first time enzyme
Solve liquid；
4) deoil：The first time enzymolysis liquid that step 3) is obtained, the pure water of 2-3 times of weight is added, is heated to 60-70 DEG C
60-120 minutes are extracted, obtain upper strata oil slick liquid and subnatant, slag mixture, are separated；
5) second of enzymolysis：Subnatant, the slag mixture that step 4) is obtained, it is 4.5 to adjust pH, is added equivalent to mixture
The cellulase of 0.1-0.2% parts by weight carries out digesting 40-60 minutes, obtains second of enzymolysis liquid, is repeated twice；
6) column chromatography：Merge second of enzymolysis liquid, filter, concentration, by column chromatography, inhaled with macroporous absorbent resin
Attached, it is colourless to clean resin to trickle with deionized water, then the ethanol solution for being 15-20% with concentration elutes, and collection is washed
De- liquid；
7) dry：Eluent is concentrated, obtains the geniposide of paste, then by being dried to obtain geniposide.
Immersion described in step 1) of the present invention, time preferred 15-24 hours.
Pectin-cellulose complex enzyme described in step 3), preferably activity are the solid-states of the active units of 1-3 ten thousand/gram (milliliter)
Or liquid pectin-fiber composite enzyme.
The preferred D101 types of macroreticular resin, DA201 types described in step 6).
Compared with prior art, advantages of the present invention：
1st, contain substantial amounts of grease in the plant cell of cape jasmine, mainly by composition for triglycerides compound group into mix
Compound, these greases in the form of elaioleucite and oil body protoplast, in discontinuous graininess, together with granule protein body irregularly
The scattered existence form such as in the cell is present.Existing extracting method, led to after directly the raw materials such as cape jasmine are smashed or crushed
Cross the modes such as water extraction/alcohol extracting, enzymolysis or Microwave Extraction directly to extract, when extraction, the grease in cell can the same time-division
Separate out, the composition such as group and geniposide, genipic acid, pigment containing grease mixes, so as to influence it is follow-up effectively into
The separation divided, add the intractability of process.The present invention is first using enzyme extraction vegetable fat, using non-oil component to oil and water
Affinity difference and profit proportion it is different and separated oily with non-oil component, add product yield and improve recovery rate.
2nd, the present invention is soaked using cape jasmine pond, and cape jasmine is immersed in water, and cape jasmine gradually softens, and moisture enters interior naturally
Portion, beneficial to the separation of vegetable fat, beneficial to subsequently digesting, deoil；Meanwhile cape jasmine is immersed in water, anaerobic bacteria amount reproduction,
Particularly summer when, can souring, pH value can drop to 4 or so, the adjustment pH of convenient process below.
3rd, the present invention first removes cell membrane using pectin-cellulose complex enzyme, discharges the grease in plant cell, adds sweet
Reveal alcohol, osmotic pressure can be kept, beneficial to the release of grease.
4th, the geniposide that the present invention obtains, is detected through HPLC, and more than 98.5%, yield improves content than prior art
25%.
Embodiment
With embodiment, the invention will be further described below, but the invention is not limited in these embodiments.
Embodiment 1：
A kind of method that geniposide is extracted from cape jasmine, specifically comprises the following steps：
1) immersion treatment：Cape jasmine is loaded into woven bag, ties mouth, is placed in pond, pond topped up with water, and on pond
Weight in pressure, soak 15 hours；
2) Feedstock treating：The cape jasmine that step 1) is obtained crushes, and adds the pure water equivalent to 2-3 times of weight of raw material, adds
Hot to 50 DEG C maintain 5 minutes, obtain paste serous material；
3) digest for the first time：The paste serous material that step 2) is obtained, it is 4 to adjust pH, adds the parts by weight of paste serous material 0.05%
Activity be 10,000 active units/gram pectin-cellulose complex enzyme and 0.001 parts by weight mannitol carry out enzymolysis 40 minutes, obtain
To first time enzymolysis liquid；
4) deoil：The first time enzymolysis liquid that step 3) is obtained, the pure water of 2 times of weight is added, be heated to 60 DEG C of extractions
120 minutes, upper strata oil slick liquid and subnatant, slag mixture are obtained, is separated；
5) second of enzymolysis：Subnatant, the slag mixture that step 4) is obtained, it is 4.5 to adjust pH, is added equivalent to mixture
The cellulase of 0.1% parts by weight carries out enzymolysis 60 minutes, obtains second of enzymolysis liquid, is repeated twice；
6) column chromatography：Merge second of enzymolysis liquid, filter, concentration, by column chromatography, entered with D101 type macroporous absorbent resins
Row absorption, it is colourless to clean resin to trickle with deionized water, then is eluted with the ethanol solution that concentration is 20%, and collection is washed
De- liquid；
7) dry：Eluent is concentrated, obtains the geniposide of paste, then by being dried to obtain geniposide, through HPLC
Detection, content 99.1%.
