CN112294725A - Preparation method of rosemary extract - Google Patents
Preparation method of rosemary extract Download PDFInfo
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- CN112294725A CN112294725A CN202011302363.2A CN202011302363A CN112294725A CN 112294725 A CN112294725 A CN 112294725A CN 202011302363 A CN202011302363 A CN 202011302363A CN 112294725 A CN112294725 A CN 112294725A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
- A61Q17/005—Antimicrobial preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
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Abstract
The invention discloses a preparation method of a rosemary extract, which relates to the technical field of rosemary extraction and aims to solve the problems that the existing preparation process of the rosemary extract is complex and a large amount of rosemary resources are wasted in the preparation process, wherein the preparation method comprises the following steps of 1, picking branches and leaves of rosemary, removing stems, cleaning and draining, then putting the branches and leaves into a drying box at the temperature of 40-50 ℃ for drying, primarily crushing the branches and leaves by using a crusher after drying, sieving the branches and leaves by using a 40-80-mesh sieve, and putting the branches and leaves into an extraction tank for low-temperature storage; step 2: distilling and extracting rosemary raw materials by using water vapor, adding the crushed rosemary raw materials into a distiller, adding water in a ratio of 0.7-1.2: 10 according to the raw materials to the water, distilling for 50-120 min to obtain a mixture of the water and the rosemary raw materials, standing, and carrying out oil-water separation to obtain crude rosemary essential oil, wherein the water and the raw materials are left in an extraction tank.
Description
Technical Field
The invention relates to the technical field of rosemary extraction, in particular to a preparation method of a rosemary extract.
Background
Rosemary, also known as Aster ageratoides, sea dew or Saint Valeriana, originally produced on the coast of the Mediterranean sea in Europe and North Africa, belongs to the evergreen shrub of Rosmarinus in Labiatae, has long and straight stem and full granules on the stem, and has narrow and sharp leaves with dark green front and grey fine villus on the back. In traditional european folks, rosemary leaves are often used to repel mosquitoes, expel parasites, relieve headaches, enhance memory, and the like. Rosemary has long been essential as a perfume ingredient in european countries, especially in french and italian cuisine, based on pleasant aroma characteristics. In recent years, with the continuous and intensive research and cognition on rosemary, rosemary extract is proved to have strong antioxidation, plays an important role in the aspects of human body immunoregulation, antibiosis and antiphlogosis, depression prevention and tumor resistance, and drives the wide development of the rosemary extract in a plurality of fields such as food functional foods, medicines, spice essences, daily chemical products and the like.
The existing preparation process of the rosemary extract is complex, and a great amount of rosemary resources are wasted in the preparation process; thus, the existing needs are not met, and a preparation method of rosemary extract is provided for the rosemary extract.
Disclosure of Invention
The invention aims to provide a preparation method of a rosemary extract, which aims to solve the problems that the existing preparation process of the rosemary extract in the background art is complex and a large amount of rosemary resources are wasted in the preparation process.
In order to achieve the purpose, the invention provides the following technical scheme: a method for preparing herba Rosmarini officinalis extract comprises the following steps:
step 1, picking rosemary branches and leaves, removing stems, cleaning and draining, then putting into a drying box at 40-50 ℃ for drying, primarily crushing by using a crusher after drying, sieving by using a 40-80 mesh sieve, and putting into an extraction tank for low-temperature storage;
step 2: distilling and extracting rosemary raw materials by using water vapor, adding the crushed rosemary raw materials into a distiller, adding water in a ratio of 0.7-1.2: 10 according to the raw materials to the water, distilling for 50-120 min to obtain a mixture of the water and the rosemary raw materials, standing, and performing oil-water separation to obtain crude rosemary essential oil, wherein the water and the raw materials are left in an extraction tank;
and step 3: extracting under reflux for 1 to 3 times in an extraction tank by using 80 to 95 percent ethanol at the reflux temperature of 50 to 60 ℃ for one and a half hours each time, combining the extracting solutions, filtering the extracting solution, concentrating under reduced pressure, cooling, and separating to obtain concentrated ursolic acid and ethanol extract;
and 4, step 4: diluting the ethanol extract concentrate with water, concentrating under reduced pressure until no alcohol smell exists, cooling, and separating to obtain carnosic acid and water solution;
and 5: spray drying the aqueous solution to obtain rosmarinic acid;
step 6: drying, crushing and sieving the ursolic acid obtained in the step 3 to obtain a finished product of the ursolic acid;
and 7: drying and crushing the carnosic acid obtained in the step 4, adding a mixed solution of a solvent and edible oil, performing reflux extraction for 3-4 times, separating, combining the extracting solutions, and recovering the solvent from the extracting solution under reduced pressure to obtain an oily product containing the carnosic acid;
and 8: and (3) separating the oily product containing carnosic acid in the step (7) by molecular distillation to obtain rosemary essential oil and a tasteless oily product of carnosic acid.
