CN103087129A - Method for extracting geniposide from gardenia yellow pigment waste liquor - Google Patents
Method for extracting geniposide from gardenia yellow pigment waste liquor Download PDFInfo
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Abstract
The invention discloses a method for extracting geniposide from gardenia yellow pigment waste liquor, which mainly comprises the following steps: concentrating gardenia yellow pigment waste liquor used as a raw material through a reverse osmosis membrane, extracting with isobutanol, decolorizing with active carbon, concentrating, performing crystallization purification twice, and finally drying. The invention can solve the waste problem that the gardenia effective component can not be economically and effectively recovered from the gardenia yellow pigment producing waste liquor in an environment-friendly way.
Description
Technical field
The present invention relates to Chinese medicine liquid waste disposal technique field, particularly a kind of from the Gardenia Yellow waste liquid method of extraction jasminoidin.
Background technology
Cape jasmine for another name Yellow Fructus Gardeniae, mountain Cape jasmine, white toad, is the fruit of madder wort cape jasmine.At present, the fruit of cape jasmine is traditional Chinese medicine, the l that belongs to Ministry of Health's promulgation criticizes the medicine-food two-purpose resource, has the effects such as the liver of protecting, cholagogic, step-down, calmness, hemostasis, detumescence, is usually used in treating the diseases such as icterohepatitis, sprain and contusion, hypertension, diabetes at tcm clinical practice.The effective constituent of cape jasmine mainly contains the iridoids such as Gardenia Yellow, jasminoidin.Wherein jasminoidin has multiple use, through the fermentation of different condition, can make natural edible coloring agent gardenia blue and gardenia red, is also simultaneously the material medicine of the diseases such as treatment cardiovascular and cerebrovascular, liver and gall and diabetes.
Gardenia Yellow is also the main effective constituent of cape jasmine, but when extract Gardenia Yellow from cape jasmine after, as adopt Chinese patent application " a kind of extracting high-purity gardenia yellow pigment by membrane separation and purification technology novel method " (publication number: CN101659794A, open day on March 3rd, 2010) technology, the waste liquid that produces in membrane separating method still contains a large amount of jasminoidin effective constituent, if just be used as general waste liquid discard processing, not only can pollute local environment, also caused certain financial loss, the technology of producing the waste liquid efficient recovery cape jasmine effective constituent of yellow pigment from membrane sepn is not yet arranged a few days ago.
Summary of the invention
The invention provides a kind of from the Gardenia Yellow waste liquid method of extraction jasminoidin, mainly solve fail from produce the Gardenia Yellow waste liquid economy, environmental protection, effectively reclaim cape jasmine effective constituent and wasting problem.
Technical scheme of the present invention is: this method that extracts jasminoidin from the Gardenia Yellow waste liquid comprises the following steps:
(1) the Gardenia Yellow waste liquid is concentrated: to adopt the method waste liquid of membrane sepn purification Gardenia Yellow as raw material by after flooding, adopt reverse osmosis membrane that the Gardenia Yellow waste liquid is concentrated, thickening temperature is controlled at 40～50 ℃, concentrated pressure-controlling is at 2.0～3.0Mpa, being concentrated into relative density is 1.0～1.20, obtains Gardenia Yellow waste liquid concentrated solution;
(2) extraction of jasminoidin: add isopropylcarbinol to stir the Gardenia Yellow waste liquid concentrated solution that obtains and carry out 2～4 extractions, combining extraction liquid, when adding isopropylcarbinol, each extraction regulates its pH value to 8～12, standing 30～60 minutes of each extraction, the volume that adds that at every turn extracts isopropylcarbinol is 1～5 times of Gardenia Yellow waste liquid concentrated solution volume;
(3) the decolouring removal of impurities of jasminoidin extraction liquid: the extraction liquid that merging is obtained decolours with gac and obtains the jasminoidin destainer;
(4) the jasminoidin destainer is concentrated: the jasminoidin destainer is carried out vacuum concentration to relative density and be 1.0～1.20 jasminoidin decolouring concentrated solution at 40～70 ℃ of temperature;
(5) the preliminary crystallization of jasminoidin: add methyl esters to separate out the jasminoidin crystal at jasminoidin decolouring concentrated solution;
(6) dissolution filter of jasminoidin crystal: the jasminoidin crystal is added acetic acid ethyl dissolution, then filter, collect filtrate;
(7) recrystallization of jasminoidin: the filtrate that obtains is carried out vacuum concentration to relative density at 40～70 ℃ of temperature be 1.0～1.20 jasminoidin concentrated solution, then through standing crystallization, filter and obtain the jasminoidin crystal;
(8) drying: the jasminoidin crystal that obtains is carried out drying.
