CN1441030A - Method of extracting rosemary as matural antioxidant - Google Patents
Method of extracting rosemary as matural antioxidant Download PDFInfo
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- CN1441030A CN1441030A CN03111866A CN03111866A CN1441030A CN 1441030 A CN1441030 A CN 1441030A CN 03111866 A CN03111866 A CN 03111866A CN 03111866 A CN03111866 A CN 03111866A CN 1441030 A CN1441030 A CN 1441030A
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- rosemary
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The present invention relates to method of extracting rosemary natural antioxidant from rosemary plant. The extraction process incldues distilling fresh rosemary plant to obtain resemary oil and material containing resemary antioxidant; crushing the material and adding food level organic solvent in a diffuser to extract rosemary leaching liquid; concentrating the resemary leaching liquid, supercritical extracting and high pressure separation to obtain extractive liquid; recovering solvent; spray or freeze drying to obtain yellowish antioxidant product. The said process obtains rosemary oil and antioxidant separately and has high yield and quality of antioxidant product.
Description
Technical field:
The present invention relates to a kind of method of from plant, extracting antioxidant, particularly utilize solvent extraction and supercritical CO
2The extraction phase combination, the method for extraction rosemary natural anti-oxidant from rosemary plant.
Background technology:
In technique known, be raw material production essential oil and antioxidant with Rosmarinus officinalis, domestic disclosed 5 patented technologies that have, the Technology of its each patent is mainly: 1, adopt the shady rosemary plant of doing, directly utilize supercritical CO
2Extract, get the mixed extraction of essential oil and antioxidant; 2, adopt supercritical CO
2The crude extract that back extraction extracts with different solvents gets essential oil and antioxidant.3, adopt medicinal extract evaporation essential oil earlier after different solvents extracts, utilize again different solvents from resistates, extract antioxidant.4, employing is carried out cell pulverization to former plant, adds different solvents, utilizes membrane sepn and infiltration technology to extract.5, adopt two-step process be distill earlier essential oil, then with different solvents extract decolour antioxidant product.And the external disclosed patent such as the U.S. mainly are the crude extracts that extracts with different solvents, handle directly adding edible oil of back through decolouring, through distilling to such an extent that contain the edible oil of rosemary antioxidant.
There is following shortcoming in various degree in comprehensive above-mentioned several rosemary plant extraction processes: 1, all be to extract with the shady former plant that does, easily cause the loss of effective constituent essential oil or antioxidant, and be unfavorable for peasant's production operation.2, technology adopts essential oil and antioxidant mixed extraction mostly, and the antioxidant product peculiar smell that obtains is big, of poor quality, is difficult to be fit to food and adds application.3, because of using different solvents to extract, solvent-oil ratio is big, and is residual many in the product, and contains non-food grade solvent in the solvent that uses, and do not meet the food service industry requirement.4, directly from former plant, extract pressure height, technical requirements harshness, difficult control with overcritical; And need big volumetrical extraction kettle, and the equipment making difficulty is big, and correlation technique is still immature, and disposable having high input, and is not suitable for large-scale industrialization production.5, add activated carbon decolorizing in process of production, easily adsorb effective constituent, influence product yield.Therefore, all exist in various degree from said extracted technology itself and to apply difficulty, shortcomings such as the big or poor product quality of suitability for industrialized production difficulty still really are not used for scale operation to these Technologies at present.So rosemary natural anti-oxidant still mainly from Japan, American-European import, and costs an arm and a leg on the China market, directly influences and restricting the application of this product.
Summary of the invention:
The purpose of this invention is to provide a kind ofly reduce technical process, unit operation is simple, yield is high, quality is good, production cost is low, be convenient to the method for extracting rosemary natural anti-oxidant from rosemary plant of large-scale production.
Realize that the production method that purpose of the present invention is taked mainly comprises following processing step:
One, directly adopts the bright grass of Rosmarinus officinalis to obtain rosemary ethereal oil and contain the raw material of rosemary antioxidant by wet distillation;
The raw material of two, will be not shady not dried rosemary antioxidant carries out coarse reduction or chopping;
Three, the raw material of the rosemary antioxidant after will pulverizing or shred adds the food grade organic solvent, and adopts the mode that gradually reduces solvent load, with 1:
Four, 5 to 1: 3 mixed is carried out the pump circulation refluxing extraction in extraction unit, extracts to obtain the rosemary antioxidant vat liquor for 2-3 time;
Five, concentrate vat liquor, reclaim solvent and get medicinal extract;
Six, medicinal extract is squeezed in the extraction kettle with pump, the extraction kettle loading amount is 20%～60%, carries out supercritical extraction, high pressure separate extraction liquid, remove colloid, pigment and remaining light constituent trace essential oil etc.;
Seven, extraction liquid is reclaimed solvent after, the spraying or lyophilize get faint yellow antioxidant finished product.