Preferably, the step 2 further comprises stopping heating when the amount of the distilled essential oil is not changed, collecting the rosemary crude essential oil and the aqueous solution respectively, and then drying and crushing the residual solid residue to obtain the treated raw material.
Preferably, the reduced pressure concentration in the step 3 is climbing film concentration or falling film concentration, and the volume concentration of the ethanol extraction concentrated solution is 1/4-3/4 of the volume of the rosemary crude essential oil.
Preferably, the volume of the water in the step 4 is 1-5 times of the volume of the ethanol extraction concentrated solution.
Preferably, the volume of the ethanol in the step 3 is 8-14 times of the weight of the rosemary raw material.
Preferably, the solvent added after the carnosic acid is dried and crushed in the step 7 is n-hexane, and the edible oil is at least one of flower seed oil, pumpkin seed oil, peanut oil, soybean oil, corn oil, rapeseed oil and olive oil.
Preferably, the temperature of the separation chamber for molecular distillation in the step 8 is room temperature, the feeding speed is 1-2 kg/min, the vacuum degree is 100-150 Pa, the distillation temperature is 40-45 ℃, the cooling temperature is 0-5 ℃, and the mass content of carnosic acid in the odorless oily product of carnosic acid is 6-20%.
Preferably, the step 8 further comprises the step of separating rosemary extract essential oil and the odorless carnosic acid oily product by a macroporous adsorption resin method.
Preferably, the macroporous adsorption resin method separation process specifically comprises the following steps: enriching active ingredients by using macroporous resin, firstly washing 8 column volumes by using 10% ethanol to remove large polar ingredients, then eluting 12 column volumes by using 90% ethanol, collecting 90% eluent, and concentrating under reduced pressure to obtain the final rosemary extract.
Preferably, the macroporous resin is AB-8 type macroporous adsorption resin.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, a pair of rosemary essential oil, carnosic acid, ursolic acid and rosmarinic acid can be extracted and separated one by one, the utilization rate of rosemary raw materials is improved, the concentration process has an efficient separation effect through a reduced pressure concentration process, and the emulsification phenomenon caused by directly adding water to dilute the extracting solution to be close to a water environment is avoided.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Example 1
A method for preparing herba Rosmarini officinalis extract comprises the following steps:
step 1, picking rosemary branches and leaves, removing stems, cleaning and draining, then putting into a drying box at 45 ℃ for drying, primarily crushing by using a crusher after drying, sieving by using a 60-mesh sieve, and putting into an extraction tank for low-temperature storage;
step 2: distilling and extracting rosemary raw materials by using water vapor, adding the crushed rosemary raw materials into a distiller, adding water in a ratio of 1:10 according to the raw materials to the water, distilling for 100min to obtain a mixture of the water and the rosemary raw materials, standing, and performing oil-water separation to obtain crude rosemary essential oil, wherein the water and the raw materials are left in an extraction tank;
and step 3: extracting with 80-95% ethanol under reflux for 2 times in an extraction tank, each time for one and a half hours at a reflux temperature of 55 deg.C, mixing extractive solutions, filtering the extractive solution, concentrating under reduced pressure, cooling, and separating to obtain concentrated ursolic acid and ethanol extract;
and 4, step 4: diluting the ethanol extract concentrate with water, concentrating under reduced pressure until no alcohol smell exists, cooling, and separating to obtain carnosic acid and water solution;
and 5: spray drying the aqueous solution to obtain rosmarinic acid;
step 6: drying, crushing and sieving the ursolic acid obtained in the step 3 to obtain a finished product of the ursolic acid;
and 7: drying and crushing the carnosic acid obtained in the step 4, adding a mixed solution of a solvent and edible oil, performing reflux extraction for 3-4 times, separating, combining the extracting solutions, and recovering the solvent from the extracting solution under reduced pressure to obtain an oily product containing the carnosic acid;
and 8: and (3) separating the oily product containing carnosic acid in the step (7) by molecular distillation to obtain rosemary essential oil and a tasteless oily product of carnosic acid.
