CN1316494A - Process for extracting antioxidizing agent and perfume from rosemary - Google Patents
Process for extracting antioxidizing agent and perfume from rosemary Download PDFInfo
- Publication number
- CN1316494A CN1316494A CN00112834A CN00112834A CN1316494A CN 1316494 A CN1316494 A CN 1316494A CN 00112834 A CN00112834 A CN 00112834A CN 00112834 A CN00112834 A CN 00112834A CN 1316494 A CN1316494 A CN 1316494A
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- CN
- China
- Prior art keywords
- antioxidant
- crude extract
- solution
- adopt
- impurity
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 11
- 241001529742 Rosmarinus Species 0.000 title abstract description 5
- 230000003064 anti-oxidating effect Effects 0.000 title abstract 4
- 239000002304 perfume Substances 0.000 title abstract 3
- 239000000126 substance Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000003960 organic solvent Substances 0.000 claims abstract description 9
- 239000012528 membrane Substances 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 241000196324 Embryophyta Species 0.000 claims abstract description 6
- 238000010298 pulverizing process Methods 0.000 claims abstract description 6
- 239000003513 alkali Substances 0.000 claims abstract description 5
- 238000000194 supercritical-fluid extraction Methods 0.000 claims abstract description 4
- 239000003963 antioxidant agent Substances 0.000 claims description 37
- 230000003078 antioxidant effect Effects 0.000 claims description 36
- 239000000287 crude extract Substances 0.000 claims description 27
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 239000012535 impurity Substances 0.000 claims description 17
- 235000013599 spices Nutrition 0.000 claims description 15
- 241001530490 Salvia rosmarinus Species 0.000 claims description 13
- 235000015639 rosmarinus officinalis Nutrition 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000004440 column chromatography Methods 0.000 claims description 8
- 238000005516 engineering process Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000011347 resin Substances 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 8
- 239000003463 adsorbent Substances 0.000 claims description 7
- 238000005374 membrane filtration Methods 0.000 claims description 7
- 238000001223 reverse osmosis Methods 0.000 claims description 7
- 238000000638 solvent extraction Methods 0.000 claims description 7
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 6
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000001913 cellulose Substances 0.000 claims description 6
- 229920002678 cellulose Polymers 0.000 claims description 6
- 239000012141 concentrate Substances 0.000 claims description 6
- 239000001814 pectin Substances 0.000 claims description 6
- 229920001277 pectin Polymers 0.000 claims description 6
- 235000010987 pectin Nutrition 0.000 claims description 6
- 102000004169 proteins and genes Human genes 0.000 claims description 6
- 108090000623 proteins and genes Proteins 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 5
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 235000019439 ethyl acetate Nutrition 0.000 claims description 3
- 150000004676 glycans Chemical class 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 3
- 239000000049 pigment Substances 0.000 claims description 3
- 229920001282 polysaccharide Polymers 0.000 claims description 3
- 239000005017 polysaccharide Substances 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 239000001294 propane Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000000605 extraction Methods 0.000 abstract description 11
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 229910001867 inorganic solvent Inorganic materials 0.000 description 2
- 239000003049 inorganic solvent Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 229910052728 basic metal Inorganic materials 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
Classifications
-
- 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
Landscapes
- Seasonings (AREA)
- Food Preservation Except Freezing, Refrigeration, And Drying (AREA)
Abstract
A process for extracting antioxidizing agent and perfume from rosemary includes such steps as pulverizing fresh ro semary plant by cell pulverizing method to obtain cell tissue substance, immersing in inorganic alkali solution, separating solution from dregs, removing impurites from solution to obtain solution A, neutralizing dregs, drying, extracting in organic solvent, concentrating to obtain B, the membrane filtering, concentrating and drying of A to obtain refined antioxidizing agent, supercritical extraction of B, concentrating and drying to obtain antioxidizing agent and perfume. Its advantages are high extraction efficiency and low cost.
Description
The present invention relates to a kind of production method of from rosemary plant, obtaining antioxidant and spices.