Organic solvent among the described step c is the mixture of food grade organic solvents such as ethanol, ethyl acetate or multiple solvent, and the Heating temperature during refluxing extraction is 30 ℃～80 ℃.
Temperature is controlled at 40 ℃～55 ℃ in the described step e, and pressure-controlling is at 15～35Mpa, and the extraction time is 2～4 hours.
In the described step F, if adopt 110 ℃～140 ℃ of the dry control of spray thing inlet temperatures, 75 ℃～95 ℃ of temperature outs.Answer controlled temperature at-30 ℃～-60 ℃ if adopt lyophilize.
Carry out the extraction of rosemary natural anti-oxidant according to the method described above, its operational path is short, and unit operation simply saves time, and production cost is low, reduces the heating number of times and the heat-up time of material simultaneously, good product quality.Because essential oil and antioxidant are separately to extract, and do not contain essential oil in the medicinal extract, obtain the antioxidant product free from extraneous odour, quality is good, yield is high.In the present invention, directly extract essential oil with bright grass, the yield height, former plant is not shady to do or is exposed to the sun, effective constituent is destroyed few, is convenient to the chemurgy operation, utilizes the raw material of the rosemary antioxidant that does not dry in the shade directly to pulverize, be not exposed to the sun or dry in the shade, can reduce loss of effective components, antioxidant product yield height; Only adopt the food grade solvent in solvent extraction, it is few to extract solvent load, and meets edible demand; At supercritical CO
2In the extraction, supercritical extraction pressure is low, and is liquid feeding, need not open the extraction kettle charging, saving of work and time; And do not require jumbo extraction kettle volume, can significantly reduce facility investment, reduce running expense.Therefore processing step of the present invention is realistic, is convenient to industrial scale production, helps the widespread use of natural additive for foodstuff in food service industry.
Embodiment:
Embodiment 1
Take by weighing 100 kilograms of Rosmarinus officinaliss aquatic foods grass, got essential oil 754 grams in 2～4 hours with wet distillation, it is standby that the raw material that contains antioxidant behind the extraction essential oil is carried out coarse reduction.The raw material that contains antioxidant after pulverizing is put in the extraction unit for 100 kilograms, adding content is 95% alcohol solvent, ratio according to material, solvent is respectively and carried out the pump circulation refluxing extraction in 1: 5～1: 33 times, leach vat liquor, solvent is reclaimed in vacuum distilling, get 35 kilograms of brown medicinal extract, this medicinal extract is squeezed into supercritical extraction reactor, carry out supercritical CO with pump
2Extraction control pressure 30-35Mpa, 40 ℃-55 ℃ of temperature extracted 4 hours, high pressure separate 25 kilograms of extraction liquids, extraction liquid is carried out spraying drying gets 7.8 kilograms of yellow finished products, yield is 7.8%.
Embodiment 2
Repeat the technological process of embodiment 1, add entrainment agent 95% ethanol when carrying out supercritical extraction, input is 10 liters/hour, and behind the recovery solvent, the result gets 10.1 kilograms of spraying drying pale yellow powders, and yield is 10.1%.
Embodiment 3
Repeat the technological process of embodiment 1, add entrainment agent 95% ethanol when carrying out supercritical extraction, input is 10 liters/hour, and extracting pressure is reduced to 15-32Mpa, spraying drying behind the recovery solvent, and the result gets 9.8 kilograms of spraying drying pale yellow powders, and yield is 9.8%
Embodiment 4
Repeat the technological process of embodiment 1, only change last spraying drying into lyophilize, control condition is-45 ℃ and gets 10.6 kilograms of faint yellow lyophilized powders that yield is 10.6, illustrates to utilize freeze drying technology to obtain to such an extent that product yield is slightly high.
Claims (4)
1, a kind of method of extracting rosemary natural anti-oxidant, it is characterized in that: the production method of rosemary natural anti-oxidant comprises the steps:
A, directly obtain rosemary ethereal oil and contain the raw material of rosemary antioxidant with wet distillation with the bright grass of Rosmarinus officinalis;
The raw material of B, will be not shady not dried rosemary antioxidant carries out coarse reduction or chopping;
The raw material of C, the rosemary antioxidant after will pulverizing or shred adds the food grade organic solvent, and employing gradually reduces the mode of solvent load, in extraction unit, carry out the pump circulation refluxing extraction with 1: 5 to 1: 3 mixed, extract and obtain the rosemary antioxidant vat liquor for 2-3 time;
D, concentrated vat liquor reclaim solvent and get medicinal extract.
One E, medicinal extract to be squeezed in the extraction kettle with pump, the extraction kettle loading amount is 20%～
2 60%, carry out supercritical extraction, high pressure separate extraction liquid, remove colloid, pigment and remaining light constituent trace essential oil etc.;
F, extraction liquid reclaimed solvent after, spraying or lyophilize get faint yellow finished product.
2, a kind of method of extracting rosemary natural anti-oxidant according to claim 1, it is characterized in that: the organic solvent among the described step C is the mixture of food grade organic solvents such as ethanol, ethyl acetate or multiple solvent, and the Heating temperature during refluxing extraction is 30 ℃～80 ℃.
3, a kind of method of extracting rosemary natural anti-oxidant according to claim 1 is characterized in that: the temperature in the described step e is controlled at 40 ℃～55 ℃, and pressure-controlling is at 15～35Mpa, and the extraction time is 2～4 hours.
4, a kind of method of extracting rosemary natural anti-oxidant according to claim 1 is characterized in that: in the described step F, if adopt 110 ℃～140 ℃ of the dry control of spray thing inlet temperatures, 75 ℃～95 ℃ of temperature outs.If adopting the lyophilize controlled temperature is-30 ℃～-60 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031118666A CN1281709C (en) | 2003-01-20 | 2003-01-20 | Method of extracting rosemary as matural antioxidant |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031118666A CN1281709C (en) | 2003-01-20 | 2003-01-20 | Method of extracting rosemary as matural antioxidant |
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| Publication Number | Publication Date |
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| CN1441030A true CN1441030A (en) | 2003-09-10 |
| CN1281709C CN1281709C (en) | 2006-10-25 |
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| CNB031118666A Expired - Fee Related CN1281709C (en) | 2003-01-20 | 2003-01-20 | Method of extracting rosemary as matural antioxidant |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102199092A (en) * | 2010-03-26 | 2011-09-28 | 禹州市森源本草天然产物有限公司 | Production technology for acquiring two antioxidant agents from Rosmarinus officinalis L. |
| CN101638580B (en) * | 2009-08-26 | 2012-08-08 | 广东省食品工业研究所 | Method for preparing rosemary natural anti-oxidant |
| CN103834475A (en) * | 2014-04-02 | 2014-06-04 | 贵州红星发展都匀绿友有限责任公司 | Room-temperature gradient extraction of antioxidant from rosmarinus officinalis |
| CN104357060A (en) * | 2014-10-23 | 2015-02-18 | 浙江师范大学 | Preparation method for rubus pungens source antioxidant |
| CN111869810A (en) * | 2020-07-23 | 2020-11-03 | 贵州省蚕业研究所(贵州省辣椒研究所) | Natural antioxidant and preparation method thereof |
-
2003
- 2003-01-20 CN CNB031118666A patent/CN1281709C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101638580B (en) * | 2009-08-26 | 2012-08-08 | 广东省食品工业研究所 | Method for preparing rosemary natural anti-oxidant |
| CN102199092A (en) * | 2010-03-26 | 2011-09-28 | 禹州市森源本草天然产物有限公司 | Production technology for acquiring two antioxidant agents from Rosmarinus officinalis L. |
| CN103834475A (en) * | 2014-04-02 | 2014-06-04 | 贵州红星发展都匀绿友有限责任公司 | Room-temperature gradient extraction of antioxidant from rosmarinus officinalis |
| CN104357060A (en) * | 2014-10-23 | 2015-02-18 | 浙江师范大学 | Preparation method for rubus pungens source antioxidant |
| CN104357060B (en) * | 2014-10-23 | 2016-06-29 | 浙江师范大学 | The preparation method of flowering raspberry source antioxidant |
| CN111869810A (en) * | 2020-07-23 | 2020-11-03 | 贵州省蚕业研究所(贵州省辣椒研究所) | Natural antioxidant and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN1281709C (en) | 2006-10-25 |
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