Further, the step 2 comprises stopping heating when the amount of distilled essential oil is not changed, collecting crude rosemary essential oil and aqueous solution respectively, drying the residual solid residue, and crushing to obtain the treated raw material.
Further, the vacuum concentration in step 3 is ascending film concentration or falling film concentration, and the volume concentration of the ethanol extraction concentrated solution is 1/4 of the volume of the rosemary crude essential oil.
Further, the volume of water in step 4 is 3 times of the volume of the ethanol extraction concentrate.
Further, the volume of ethanol in step 3 is 10 times of the weight of the rosemary raw material.
Further, in the step 7, after the carnosic acid is dried and crushed, the added solvent is n-hexane, and the edible oil is the flower seed oil.
Further, the temperature of the separation chamber for molecular distillation in step 8 was room temperature, the feeding rate was 2kg/min, the vacuum degree was 120Pa, the distillation temperature was 43 ℃, the cooling temperature was 2 ℃, and the mass content of carnosic acid in the odorless oily product of carnosic acid was 10%.
Further, step 8 includes the step of separating rosemary extract essential oil and odorless carnosic acid oily product by a macroporous adsorption resin method.
Further, the separation process by a macroporous adsorption resin method specifically comprises the following steps: enriching active ingredients by using macroporous resin, firstly washing 8 column volumes by using 10% ethanol to remove large polar ingredients, then eluting 12 column volumes by using 90% ethanol, collecting 90% eluent, and concentrating under reduced pressure to obtain the final rosemary extract.
Further, the macroporous resin is AB-8 type macroporous adsorption resin.
Example 2
A method for preparing herba Rosmarini officinalis extract comprises the following steps:
step 1, picking rosemary branches and leaves, removing stems, cleaning and draining, then placing into a drying box at 50 ℃ for drying, primarily crushing by using a crusher after drying, sieving by using a 80-mesh sieve, and placing in an extraction tank for low-temperature storage;
step 2: distilling and extracting rosemary raw materials by using water vapor, adding the crushed rosemary raw materials into a distiller, adding water with the ratio of the raw materials to the water of 0.8:10, distilling for 120min to obtain a mixture of the water and the rosemary raw materials, standing, and carrying out oil-water separation to obtain crude rosemary essential oil, wherein the water and the raw materials are left in an extraction tank;
and step 3: extracting with 80-95% ethanol under reflux for 3 times in an extraction tank at 50 deg.C for one and a half hours each time, mixing extractive solutions, filtering, concentrating under reduced pressure, cooling, and separating to obtain concentrated ursolic acid and ethanol extract;
and 4, step 4: diluting the ethanol extract concentrate with water, concentrating under reduced pressure until no alcohol smell exists, cooling, and separating to obtain carnosic acid and water solution;
and 5: spray drying the aqueous solution to obtain rosmarinic acid;
step 6: drying, crushing and sieving the ursolic acid obtained in the step 3 to obtain a finished product of the ursolic acid;
and 7: drying and crushing the carnosic acid obtained in the step 4, adding a mixed solution of a solvent and edible oil, performing reflux extraction for 3-4 times, separating, combining the extracting solutions, and recovering the solvent from the extracting solution under reduced pressure to obtain an oily product containing the carnosic acid;
and 8: and (3) separating the oily product containing carnosic acid in the step (7) by molecular distillation to obtain rosemary essential oil and a tasteless oily product of carnosic acid.
Further, the step 2 comprises stopping heating when the amount of distilled essential oil is not changed, collecting crude rosemary essential oil and aqueous solution respectively, drying the residual solid residue, and crushing to obtain the treated raw material.
Further, the vacuum concentration in step 3 is ascending film concentration or falling film concentration, and the volume concentration of the ethanol extraction concentrated solution is 3/4 of the volume of the rosemary crude essential oil.
Further, the volume of water in step 4 is 4 times of the volume of the ethanol extraction concentrate.
Further, the volume of ethanol in step 3 is 12 times of the weight of the rosemary raw material.
Further, in the step 7, the solvent added after the carnosic acid is dried and crushed is n-hexane, and the edible oil is pumpkin seed oil.
Further, the temperature of the separation chamber for molecular distillation in step 8 was room temperature, the feed rate was 1kg/min, the vacuum was 140Pa, the distillation temperature was 45 ℃, the cooling temperature was 1 ℃, and the mass content of carnosic acid in the odorless oily product of carnosic acid was 18%.
Further, step 8 includes the step of separating rosemary extract essential oil and odorless carnosic acid oily product by a macroporous adsorption resin method.
Further, the separation process by a macroporous adsorption resin method specifically comprises the following steps: enriching active ingredients by using macroporous resin, firstly washing 8 column volumes by using 10% ethanol to remove large polar ingredients, then eluting 12 column volumes by using 90% ethanol, collecting 90% eluent, and concentrating under reduced pressure to obtain the final rosemary extract.
Further, the macroporous resin is AB-8 type macroporous adsorption resin.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (10)
1. A preparation method of rosemary extract is characterized in that: the method comprises the following steps:
step 1, picking rosemary branches and leaves, removing stems, cleaning and draining, then putting into a drying box at 40-50 ℃ for drying, primarily crushing by using a crusher after drying, sieving by using a 40-80 mesh sieve, and putting into an extraction tank for low-temperature storage;
step 2: distilling and extracting rosemary raw materials by using water vapor, adding the crushed rosemary raw materials into a distiller, adding water in a ratio of 0.7-1.2: 10 according to the raw materials to the water, distilling for 50-120 min to obtain a mixture of the water and the rosemary raw materials, standing, and performing oil-water separation to obtain crude rosemary essential oil, wherein the water and the raw materials are left in an extraction tank;
and step 3: extracting under reflux for 1 to 3 times in an extraction tank by using 80 to 95 percent ethanol at the reflux temperature of 50 to 60 ℃ for one and a half hours each time, combining the extracting solutions, filtering the extracting solution, concentrating under reduced pressure, cooling, and separating to obtain concentrated ursolic acid and ethanol extract;
and 4, step 4: diluting the ethanol extract concentrate with water, concentrating under reduced pressure until no alcohol smell exists, cooling, and separating to obtain carnosic acid and water solution;
and 5: spray drying the aqueous solution to obtain rosmarinic acid;
step 6: drying, crushing and sieving the ursolic acid obtained in the step 3 to obtain a finished product of the ursolic acid;
and 7: drying and crushing the carnosic acid obtained in the step 4, adding a mixed solution of a solvent and edible oil, performing reflux extraction for 3-4 times, separating, combining the extracting solutions, and recovering the solvent from the extracting solution under reduced pressure to obtain an oily product containing the carnosic acid;
and 8: and (3) separating the oily product containing carnosic acid in the step (7) by molecular distillation to obtain rosemary essential oil and a tasteless oily product of carnosic acid.
2. The method of claim 1, wherein the rosemary extract is prepared by the following steps: and the step 2 also comprises stopping heating when the amount of the distilled essential oil is not changed any more, respectively collecting the rosemary crude essential oil and the rosemary aqueous solution, and then drying and crushing the residual solid residue to obtain the treated raw material.
3. The method of claim 1, wherein the rosemary extract is prepared by the following steps: and 3, performing vacuum concentration in the step 3 by adopting climbing film concentration or falling film concentration, wherein the volume concentration of an ethanol extraction concentrated solution is 1/4-3/4 of the volume of the rosemary crude essential oil.
4. The method of claim 1, wherein the rosemary extract is prepared by the following steps: and in the step 4, the volume of water is 1-5 times of the volume of the ethanol extraction concentrated solution.
5. The method of claim 1, wherein the rosemary extract is prepared by the following steps: and in the step 3, the volume of the ethanol is 8-14 times of the weight of the rosemary raw material.
6. The method of claim 1, wherein the rosemary extract is prepared by the following steps: in the step 7, the solvent added after the carnosic acid is dried and crushed is n-hexane, and the edible oil is at least one of flower seed oil, pumpkin seed oil, peanut oil, soybean oil, corn oil, rapeseed oil and olive oil.
7. The method of claim 1, wherein the rosemary extract is prepared by the following steps: the temperature of a separation chamber for molecular distillation in the step 8 is room temperature, the feeding speed is 1-2 kg/min, the vacuum degree is 100-150 Pa, the distillation temperature is 40-45 ℃, the cooling temperature is 0-5 ℃, and the mass content of carnosic acid in the odorless oily product of carnosic acid is 6-20%.
8. The method for preparing rosemary extract according to claim 1, wherein the step 8 further comprises subjecting rosemary essential oil and the odorless oily product of carnosic acid to a separation process by a macroporous adsorbent resin method.
9. The method for preparing rosemary extract according to claim 8, wherein the macroporous adsorbent resin separation process specifically comprises: enriching active ingredients by using macroporous resin, firstly washing 8 column volumes by using 10% ethanol to remove large polar ingredients, then eluting 12 column volumes by using 90% ethanol, collecting 90% eluent, and concentrating under reduced pressure to obtain the final rosemary extract.
10. The method of claim 9, wherein the rosemary extract is prepared by the following steps: the macroporous resin is AB-8 type macroporous adsorption resin.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113041279A (en) * | 2021-05-28 | 2021-06-29 | 湖南绿蔓生物科技股份有限公司 | Method for separating effective components from momordica grosvenori flowers |
| WO2024082329A1 (en) * | 2022-10-20 | 2024-04-25 | 湖南祥民制药有限公司 | Freeze-drying method for rosmarinus officinalis |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286059A (en) * | 2011-09-08 | 2011-12-21 | 南京泽朗医药科技有限公司 | Method for extracting ursolic acid, carnosic acid and rosmarinic acid from rosmarinus officinalis |
| CN108070453A (en) * | 2016-11-11 | 2018-05-25 | 长沙卫生物科技有限公司 | A kind of method that extraction separates Rosemary Oil, Rosmarinic acid, ursolic acid and carnosic acid from rosemary |
-
2020
- 2020-11-19 CN CN202011302363.2A patent/CN112294725A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286059A (en) * | 2011-09-08 | 2011-12-21 | 南京泽朗医药科技有限公司 | Method for extracting ursolic acid, carnosic acid and rosmarinic acid from rosmarinus officinalis |
| CN108070453A (en) * | 2016-11-11 | 2018-05-25 | 长沙卫生物科技有限公司 | A kind of method that extraction separates Rosemary Oil, Rosmarinic acid, ursolic acid and carnosic acid from rosemary |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113041279A (en) * | 2021-05-28 | 2021-06-29 | 湖南绿蔓生物科技股份有限公司 | Method for separating effective components from momordica grosvenori flowers |
| WO2024082329A1 (en) * | 2022-10-20 | 2024-04-25 | 湖南祥民制药有限公司 | Freeze-drying method for rosmarinus officinalis |
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Application publication date: 20210202 |