The processing technology of the former plant of Rosmarinus officinalis is mainly divided two portions, and the one, the extraction of Rosmarinus officinalis spices, the 2nd, the extraction separation of antioxidant.At present, obtain the antioxidant in the rosemary plant and the method for spices in the prior art and generally adopt inorganic solvent extraction method, organic solvent extraction method and three kinds of main method of supercritical carbon dioxide extraction method, though the inorganic solvent extraction method has the higher and low advantage of tooling cost of relative yield, but exist but that product purity is not enough, band impurity color, be shortcoming such as peculiar smell, thereby its use range is restricted; Though the organic solvent extraction method has the advantage that technology is simple, investment is less, exist that yield is low, the organic solvent residual height of product, the higher shortcoming of tooling cost; Though and supercritical carbon dioxide process has the low advantage of the organic solvent residual of its product, its production unit is once invested too big, general unable the bearing of domestic enterprise.
The objective of the invention is: the production method of obtaining antioxidant and spices in the Rosmarinus officinalis that provides that a kind of extraction yield is higher, product purity is higher, investment is less, production cost is lower.
The present invention is achieved in that its former plant of Rosmarinus officinalis after will cleaning pulverizes with the cell pulverization method under fresh state, get the cell grade tissue substance, inorganic alkali solution with PH8～12 is to extract solvent impregnated this tissue substance, get the lixiviate mixture, with the lixiviate mixture by centrifugal solid-liquid separate solution and residue, solution part is carried out earlier after neutralization precipitation handles, remove wherein most of pectin through separating technology again, Mierocrystalline cellulose, protein impurities, its surplus solution is the crude extract A that contains antioxidant, gets the crude extract B that mainly contains spices and antioxidant and other impurity after in the residue and dry back is concentrated with organic solvent extraction; Crude extract A is carried out membrane filtration, slough wherein remaining bigger pectin, Mierocrystalline cellulose, protein and other polysaccharide impurity of molecular weight, adjusting membrane pore size can remove pigment and smell substance among the crude extract A, the crude extract A behind the membrane filtration is carried out promptly getting after reverse osmosis or spray method concentrate drying are handled make with extra care antioxidant product; With the super critical extraction of adding entrainment agent crude extract B is handled, entrainment agent can adopt ethanol, methyl alcohol, acetone, acetic ester, methylene dichloride, ethane, propane, water, promptly gets antioxidant and Rosmarinus officinalis spice product after adopting reverse osmosis or spray method concentrate drying to handle again; Also can under normal temperature condition, adopt the macroporous adsorbent resin method to carry out column chromatography for the antioxidant product that from crude extract A, makes and handle, further to remove variegated, peculiar smell and the impurity in its antioxidant; Also can under normal temperature condition, adopt the macroporous adsorbent resin method to carry out column chromatography for the antioxidant product that from crude extract B, makes and handle, or adopt membrane filtering method to handle, further to remove variegated, peculiar smell and the impurity in its antioxidant.
Owing to adopted technique scheme, the present invention adopts the cell pulverization method to make the cell rupture of rosemary plant, various effective ingredients or invalid impurity ooze out, its antioxidant can fully be contacted with the extraction solvent, thereby improved extraction yield greatly, the supercritical methanol technology of Cai Yonging is that plant material is directly handled in the prior art, and the supercritical methanol technology that adopts in the present invention just is used for the processing of crude extract B, therefore its treatment capacity is 1/tens of a direct facture, so the volume of its equipment and also corresponding the significantly reducing of investment, and the present invention adds entrainment agent in supercritical carbon dioxide process, has solved crude extract B at one stroke and has removed peculiar smell, separate spices, obtain the problem of antioxidant; Extract all essential high temperature that adopts of antioxidant in the prior art; and antioxidant oxidation voluntarily easily under hot conditions; in order to obtain high in antioxidants; prior art generally adopts high temperature extraction under the nitrogen protection; thereby increased production cost; and the present invention adopts cytoclasis earlier; increase the solvent contact area; again adopt normal temperature art breading such as membrane sepn supercritical methanol technology, the precipitator method, macroporous resin column chromatography thereafter; effectively compensate the extraction yield loss that high temperature brings, thereby solved extraction yield and this contradiction of oxidation-resistance effectively.Therefore, the present invention compared with prior art has the advantage that extraction yield is higher, product purity is higher, investment is less, production cost is lower.