In technique scheme, preferred scheme is that what described reverse osmosis membrane adopted is composite membrane.
Owing to having adopted technique scheme, the present invention compared with prior art has following beneficial effect:
1. a kind of method that extracts jasminoidin from the Gardenia Yellow waste liquid is provided, has effectively improved the raw-material utilization ratio of cape jasmine;
2. the yield that is extraction jasminoidin the Gardenia Yellow waste liquid of 10---12% from Determination of Gardenoside is 50～70%; The jasminoidin purity that obtains reaches more than 98%;
3. all method materials of the present invention are all recyclable, and environment is not had a negative impact.And the remaining water solvent only of the Gardenia Yellow waste liquid after processing through present technique, water used when this water solvent can be used as from cape jasmine starting material flooding Gardenia Yellow, thus reach the zero release of industrial effluent, saved simultaneously process water;
4. one ton of Determination of Gardenoside of every processing is 10---12% Gardenia Yellow waste liquid, and its production cost is 40～70 yuan.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described further.
Embodiment 1
(1) the Gardenia Yellow waste liquid is concentrated: take by adopting the waste liquid as 10% of Determination of Gardenoside after membrane sepn purification Gardenia Yellow as raw material after flooding, adopt reverse osmosis membrane that the Gardenia Yellow waste liquid is concentrated, thickening temperature is controlled at 40 ℃, concentrated pressure-controlling is at 2.0Mpa, being concentrated into relative density is 1.0, obtains Gardenia Yellow waste liquid concentrated solution;
(2) extraction of jasminoidin: add isopropylcarbinol to stir the Gardenia Yellow waste liquid concentrated solution that obtains and carry out 2 extractions, combining extraction liquid, when adding isopropylcarbinol, each extraction regulates its pH value to 8, standing 30 minutes of each extraction, the volume that adds that at every turn extracts isopropylcarbinol is 1 times of Gardenia Yellow waste liquid concentrated solution volume;
(3) the decolouring removal of impurities of jasminoidin extraction liquid: the extraction liquid that merging is obtained decolours with gac and obtains the jasminoidin destainer;
(4) the jasminoidin destainer is concentrated: the jasminoidin destainer is carried out vacuum concentration to relative density and be 1.0 jasminoidin decolouring concentrated solution at 40 ℃ of temperature;
(5) the preliminary crystallization of jasminoidin: add methyl esters to separate out the jasminoidin crystal at jasminoidin decolouring concentrated solution;
(6) dissolution filter of jasminoidin crystal: the jasminoidin crystal is added acetic acid ethyl dissolution, then filter, collect filtrate;
(7) recrystallization of jasminoidin: the filtrate that obtains is carried out vacuum concentration to relative density at 40 ℃ of temperature be 1.0 jasminoidin concentrated solution, then through standing crystallization, filter and obtain the jasminoidin crystal;
(8) drying: the jasminoidin crystal that obtains is carried out drying.
In technique scheme, what described reverse osmosis membrane adopted is composite membrane.
Owing to having adopted technique scheme, the present invention compared with prior art has following beneficial effect:
1, provide a kind of method that extracts jasminoidin from the Gardenia Yellow waste liquid, effectively improved the raw-material utilization ratio of cape jasmine;
2, the yield that is extraction jasminoidin 10% Gardenia Yellow waste liquid from Determination of Gardenoside is 50%; The jasminoidin purity that obtains reaches 98%;
3, all method materials of the present invention are all recyclable, and environment is not had a negative impact.And the remaining aqueous solvent only of the Gardenia Yellow waste liquid after processing through present technique, water used when this water solvent can be used as from cape jasmine starting material flooding Gardenia Yellow, thus reach the zero release of industrial effluent, saved simultaneously process water;
4, one ton of Determination of Gardenoside of every processing is 10% Gardenia Yellow waste liquid, and its production cost is 40 yuan.