Embodiment 2：
A kind of method that geniposide is extracted from cape jasmine, specifically comprises the following steps：
1) immersion treatment：Cape jasmine is loaded into woven bag, ties mouth, is placed in pond, pond topped up with water, and on pond
Weight in pressure, soak 24 hours；
2) Feedstock treating：The cape jasmine that step 1) is obtained crushes, and adds the pure water equivalent to 2-3 times of weight of raw material, adds
Hot to 60 DEG C maintain 8 minutes, obtain paste serous material；
3) digest for the first time：The paste serous material that step 2) is obtained, it is 4.5 to adjust pH, adds the parts by weight of paste serous material 0.1%
Activity is that the pectin-cellulose complex enzyme of 20,000 active units/milliliter and the mannitol of 0.001 parts by weight carry out enzymolysis 50 minutes,
Obtain first time enzymolysis liquid；
4) deoil：The first time enzymolysis liquid that step 3) is obtained, the pure water of 3 times of weight is added, be heated to 70 DEG C of extractions
60 minutes, upper strata oil slick liquid and subnatant, slag mixture are obtained, is separated；
5) second of enzymolysis：Subnatant, the slag mixture that step 4) is obtained, it is 4.5 to adjust pH, is added equivalent to mixture
The cellulase of 0.15% parts by weight carries out enzymolysis 50 minutes, obtains second of enzymolysis liquid, is repeated twice；
6) column chromatography：Merge second of enzymolysis liquid, filter, concentration, by column chromatography, with DA201 type macroporous absorbent resins
Adsorbed, it is colourless to clean resin to trickle with deionized water, then is eluted with the ethanol solution that concentration is 15%, is collected
Eluent；
7) dry：Eluent is concentrated, obtains the geniposide of paste, then by being dried to obtain geniposide, through HPLC
Detection, content 99.3%.
Embodiment 3：
1) immersion treatment：Cape jasmine is loaded into woven bag, ties mouth, is placed in pond, pond topped up with water, and on pond
Weight in pressure, soak 18 hours；
2) Feedstock treating：The cape jasmine that step 1) is obtained crushes, and adds the pure water equivalent to 2-3 times of weight of raw material, adds
Hot to 55 DEG C maintain 10 minutes, obtain paste serous material；
3) digest for the first time：The paste serous material that step 2) is obtained, it is 5 to adjust pH, adds the parts by weight of paste serous material 0.08%
Activity be 30,000 active units/gram pectin-cellulose complex enzyme and 0.001 parts by weight mannitol carry out enzymolysis 60 minutes, obtain
To first time enzymolysis liquid；
4) deoil：The first time enzymolysis liquid that step 3) is obtained, the pure water of 2 times of weight is added, be heated to 65 DEG C of extractions
100 minutes, upper strata oil slick liquid and subnatant, slag mixture are obtained, is separated；
5) second of enzymolysis：Subnatant, the slag mixture that step 4) is obtained, it is 4.5 to adjust pH, is added equivalent to mixture
The cellulase of 0.2% parts by weight carries out enzymolysis 40 minutes, obtains second of enzymolysis liquid, is repeated twice；
6) column chromatography：Merge second of enzymolysis liquid, filter, concentration, by column chromatography, entered with D101 type macroporous absorbent resins
Row absorption, it is colourless to clean resin to trickle with deionized water, then is eluted with the ethanol solution that concentration is 20%, and collection is washed
De- liquid；
7) dry：Eluent is concentrated, obtains the geniposide of paste, then by being dried to obtain geniposide, through HPLC
Detection, content 98.9%.
Claims (4)
- A kind of 1. method that geniposide is extracted from cape jasmine, it is characterised in that comprise the following steps：1) immersion treatment：Cape jasmine is loaded into woven bag, ties mouth, is placed in pond, pond topped up with water, and on pond in face pressure Weight, immersion；2) Feedstock treating：The cape jasmine that step 1) is obtained crushes or crushed, and adds the pure water equivalent to 2-3 times of weight of raw material, 50-60 DEG C of maintenance 5-10 minute is heated to, obtains paste serous material；3) digest for the first time：The paste serous material that step 2) is obtained, tune pH are 4-5, add paste serous material 0.05-0.1% weight The pectin-cellulose complex enzyme of part and the mannitol of 0.001 parts by weight carry out digesting 40-60 minutes, obtain first time enzymolysis liquid；4) deoil：The first time enzymolysis liquid that step 3) is obtained, the pure water of 2-3 times of weight is added, be heated to 60-70 DEG C of extraction 60-120 minutes, upper strata oil slick liquid and subnatant, slag mixture are obtained, separated；5) second of enzymolysis：Subnatant, the slag mixture that step 4) is obtained, it is 4.5 to adjust pH, is added equivalent to mixture 0.1- The cellulase of 0.2% parts by weight carries out digesting 40-60 minutes, obtains second of enzymolysis liquid, is repeated twice；6) column chromatography：Merge second of enzymolysis liquid, filter, concentration, by column chromatography, adsorbed with macroporous absorbent resin, used It is colourless that deionized water, which cleans resin to trickle, then the ethanol solution for being 15-20% with concentration elutes, and collects eluent；7) dry：Eluent is concentrated, obtains the geniposide of paste, then by being dried to obtain geniposide.
- A kind of 2. method that geniposide is extracted from cape jasmine according to claim 1, it is characterised in that：Step 1) is described Immersion, the time is 15-24 hours.
- A kind of 3. method that geniposide is extracted from cape jasmine according to claim 1, it is characterised in that：Step 3) is described Pectin-cellulose complex enzyme, for activity be the active units of 1-3 ten thousand/gram solid-state or 1-3 ten thousand active units/milliliter liquid Pectin-fiber composite enzyme.
- A kind of 4. method that geniposide is extracted from cape jasmine according to claim 1, it is characterised in that：Step 6) is described Macroreticular resin for D101 types, DA201 types.
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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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2015
- 2015-08-31 CN CN201510541584.8A patent/CN105037463B/en not_active Expired - Fee Related
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 |
|---|
| 栀子中栀子甙的提取工艺研究;赵超 等;《河南大学学报（医学版）》;20070228;第26卷(第1期);第43-44页 * |
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