Embodiments of the invention: the former plant of the Rosmarinus officinalis after will cleaning is crushed to 1～10 order with the cell pulverization method under fresh state, the cell grade tissue substance, be solvent impregnated this tissue substance of extraction with the inorganic alkali solution of PH8～12, mineral alkali can adopt Na
2CO
3, NaHCO
3, NaOH, K
2CO
3, KHCO
3Basic metal such as KOH series weak base formula highly basic or its mixture, steeping process carries out at normal temperatures, tissue substance gets the lixiviate mixture behind dipping, with the lixiviate mixture by centrifugal solid-liquid separate solution and residue, solution part is carried out earlier after neutralization precipitation handles, remove wherein most of pectin through separating technology again, Mierocrystalline cellulose, protein impurities, its surplus solution is the crude extract A that contains antioxidant, after in the residue and dry back concentrated with organic solvent extraction mainly contain the crude extract B of spices and antioxidant and other impurity, crude extract A is carried out membrane filtration, membrane filtration can adopt millipore filtration, the single filtration of ultrafiltration and reverse osmosis or its combination filtration procedure, slough the bigger pectin of molecular weight remaining among the crude extract A, Mierocrystalline cellulose, protein and other polysaccharide impurity, adjusting membrane pore size can remove pigment and smell substance among the crude extract A, the crude extract A behind the membrane filtration is carried out promptly getting after reverse osmosis or spray method concentrate drying are handled make with extra care antioxidant product; With the super critical extraction of adding entrainment agent crude extract B is handled, entrainment agent can adopt ethanol, methyl alcohol, acetone, acetic ester, methylene dichloride, ethane, propane, water, during processing, the operating pressure of its extractor is controlled at 100atm～200atm, its working temperature is controlled between 20 ℃～40 ℃, promptly gets antioxidant and Rosmarinus officinalis spice product after adopting reverse osmosis or spray method concentrate drying to handle again; Also can under normal temperature condition, adopt the macroporous adsorbent resin method to carry out column chromatography for the antioxidant product that from crude extract A, makes and handle, further to remove variegated, peculiar smell and the impurity in its antioxidant; Also can under normal temperature condition, adopt the macroporous adsorbent resin method to carry out column chromatography for the antioxidant product that from crude extract B, makes and handle, or adopt membrane filtering method to handle, further to remove variegated, peculiar smell and the impurity in its antioxidant.When adopting the macroporous adsorbent resin method to carry out the column chromatography processing, its column temperature preferably maintains between 20 ℃～40 ℃, and its organic solvent can adopt methyl alcohol, ethanol, acetone and the aqueous solution thereof or its mixture.
Claims (3)
1, a kind of production method of obtaining antioxidant and spices in the Rosmarinus officinalis, it is characterized in that: the Rosmarinus officinalis after will cleaning is pulverized with the cell pulverization method under fresh state by former plant, get the cell grade tissue substance, inorganic alkali solution with PH8～12 is to extract solvent impregnated this tissue substance, get the lixiviate mixture, with the lixiviate mixture by centrifugal solid-liquid separate solution and residue, solution part is carried out earlier after neutralization precipitation handles, remove wherein most of pectin through separating technology again, Mierocrystalline cellulose, protein impurities, its surplus solution is the crude extract A that contains antioxidant, gets the crude extract B that mainly contains spices and antioxidant and other impurity after in the residue and dry back is concentrated with organic solvent extraction; Crude extract A is carried out membrane filtration, slough wherein remaining bigger pectin, Mierocrystalline cellulose, protein and other polysaccharide impurity of molecular weight, adjusting membrane pore size can remove pigment and smell substance among the crude extract A, the crude extract A behind the membrane filtration is carried out promptly getting after reverse osmosis or spray method concentrate drying are handled make with extra care antioxidant product; With the super critical extraction of adding entrainment agent crude extract B is handled, entrainment agent can adopt ethanol, methyl alcohol, acetone, acetic ester, methylene dichloride, ethane, propane, water, promptly gets antioxidant and Rosmarinus officinalis spice product after adopting reverse osmosis or spray method concentrate drying to handle again.