Embodiment 2
(1) the Gardenia Yellow waste liquid is concentrated: take by adopting the waste liquid as 1% of Determination of Gardenoside after membrane sepn purification Gardenia Yellow as raw material after flooding, adopt reverse osmosis membrane that the Gardenia Yellow waste liquid is concentrated, thickening temperature is controlled at 45 ℃, concentrated pressure-controlling is at 2.5Mpa, being concentrated into relative density is 1.10, obtains Gardenia Yellow waste liquid concentrated solution;
(2) extraction of jasminoidin: add isopropylcarbinol to stir the Gardenia Yellow waste liquid concentrated solution that obtains and carry out 3 extractions, combining extraction liquid, when adding isopropylcarbinol, each extraction regulates its pH value to 10, standing 45 minutes of each extraction, the volume that adds that at every turn extracts isopropylcarbinol is 3 times of Gardenia Yellow waste liquid concentrated solution volume;
(3) the decolouring removal of impurities of jasminoidin extraction liquid: the extraction liquid that merging is obtained decolours with gac and obtains the jasminoidin destainer;
(4) the jasminoidin destainer is concentrated: the jasminoidin destainer is carried out vacuum concentration to relative density and be 1.10 jasminoidin decolouring concentrated solution at 55 ℃ of temperature;
(5) the preliminary crystallization of jasminoidin: add methyl esters to separate out the jasminoidin crystal at jasminoidin decolouring concentrated solution;
(6) dissolution filter of jasminoidin crystal: the jasminoidin crystal is added acetic acid ethyl dissolution, then filter, collect filtrate;
(7) recrystallization of jasminoidin: the filtrate that obtains is carried out vacuum concentration to relative density at 55 ℃ of temperature be 1.10 jasminoidin concentrated solution, then through standing crystallization, filter and obtain the jasminoidin crystal;
(8) drying: the jasminoidin crystal that obtains is carried out drying.
In technique scheme, what described reverse osmosis membrane adopted is composite membrane.
Owing to having adopted technique scheme, the present invention compared with prior art has following beneficial effect:
1, provide a kind of method that extracts jasminoidin from the Gardenia Yellow waste liquid, effectively improved the raw-material utilization ratio of cape jasmine;
2, the yield that is extraction jasminoidin 11% Gardenia Yellow waste liquid from Determination of Gardenoside is 65%; The jasminoidin purity that obtains reaches 98.4%;
3, all method materials of the present invention are all recyclable, and environment is not had a negative impact.And the remaining water solvent only of the Gardenia Yellow waste liquid after processing through present technique, water used when this water solvent can be used as from cape jasmine starting material flooding Gardenia Yellow, thus reach the zero release of industrial effluent, saved simultaneously process water;
4, one ton of Determination of Gardenoside of every processing is 11% Gardenia Yellow waste liquid, and its production cost is 55 yuan.
Embodiment 3
(1) the Gardenia Yellow waste liquid is concentrated: take by adopting the waste liquid as 12% of Determination of Gardenoside after membrane sepn purification Gardenia Yellow as raw material after flooding, adopt reverse osmosis membrane that the Gardenia Yellow waste liquid is concentrated, thickening temperature is controlled at 50 ℃, concentrated pressure-controlling is at 3.0Mpa, being concentrated into relative density is 1.20, obtains Gardenia Yellow waste liquid concentrated solution;
(2) extraction of jasminoidin: add isopropylcarbinol to stir the Gardenia Yellow waste liquid concentrated solution that obtains and carry out 4 extractions, combining extraction liquid, when adding isopropylcarbinol, each extraction regulates its pH value to 12, standing 60 minutes of each extraction, the volume that adds that at every turn extracts isopropylcarbinol is 5 times of Gardenia Yellow waste liquid concentrated solution volume;
(3) the decolouring removal of impurities of jasminoidin extraction liquid: the extraction liquid that merging is obtained decolours with gac and obtains the jasminoidin destainer;
(4) the jasminoidin destainer is concentrated: the jasminoidin destainer is carried out vacuum concentration to relative density and be 1.20 jasminoidin decolouring concentrated solution at 70 ℃ of temperature;
(5) the preliminary crystallization of jasminoidin: add methyl esters to separate out the jasminoidin crystal at jasminoidin decolouring concentrated solution;
(6) dissolution filter of jasminoidin crystal: the jasminoidin crystal is added acetic acid ethyl dissolution, then filter, collect filtrate;
(7) recrystallization of jasminoidin: the filtrate that obtains is carried out vacuum concentration to relative density at 70 ℃ of temperature be 1.20 jasminoidin concentrated solution, then through standing crystallization, filter and obtain the jasminoidin crystal;
(8) drying: the jasminoidin crystal that obtains is carried out drying.
In technique scheme, what described reverse osmosis membrane adopted is composite membrane.
Owing to having adopted technique scheme, the present invention compared with prior art has following beneficial effect:
1, provide a kind of method that extracts jasminoidin from the Gardenia Yellow waste liquid, effectively improved the raw-material utilization ratio of cape jasmine;
2, the yield that is extraction jasminoidin 12% Gardenia Yellow waste liquid from Determination of Gardenoside is 70%; The jasminoidin purity that obtains reaches 98.7%;
3, all method materials of the present invention are all recyclable, and environment is not had a negative impact.And the remaining water solvent only of the Gardenia Yellow waste liquid after processing through present technique, water used when this water solvent can be used as from cape jasmine starting material flooding Gardenia Yellow, thus reach the zero release of industrial effluent, saved simultaneously process water;
4, one ton of Determination of Gardenoside of every processing is 12% Gardenia Yellow waste liquid, and its production cost is 70 yuan.
Claims (2)
- One kind from the Gardenia Yellow waste liquid extraction jasminoidin method, it is characterized in that comprising the following steps:(1) the Gardenia Yellow waste liquid is concentrated: to adopt the method waste liquid of membrane sepn purification Gardenia Yellow as raw material by after flooding, adopt reverse osmosis membrane that the Gardenia Yellow waste liquid is concentrated, thickening temperature is controlled at 40～50 ℃, concentrated pressure-controlling is at 2.0～3.0Mpa, being concentrated into relative density is 1.0～1.20, obtains Gardenia Yellow waste liquid concentrated solution;(2) extraction of jasminoidin: add isopropylcarbinol to stir the Gardenia Yellow waste liquid concentrated solution that obtains and carry out 2～4 extractions, combining extraction liquid, when adding isopropylcarbinol, each extraction regulates its pH value to 8～12, standing 30～60 minutes of each extraction, the volume that adds that at every turn extracts isopropylcarbinol is 1～5 times of Gardenia Yellow waste liquid concentrated solution volume;(3) the decolouring removal of impurities of jasminoidin extraction liquid: the extraction liquid that merging is obtained decolours with gac and obtains the jasminoidin destainer;(4) the jasminoidin destainer is concentrated: the jasminoidin destainer is carried out vacuum concentration to relative density and be 1.0～1.20 jasminoidin decolouring concentrated solution at 40～70 ℃ of temperature;(5) the preliminary crystallization of jasminoidin: add methyl esters to separate out the jasminoidin crystal at jasminoidin decolouring concentrated solution;(6) dissolution filter of jasminoidin crystal: the jasminoidin crystal is added acetic acid ethyl dissolution, then filter, collect filtrate;(7) recrystallization of jasminoidin: the filtrate that obtains is carried out vacuum concentration to relative density at 40～70 ℃ of temperature be 1.0～1.20 jasminoidin concentrated solution, then through standing crystallization, filter and obtain the jasminoidin crystal;(8) drying: the jasminoidin crystal that obtains is carried out drying.
- According to claim 1 a kind of from the Gardenia Yellow waste liquid method of extraction jasminoidin, it is characterized in that: what described reverse osmosis membrane adopted is composite membrane.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103525883A (en) * | 2013-10-23 | 2014-01-22 | 宁德师范学院 | Method for preparing high-color-value gardenia blue pigment |
| CN104356184A (en) * | 2014-12-03 | 2015-02-18 | 邵阳学院 | Method for separating and purifying geniposide by using isopropanol-salt double-aqueous-phase system |
| CN107075271A (en) * | 2014-10-30 | 2017-08-18 | 三荣源有限公司 | By geniposide, Geniposide or both method removed |
| CN108794551A (en) * | 2018-08-28 | 2018-11-13 | 郑州中科新兴产业技术研究院 | A method of preparing high-purity gardenoside from gardenia yellow pigment waste liquor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103525883A (en) * | 2013-10-23 | 2014-01-22 | 宁德师范学院 | Method for preparing high-color-value gardenia blue pigment |
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| CN107075271B (en) * | 2014-10-30 | 2021-05-28 | 三荣源有限公司 | Method for removing geniposide, genipin or both |
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| CN104356184B (en) * | 2014-12-03 | 2016-07-27 | 邵阳学院 | A kind of method of isopropanol-isolated and purified jasminoidin of salt double-aqueous phase system |
| CN108794551A (en) * | 2018-08-28 | 2018-11-13 | 郑州中科新兴产业技术研究院 | A method of preparing high-purity gardenoside from gardenia yellow pigment waste liquor |
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