Preparation method of rosemary extract

Abstract

The invention belongs to the technical field of rosemary extract preparation, and discloses a rosemary extract preparation method, which comprises: S1, raw material preparation and pretreatment: a, selecting high-quality rosemary as a raw material; b, carrying out drying treatment on the picked rosemary; through the high-pressure micro-jet technology, the extraction time is greatly shortened, and the production efficiency is improved; the cell structure of the raw material is physically destroyed through the high-pressure treatment process, the use of chemical solvents is avoided, so that the purity and safety of the extract are ensured, the quality of the extract can be further optimized by accurately controlling treatment parameters (such as pressure, flow, temperature and cycle index), and the extract is ensured to meet the requirements of high quality and high purity; essential oil components can be more thoroughly released by utilizing a high-pressure micro-jet technology, so that the yield of an extract is improved, more impurities and bad components can be removed through multiple times of circulating jet finishing treatment, and the purity of the essential oil is improved.

Description

Technical Field

[0001] The invention belongs to the technical field of rosemary extract preparation, and specifically relates to a method for preparing the rosemary extract. Background Art

[0002] Rosemary extract is a substance extracted from Rosemary (Rosmarinus of ici na lis L.), a plant of the genus Salvia in the family Lamiaceae. It contains a variety of biologically active ingredients, especially essential oil components, which give rosemary extract a wide range of application value in many fields.

[0003] In the prior art, during the preparation of the rosemary extract, the powder accumulated in the distillation tower has a relatively small area. Although distillation is performed after adding distilled water, the actual dispersion effect of the powder is still limited. In addition, under the static distillation effect, the release effect of the essential oil in the rosemary powder is poor, so that the essential oil content in the mixed gas output per unit time of distillation is low, the comprehensive extraction efficiency is low, the distillation effect is not good, and the mixed solution after the essential oil is condensed needs to be fully separated and processed. The extract is separated from the water. During the separation process, there is impurity contamination, the separation is not thorough enough, and there is partial contamination after the separation and extraction, and the comprehensive extraction preparation effect is not good. Summary of the invention

[0004] The object of the present invention is to provide a method for preparing a rosemary extract to solve the problems raised in the above background technology.

[0005] In order to achieve the above object, the present invention provides the following technical solution: a method for preparing rosemary extract, comprising the following preparation steps:

[0006] S1. Raw material preparation and pretreatment:

[0007] aSelect high-quality rosemary as raw material;

[0008] b. drying the picked rosemary, specifically freeze drying;

[0009] c. crushing the dried rosemary, wherein the particle size of the crushed rosemary is usually controlled within the range of 20-60 meshes, and then sieving the crushed rosemary;

[0010] S2. Steam distillation extraction:

[0011] a. Load the crushed and sieved rosemary raw material into the distiller;

[0012] b. Add appropriate amount of water according to the ratio of raw materials to water;

[0013] c. Use high-pressure microfluidization technology to distill the powder after jetting.

[0014] d. filling enzymatic agent to carry out enzymatic assisted distillation;

[0015] e. The water vapor takes out the essential oil components in the rosemary, and the distilled water vapor and essential oil mixture is passed into a condensation device, and the water and essential oil components are condensed to obtain a mixed condensate;

[0016] S3, separation and purification:

[0017] a. subjecting the mixed condensate to oil-water separation treatment, and obtaining crude rosemary essential oil by supercritical fluid extraction technology;

[0018] b. further refining the crude rosemary essential oil;

[0019] S4. Drying and packaging:

[0020] a. drying the refined rosemary extract;

[0021] b. Package the dried rosemary extract and store it in a constant temperature, light-proof, dry environment.

[0022] Preferably, in S1, the high-quality rosemary is: a rosemary plant with good growth, full leaves and emerald green color, and the time of picking is the plant at the beginning of the flowering period and shortly after flowering. During this period, the picked rosemary is strictly screened to remove diseased and insect-infested leaves, yellow leaves, dead leaves and mixed impurities.

[0023] Preferably, in S1, during the freeze-drying process, the rosemary is frozen at a low temperature of -40°C and then sublimated and dried under vacuum conditions; the dried rosemary is pulverized using a low-temperature pulverizer, and the internal temperature of the pulverizer is controlled below -10°C.

[0024] Preferably, in S2, the charging amount is controlled according to the capacity of the distiller and the density of the rosemary raw material, and the charging amount is 2 / 5 of the volume of the distiller; according to the water content and essential oil content of the rosemary raw material, the added water is calculated, and the ratio of the raw material to water is controlled at 0.8:10.

[0025] Preferably, in S2, the pressure of the high-pressure microjet is 50-200 MPa, the flow rate is 1-10 L / min, the heat in the jet process is 25-50°C, and during the high-pressure microjet treatment, the material is subjected to cyclic jet finishing treatment, and the number of cycles is 8-12 times.

[0026] Preferably, in S2, the enzymatic agent includes one or any one of cellulase, pectinase and hemicellulase, the enzymatic hydrolysis temperature is 25-50°C, the enzymatic hydrolysis time is 4.0-6.0h, and the enzyme dosage is 0.1%-5% of the weight of the raw material.

[0027] Preferably, in S3, a supercritical fluid extraction device with the function of accurately controlling pressure and temperature is selected, specifically a carbon dioxide supercritical extraction device, the pressure is set to 5-10MPa, and the temperature is set to 30-60°C. During the specific implementation, the carbon dioxide fluid is made to enter a supercritical state, and the fluid is sent into an extraction kettle through a circulation pump to fully contact with the crude rosemary essential oil to achieve selective extraction of the target essential oil.

[0028] Preferably, in S4, the drying method is spray drying, and the drying temperature is controlled between 40-60°C.

[0029] The beneficial effects of the present invention are as follows:

[0030] 1. The present invention can quickly and effectively destroy the cell structure of rosemary raw materials by utilizing the physical fragmentation effect of high-pressure microjets, so that the essential oil components in the cells can be quickly released. Compared with traditional extraction methods, the high-pressure microjets technology greatly shortens the extraction time and improves production efficiency; the cell structure of the raw materials is physically destroyed by the high-pressure treatment process, thereby avoiding the use of chemical solvents, thereby ensuring the purity and safety of the extract, and by accurately controlling the processing parameters (such as pressure, flow, temperature and number of cycles), the quality of the extract can be further optimized to ensure that it meets the requirements of high quality and high purity; by utilizing the high-pressure microjets technology, the essential oil components can be released more thoroughly, thereby improving the yield of the extract, and by multiple cycles of jet finishing treatment, more impurities and undesirable components can be removed to improve the purity of the essential oil.

[0031] 2. The present invention utilizes enzymolysis-assisted distillation technology to add specific enzymes to specifically decompose cell wall components of rosemary raw materials, such as cellulose, pectin, etc., so as to more effectively release the essential oil components in the cells. The action mode of this biological enzyme is mild and efficient, avoiding the problems of incomplete cell structure destruction or impurity introduction that may be caused by traditional physical or chemical methods; enzymolysis can accelerate the rupture of cell walls, making it easier for essential oil components to migrate from cells to extraction solvents. Compared with a single distillation method, enzymolysis-assisted distillation technology can significantly improve the extraction efficiency of essential oils, shorten extraction time, and reduce energy consumption; the enzymolysis process can selectively decompose cell wall components, while having little effect on the essential oil components themselves, thereby ensuring the purity and quality of the extract; enzymolysis-assisted distillation technology can reduce the impurity content in the extract and improve the purity of the essential oil. At the same time, enzymolysis can also improve the stability of the extract, extend its shelf life, and provide a strong guarantee for the subsequent application of the product.

[0032] 3. The present invention utilizes carbon dioxide in a supercritical state as a solvent through supercritical carbon dioxide extraction technology, has strong dissolving power and selectivity, and can efficiently extract the essential oil components in rosemary. This technology avoids impurities and chemical residues that may be introduced in traditional extraction methods, thereby protecting the purity and natural characteristics of the essential oil. The supercritical carbon dioxide extraction technology is usually extracted at close to room temperature (35-40°C) and under the cover of CO2 gas, avoiding the destruction of heat-sensitive essential oil components by high temperature. This gentle extraction condition helps to retain the active ingredients and aroma in the rosemary essential oil, and improves the quality of the extract. The supercritical carbon dioxide extraction technology can accurately control the extraction process by adjusting parameters such as pressure and temperature, and realize process optimization. The technology is also easy to be combined with automated equipment to realize automation and intelligence of the production process, and improve production efficiency and product quality. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 It is a schematic diagram of the preparation process of the present invention; DETAILED DESCRIPTION

[0034] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0035] like Figure 1 As shown, the embodiment of the present invention provides a method for preparing a rosemary extract, comprising the following preparation steps:

[0036] S1. Raw material preparation and pretreatment:

[0037] aSelect high-quality rosemary as raw material;

[0038] b. drying the picked rosemary, specifically freeze drying;

[0039] c. crushing the dried rosemary, wherein the particle size of the crushed rosemary is usually controlled within the range of 20-60 meshes, and then sieving the crushed rosemary;

[0040] S2. Steam distillation extraction:

[0041] a. Load the crushed and sieved rosemary raw material into the distiller;

[0042] b. Add appropriate amount of water according to the ratio of raw materials to water;

[0043] c. Use high-pressure microfluidization technology to distill the powder after jetting.

[0044] d. filling enzymatic agent to carry out enzymatic assisted distillation;

[0045] e. The water vapor takes out the essential oil components in the rosemary, and the distilled water vapor and essential oil mixture is passed into a condensation device, and the water and essential oil components are condensed to obtain a mixed condensate;

[0046] S3, separation and purification:

[0047] a. subjecting the mixed condensate to oil-water separation treatment, and obtaining crude rosemary essential oil by supercritical fluid extraction technology;

[0048] b. further refining the crude rosemary essential oil;

[0049] S4. Drying and packaging:

[0050] a. drying the refined rosemary extract;

[0051] b. Package the dried rosemary extract and store it in a constant temperature, light-proof, dry environment.

[0052] Among them, in S1, high-quality rosemary refers to: rosemary plants with good growth, full leaves and emerald green color, and the time of picking is the plants in the early flowering period and shortly after flowering. During this period, the picked rosemary is strictly screened to remove diseased and insect-infested leaves, yellow leaves, dead leaves and mixed impurities.

[0053] The health and vitality of the rosemary raw materials are ensured by using well-grown rosemary plants with full leaves and emerald green color. Well-grown rosemary plants usually contain more active ingredients, such as rosmarinic acid, carnosic acid, etc. These ingredients are essential for the flavor, antioxidant and functionality of the extract. Full leaves and emerald green color indicate that the plants are well-nourished and not subject to serious environmental stress or pests and diseases. By determining the time of picking, plants are picked at the beginning of the flowering period and shortly after flowering to ensure a high content of active ingredients in the rosemary leaves, while avoiding the bitter taste or changes in composition that may be caused by the full opening of the flowers, helping to ensure the best functionality of the extract.

[0054] By removing diseased and insect-infested leaves, yellow leaves, and dead leaves, we can avoid high levels of disease and insect residues or degraded active ingredients. By strictly screening and removing these leaves, we can avoid their adverse effects on the quality of the final extract. Removing impurities including soil, stones, dead branches and leaves will not only reduce the purity of the extract, but may also introduce unnecessary pollutants or odors.

[0055] Among them, in S1, during the freeze-drying process, the rosemary is frozen at a low temperature of -40°C, and then sublimation drying is performed under vacuum conditions; the dried rosemary is crushed using a low-temperature crusher, and the internal temperature of the crusher is controlled below -10°C.

[0056] Freezing rosemary at a low temperature of -40°C can quickly fix the active ingredients in rosemary and prevent chemical changes or degradation during the drying process. Low-temperature freezing can also effectively kill or inhibit the growth of microorganisms, thereby improving the sanitary quality of the product. Sublimation drying is carried out under vacuum conditions, that is, the principle of ice crystals directly sublimating into water vapor is used to remove moisture from rosemary, avoiding the active ingredients being taken away by water evaporation during the traditional drying process, thereby retaining the internal substances of rosemary to the greatest extent. Vacuum conditions can also effectively prevent the occurrence of oxidation reactions, further protecting the active ingredients in rosemary.

[0057] A low-temperature pulverizer is used, the internal temperature of which is controlled below -10°C during use, to pulverize the dried rosemary into particles of a size suitable for subsequent extraction while maintaining the stability of its active ingredients. Pulverizing in a low-temperature environment can effectively prevent the active ingredients in rosemary from being degraded or inactivated due to increased temperature. In addition, the low temperature can also slow down the adverse effects of the heat generated during the pulverization process on the quality of rosemary, ensuring that the quality of the final product is stable and reliable.

[0058] The active ingredients of rosemary that has been freeze-dried and cryogenically crushed are effectively retained, and the particle size is moderate, which is conducive to solvent penetration and release of active ingredients in the subsequent extraction process, thereby improving the extraction efficiency; the freeze-drying and cryogenically crushing process can retain the value of rosemary to the greatest extent, while reducing the generation of impurities, thereby improving the quality of the final product.

[0059] Among them, in S2, the charging amount is controlled according to the capacity of the distiller and the density of the rosemary raw material, and the charging amount is 2 / 5 of the volume of the distiller; according to the water content and essential oil content of the rosemary raw material, the added water is calculated, and the ratio of raw material to water is controlled at 0.8:10.

[0060] By considering the actual capacity of the distiller and the density of the rosemary raw material, the loading amount is determined, which not only ensures that the raw materials in the distiller can be fully heated and distilled, but also avoids the problem of incomplete distillation or blockage caused by excessive loading. A reasonable loading amount can ensure the heat transfer efficiency during the distillation process, so that the essential oil components in the raw materials can be extracted more effectively. At the same time, avoiding excessive loading can also reduce energy consumption and time costs in the distillation process and improve overall production efficiency; by accurately controlling the loading amount, incomplete distillation caused by excessive raw materials can be avoided, thereby ensuring the purity and quality of the final extract.

[0061] By precisely controlling the loading amount and the water addition ratio, the purity of the final extract can be ensured, the content of impurities and undesirable components can be reduced, the yield of the extract can be increased, and the production cost can be reduced.

[0062] Among them, in S2, the pressure of the high-pressure microjet is 50-200MPa, the flow rate is 1-10L / min, the heat in the jet process is 25-50°C, and during the high-pressure microjet treatment process, the material is subjected to cyclic jet finishing treatment, and the number of cycles is 8-12 times.

[0063] High-pressure micro-jet technology uses high-pressure water flow to impact and shear the rosemary raw material at high speed. The strong mechanical force can destroy the plant cell wall, making it easier to release the essential oils and other active ingredients in the cells. According to the hardness, cell structure and properties of the target extract of the rosemary raw material, it is determined through experiments that the pressure is 50-200MPa, which has a better crushing effect.

[0064] The physical fragmentation of high-pressure microfluidics can quickly and effectively destroy the cell structure of rosemary raw materials, allowing the essential oil components in the cells to be quickly released. Compared with traditional extraction methods, high-pressure microfluidics technology greatly shortens the extraction time and improves production efficiency.

[0065] The cell structure of the raw materials is physically destroyed through the high-pressure treatment process, avoiding the use of chemical solvents, thereby ensuring the purity and safety of the extract. By precisely controlling the processing parameters (such as pressure, flow, temperature and number of cycles), the quality of the extract can be further optimized to ensure that it meets the requirements of high quality and high purity.

[0066] By utilizing high-pressure micro-jet technology, the essential oil components can be released more thoroughly, thereby increasing the yield of the extract, and through multiple cycles of jet finishing treatment, more impurities and undesirable components can be removed, thereby improving the purity of the essential oil.

[0067] Among them, in S2, the enzymatic agent includes one or any one of cellulase, pectinase, and hemicellulase, the enzymatic hydrolysis temperature is 25-50°C, the enzymatic hydrolysis time is 4.0-6.0h, and the enzyme dosage is 0.1%-5% of the weight of the raw material.

[0068] By adding specific enzymes, enzymatic assisted distillation technology can specifically decompose the cell wall components of rosemary raw materials, such as cellulose, pectin, etc., so as to more effectively release the essential oil components in the cells. The action mode of this biological enzyme is mild and efficient, avoiding the problems of incomplete cell structure destruction or introduction of impurities that may be caused by traditional physical or chemical methods; enzymatic hydrolysis can accelerate the rupture of cell walls, making it easier for essential oil components to migrate from the cells to the extraction solvent. Compared with the single distillation method, enzymatic assisted distillation technology can significantly improve the extraction efficiency of essential oils, shorten the extraction time, and reduce energy consumption; the enzymatic hydrolysis process can selectively decompose cell wall components with little effect on the essential oil components themselves, thereby ensuring the purity and quality of the extract; enzymatic assisted distillation technology can reduce the impurity content in the extract and improve the purity of the essential oil. At the same time, enzymatic hydrolysis can also improve the stability of the extract and extend its shelf life, providing strong guarantees for the subsequent application of the product.

[0069] By precisely controlling the type, concentration and treatment time of the enzyme, the quality of the extract can be further optimized to meet the market demand for high-quality, high-purity essential oils.

[0070] Among them, in S3, a supercritical fluid extraction device with the function of accurately controlling pressure and temperature is selected, specifically a carbon dioxide supercritical extraction device, with a set pressure of 5-10MPa and a temperature of 30-60°C. During implementation, the carbon dioxide fluid is put into a supercritical state, and the fluid is sent into the extraction kettle through a circulation pump to fully contact with the crude rosemary essential oil to achieve selective extraction of the target essential oil.

[0071] The supercritical carbon dioxide extraction technology uses supercritical carbon dioxide as a solvent, which has strong dissolving power and selectivity, and can efficiently extract the essential oil components in rosemary. This technology avoids impurities and chemical residues that may be introduced in traditional extraction methods, thereby protecting the purity and natural properties of the essential oil. The supercritical carbon dioxide extraction technology is usually carried out at close to room temperature (35-40°C) and under the cover of CO2 gas, avoiding the damage of high temperature to heat-sensitive essential oil components. This mild extraction condition helps to retain the active ingredients and aroma in rosemary essential oil and improve the quality of the extract. The supercritical carbon dioxide extraction technology can accurately control the extraction process and achieve process optimization by adjusting parameters such as pressure and temperature. This technology is also easy to combine with automated equipment to realize automation and intelligence of the production process, thereby improving production efficiency and product quality.

[0072] Among them, in S4, the drying method is spray drying, and the drying temperature is controlled between 40-60°C.

[0073] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for preparing a rosemary extract is characterized in that: The method comprises the following preparation steps: S1. Raw material preparation and pretreatment: aSelect high-quality rosemary as raw material; b. drying the picked rosemary, specifically freeze drying; c. crushing the dried rosemary, wherein the particle size of the crushed rosemary is usually controlled within the range of 20-60 meshes, and then sieving the crushed rosemary; S2. Steam distillation extraction: a. Load the crushed and sieved rosemary raw material into the distiller; b. Add appropriate amount of water according to the ratio of raw materials to water; c. Use high-pressure microfluidization technology to distill the powder after jetting. d. filling enzymatic agent to carry out enzymatic assisted distillation; e. The water vapor takes out the essential oil components in the rosemary, and the distilled water vapor and essential oil mixture is passed into a condensation device, and the water and essential oil components are condensed to obtain a mixed condensate; S3, separation and purification: a. subjecting the mixed condensate to oil-water separation treatment, and obtaining crude rosemary essential oil by supercritical fluid extraction technology; b. further refining the crude rosemary essential oil; S4. Drying and packaging: a. drying the refined rosemary extract; b. Package the dried rosemary extract and store it in a constant temperature, light-proof, dry environment.

2. The method for preparing a rosemary extract according to claim 1, wherein: In S1, high-quality rosemary refers to rosemary plants with good growth, full leaves and emerald green color, and the time of picking is the plants at the beginning of the flowering period and shortly after flowering. During this period, the picked rosemary is strictly screened to remove diseased and insect-infested leaves, yellow leaves, dead leaves and mixed impurities.

3. The method for preparing a rosemary extract according to claim 2, wherein: In S1, during the freeze-drying process, the rosemary is frozen at a low temperature of -40°C and then sublimated and dried under vacuum conditions; the dried rosemary is pulverized using a low-temperature pulverizer, and the internal temperature of the pulverizer is controlled to be below -10°C.

4. The method for preparing a rosemary extract according to claim 1, wherein: In the S2, the charging amount is controlled according to the capacity of the distiller and the density of the rosemary raw material, and the charging amount is 2 / 5 of the volume of the distiller; according to the water content and essential oil content of the rosemary raw material, the added water is calculated, and the ratio of the raw material to water is controlled at 0.8:

10.

5. The method for preparing a rosemary extract according to claim 4, characterized in that: In S2, the pressure of the high-pressure micro jet is 50-200 MPa, the flow rate is 1-10 L / min, the heat in the jet process is 25-50° C. During the high-pressure micro jet treatment process, the material is subjected to cyclic jet finishing treatment, and the number of cycles is 8-12 times.

6. The method for preparing a rosemary extract according to claim 5, characterized in that: In S2, the enzymatic agent includes one or any of cellulase, pectinase and hemicellulase, the enzymatic hydrolysis temperature is 25-50°C, the enzymatic hydrolysis time is 4.0-6.0h, and the enzyme dosage is 0.1%-5% of the weight of the raw material.

7. The method for preparing a rosemary extract according to claim 1, characterized in that: In S3, a supercritical fluid extraction device with the function of accurately controlling pressure and temperature is selected, specifically a carbon dioxide supercritical extraction device, and the pressure is set to 5-10MPa and the temperature is set to 30-60°C. During the specific implementation, the carbon dioxide fluid is put into a supercritical state, and the fluid is sent into the extraction kettle through a circulation pump to fully contact with the crude rosemary essential oil to achieve selective extraction of the target essential oil.

8. The method for preparing a rosemary extract according to claim 1, characterized in that: In S4, the drying method is spray drying, and the drying temperature is controlled between 40-60°C.

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