2, the production method of obtaining antioxidant and spices in the Rosmarinus officinalis according to claim 1, it is characterized in that: also can under normal temperature condition, adopt the macroporous adsorbent resin method to carry out column chromatography for the antioxidant product that from crude extract A, makes and handle, further to remove variegated, peculiar smell and the impurity in its antioxidant.
3, the production method of obtaining antioxidant and spices in the Rosmarinus officinalis according to claim 1, it is characterized in that: also can under normal temperature condition, adopt the macroporous adsorbent resin method to carry out column chromatography for the antioxidant product that from crude extract B, makes and handle, or adopt membrane filtering method to handle, further to remove variegated, peculiar smell and the impurity in its antioxidant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00112834A CN1316494A (en) | 2000-04-06 | 2000-04-06 | Process for extracting antioxidizing agent and perfume from rosemary |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00112834A CN1316494A (en) | 2000-04-06 | 2000-04-06 | Process for extracting antioxidizing agent and perfume from rosemary |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1316494A true CN1316494A (en) | 2001-10-10 |
Family
ID=4582664
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN00112834A Pending CN1316494A (en) | 2000-04-06 | 2000-04-06 | Process for extracting antioxidizing agent and perfume from rosemary |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1316494A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102031116A (en) * | 2010-11-17 | 2011-04-27 | 合肥工业大学科教开发部 | New method for preparing rosemary natural antioxidant |
| CN101744360B (en) * | 2010-01-12 | 2012-05-23 | 广东神农烟科技术有限公司 | Antrodia camphorata extract and cigarette containing antrodia camphorata extract |
| CN103205312A (en) * | 2013-04-12 | 2013-07-17 | 红云红河烟草(集团)有限责任公司 | Preparation method of aromatic wood spice for cigarettes |
| 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 |
| CN103966027A (en) * | 2014-05-15 | 2014-08-06 | 嘉兴市得百科新材料科技有限公司 | Preparation method of compound rosemary extract |
| CN107868701A (en) * | 2017-11-09 | 2018-04-03 | 鹰潭华宝香精有限公司 | The preparation method of apricot extract |
| CN112920043A (en) * | 2021-01-26 | 2021-06-08 | 桂林莱茵生物科技股份有限公司 | Preparation method of carnosic acid with content of more than 99% |
-
2000
- 2000-04-06 CN CN00112834A patent/CN1316494A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101744360B (en) * | 2010-01-12 | 2012-05-23 | 广东神农烟科技术有限公司 | Antrodia camphorata extract and cigarette containing antrodia camphorata extract |
| CN102031116A (en) * | 2010-11-17 | 2011-04-27 | 合肥工业大学科教开发部 | New method for preparing rosemary natural antioxidant |
| CN103205312A (en) * | 2013-04-12 | 2013-07-17 | 红云红河烟草(集团)有限责任公司 | Preparation method of aromatic wood spice for cigarettes |
| 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 |
| CN103966027A (en) * | 2014-05-15 | 2014-08-06 | 嘉兴市得百科新材料科技有限公司 | Preparation method of compound rosemary extract |
| CN103966027B (en) * | 2014-05-15 | 2016-06-29 | 青岛金智高新技术有限公司 | A kind of preparation method of the composite extract of Herba Rosmarini Officinalis |
| CN107868701A (en) * | 2017-11-09 | 2018-04-03 | 鹰潭华宝香精有限公司 | The preparation method of apricot extract |
| CN112920043A (en) * | 2021-01-26 | 2021-06-08 | 桂林莱茵生物科技股份有限公司 | Preparation method of carnosic acid with content of more than 99% |
| CN112920043B (en) * | 2021-01-26 | 2023-10-27 | 桂林莱茵生物科技股份有限公司 | Preparation method of carnosic acid with content of more than 99% |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |