A kind of technology of extracting rosemary essential oil

Abstract

The present invention relates to a process for extracting rosemary essential oil, and the process for extracting rosemary essential oil comprises the following steps: S1, cutting, crushing and fermenting rosemary to obtain pretreated rosemary; S2, mixing the pretreated rosemary with modified activated carbon, introducing humid air, and standing for adsorption; S3, desorbing the modified activated carbon to obtain rosemary essential oil; wherein the modified activated carbon is cellulose or polyacrylic acid modified activated carbon. The present invention first ferments rosemary, then uses modified activated carbon to adsorb essential oil in rosemary, and finally obtains essential oil through desorption. The essential oil in rosemary branches and leaves can be efficiently separated by combining multiple processes, effectively improving the yield and purity of the essential oil, and solving the problems existing in the prior art.

Description

Technical Field

[0001] The invention relates to the technical field of plant extracts, in particular to a process for extracting rosemary essential oil. Background Art

[0002] Rosemary is an economic crop with multiple uses. Its leaves have a fragrant smell and have been widely used in spices, medicine, food, etc. Extracting essential oil with active ingredients from rosemary is one of the main processing methods at present.

[0003] Rosemary essential oil contains a large amount of terpenes, flavonoids, and organic acids such as carnosic acid, rosmarinic acid, and rosmarinic acid, which give it a rich flavor. It also has antibacterial, insect repellent, antioxidant, anti-tumor, and liver-protecting effects. Therefore, rosemary essential oil products are used as raw materials in perfumes, shower gels, shampoos, antioxidants, seasonings, health products, medicines, and other products.

[0004] Rosemary essential oil is traditionally extracted by steam distillation or solvent method. These two methods are simple and low-cost. However, these two methods have the problems of high extraction temperature and long extraction time, which may destroy the structure of active ingredients and affect the quality and performance of essential oil. 2 Rosemary essential oil is extracted by extraction and microwave-assisted methods, but the essential oil components obtained by this method are somewhat different from those extracted by traditional methods, and there are also defects such as insufficient essential oil quality, high production cost and high energy consumption.

[0005] In summary, it is necessary to develop a new technical solution to solve the deficiencies in the prior art. Summary of the invention

[0006] Based on this, the present invention provides a process for extracting rosemary essential oil. The present invention first ferments rosemary, then uses modified activated carbon to adsorb the essential oil in the rosemary, and finally obtains the essential oil through desorption. The essential oil in the rosemary branches and leaves can be efficiently separated by combining multiple processes, effectively improving the yield and purity of the essential oil, and solving the problems existing in the prior art.

[0007] An object of the present invention is to provide a process for extracting rosemary essential oil, the process for extracting rosemary essential oil comprising the following steps:

[0008] S1, cutting, crushing and fermenting rosemary to obtain pretreated rosemary;

[0009] S2, mixing the pretreated rosemary with modified activated carbon, introducing humid air, and allowing to stand for adsorption;

[0010] S3, desorbing the modified activated carbon to obtain rosemary essential oil;

[0011] in,

[0012] The modified activated carbon is cellulose or polyacrylic acid modified activated carbon.

[0013] Furthermore, the rosemary is selected from rosemary leaves and young branches.

[0014] Furthermore, the fermentation uses one or more of lactic acid bacteria, yeast, and mold.

[0015] Furthermore, the fineness of the pulverization is 200-500 mesh.

[0016] Furthermore, the humidity of the humid air is 30-60%.

[0017] Furthermore, the static adsorption time is 24-48 hours and the temperature is 30-40°C.

[0018] Furthermore, the preparation method of the modified activated carbon comprises the following steps:

[0019] L1, mixing activated carbon, acrylic acid monomer and initiator, heating and reacting under an inert gas atmosphere to obtain an intermediate product;

[0020] L2. The intermediate product and cellulose are blended, ultrasonically treated, and then pressed to obtain modified activated carbon.

[0021] Furthermore, the heating reaction temperature is 60-80°C and the time is 2-4h.

[0022] Furthermore, the mass ratio of the activated carbon to the acrylic acid monomer is 1:(0.1-1).

[0023] Furthermore, the mass ratio of the intermediate product to cellulose is 1:(0.1-1).

[0024] Furthermore, the pressing is: pressing into a cube with a side length of 1-10 mm.

[0025] The present invention has the following beneficial effects:

[0026] 1. In the process for extracting rosemary essential oil provided by the present invention, modified activated carbon is used as an adsorbent. The modified activated carbon is firstly grafted with acrylic acid monomers on the surface of the activated carbon by a surface-initiated graft polymerization method to introduce a carboxyl functional group, and then mixed with hydroxy cellulose and ultrasonically treated to form crosslinks between oxygen-containing active groups of the cellulose, and the cellulose is bound to the surface of the activated carbon by intermolecular forces and electrostatic forces, thereby introducing a polysaccharide structure, which not only improves the compatibility and affinity of the modified activated carbon with the active substances in rosemary, but also helps to increase the specific surface area of ​​the activated carbon and enhance the adsorption capacity; at the same time, the modified activated carbon increases the content of groups such as hydroxyl, ester, and carboxyl, increases the binding sites with active ingredients such as carnosic acid, rosmarinic acid, and rosmarinic phenol in rosemary, thereby significantly improving the adsorption effect of the essential oil and achieving efficient extraction and separation.

[0027] 2. The present invention performs mixed bacterial fermentation treatment on rosemary raw materials. Cellulase and protease produced by microorganisms can destroy structures such as plant cell walls and release more active ingredients, thereby increasing the adsorption capacity of activated carbon, and ultimately achieving an improvement in the yield and quality of essential oils.

[0028] 3. The present invention also presses the modified activated carbon into a cubic shape with a larger particle size, so that after the adsorption is completed, it is easy to separate from the rosemary and carry out the next step of desorption. The modified activated carbon can be recycled and reused many times, and the rosemary powder can also be used for the preparation of other products, avoiding the waste of raw materials, and has good application prospects. DETAILED DESCRIPTION

[0029] In order to more clearly illustrate the technical solution of the present invention, the following examples are listed. Unless otherwise stated, the raw materials, reactions and post-treatment methods shown in the examples are common raw materials on the market and technical methods well known to those skilled in the art.

[0030] The words "preferred", "preferably", "more preferably", etc. in the present invention refer to embodiments of the present invention that can provide certain beneficial effects in certain circumstances. However, other embodiments may also be preferred under the same circumstances or other circumstances. In addition, the description of one or more preferred embodiments does not imply that other embodiments are not applicable, nor is it intended to exclude other embodiments from the scope of the present invention.

[0031] It should be understood that, except in any operating examples, or where otherwise indicated, all numbers indicating, for example, the amounts of ingredients used in the specification and claims should be understood to be modified in all cases by the term "about". Therefore, unless indicated to the contrary, the numerical parameters set forth in the following specification and the appended claims are approximate values ​​that vary depending on the desired properties to be obtained by the present invention.

[0032] The rosemary in the embodiment of the present invention is fresh rosemary leaves.

[0033] The Monascus liquid in the embodiment of the present invention is prepared by activating and expanding Monascus (GIM 3.592, GDMCC) to prepare 1×10 6 / mL of seed solution.

[0034] The brewer's yeast culture liquid in the embodiment of the present invention is: brewer's yeast (purchased from Luzhou Longmatan District Ruihua Biological Koji Making Co., Ltd.) is activated and expanded to prepare 1×10 8 / mL of seed solution.

[0035] The method for preparing modified activated carbon in the embodiment of the present invention comprises the following steps:

[0036] L1. Add 4 parts of activated carbon (200 mesh) and 0.5 parts of methacrylic acid to 100 parts of water, then add 0.01 parts of sodium persulfate, react at 70°C for 2 hours under nitrogen atmosphere, centrifuge, wash and dry to obtain an intermediate product;

[0037] L2. Add 5 parts of the intermediate product and 0.5 parts of hydroxypropyl cellulose to 50 parts of ethanol, perform ultrasonic treatment for 2 hours, centrifuge and wash, press into a cube with a side length of 1 mm, and obtain modified activated carbon after drying.

[0038] The "parts" in the embodiments of the present invention refer to parts by mass.

[0039] Example 1

[0040] A process for extracting rosemary essential oil, characterized in that the process for extracting rosemary essential oil comprises the following steps:

[0041] S1, cutting and crushing rosemary, passing through a 200-mesh sieve, adding to a fermentation tank, adding Monascus spp. and Saccharomyces cerevisiae spp. inoculation amounts of 5% and 3%, respectively, and culturing at 37° C. for 24 h to obtain pretreated rosemary;

[0042] S2, mixing the pretreated rosemary with modified activated carbon in a mass ratio of 10:1, introducing air with a humidity of 60%, standing at 30° C. for adsorption for 48 hours, and then separating the modified activated carbon;

[0043] S3, the modified activated carbon and ether were suspended in a column (150cm×1.2cm) at a flow rate of 2cm 3 / min of ether for 2h, drying the eluate with anhydrous sodium sulfate, filtering, evaporating the solvent, obtaining rosemary essential oil, and finally recovering the modified activated carbon.

[0044] Example 2

[0045] A process for extracting rosemary essential oil, characterized in that the process for extracting rosemary essential oil comprises the following steps:

[0046] S1, cutting and crushing rosemary, passing through a 300-mesh sieve, adding to a fermentation tank, adding Monascus spp. and Saccharomyces cerevisiae spp. inoculation amounts of 5% and 3%, respectively, and culturing at 37° C. for 24 h to obtain pretreated rosemary;

[0047] S2, mixing the pretreated rosemary with modified activated carbon in a mass ratio of 10:1, introducing air with a humidity of 60%, standing at 35° C. for adsorption for 48 hours, and then separating the modified activated carbon;

[0048] S3, the modified activated carbon and ether were suspended in a column (150cm×1.2cm) at a flow rate of 2cm 3 / min of ether for 2h, drying the eluate with anhydrous sodium sulfate, filtering, evaporating the solvent, obtaining rosemary essential oil, and finally recovering the modified activated carbon.

[0049] Example 3

[0050] A process for extracting rosemary essential oil, characterized in that the process for extracting rosemary essential oil comprises the following steps:

[0051] S1, cutting and crushing rosemary, passing through a 300-mesh sieve, adding to a fermentation tank, adding Monascus spp. and Saccharomyces cerevisiae spp. inoculation amounts of 5% and 3%, respectively, and culturing at 37° C. for 24 h to obtain pretreated rosemary;

[0052] S2, mixing the pretreated rosemary with modified activated carbon in a mass ratio of 10:1, introducing air with a humidity of 50%, standing at 40° C. for adsorption for 36 hours, and then separating the modified activated carbon;

[0053] S3, the modified activated carbon and ether were suspended in a column (150cm×1.2cm) at a flow rate of 2cm 3 / min of ether for 2h, drying the eluate with anhydrous sodium sulfate, filtering, evaporating the solvent, obtaining rosemary essential oil, and finally recovering the modified activated carbon.

[0054] Comparative Example

[0055] A process for extracting rosemary essential oil. The difference between this comparative example and Example 1 is that the modified activated carbon is replaced with unmodified activated carbon, and the other processes are the same as those in Example 1.

[0056] Test Case

[0057] The essential oil yields of the processes for extracting rosemary essential oil in Examples 1-3 and Comparative Example were compared.

[0058] Sensory evaluation of each essential oil sample:

[0059] Appearance evaluation: colorless or lighter in color, clear and transparent is excellent; yellowish in color, clear and transparent is medium; turbid in color is poor;

[0060] Odor evaluation: strong and fragrant odor is excellent; aromatic odor with a slightly sour taste is medium; strong sour odor is poor.

[0061] The test results are shown in Table 1.

[0062] Table 1 Performance test results

[0063] project Example 1 Example 2 Example 3 Comparative Example Activated carbon dosage / kg 10 10 10 10 Essential oil yield / g 1446 1492 1432 1335 Appearance Assessment excellent excellent excellent excellent Odor Assessment excellent excellent excellent middle

[0064] According to Table 1, it can be seen that the process for extracting rosemary essential oil of Examples 1-3 of the present invention has a higher essential oil yield, and the essential oil sensory evaluation is good, and has good appearance and smell, while the comparative example replaces the modified activated carbon, resulting in reduced adsorption and extraction effects, and the essential oil yield is significantly reduced, and the ideal technical effect cannot be achieved. In summary, the process for extracting rosemary essential oil of the present invention solves the defects existing in the prior art and has good application prospects.

[0065] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the present invention can be implemented in other specific forms without departing from the spirit or essential features of the present invention. Therefore, the embodiments should be considered exemplary and non-restrictive in all respects, and the scope of the present invention is defined by the appended claims rather than the above description, and it is intended that all changes falling within the meaning and scope of the equivalent elements of the claims be included in the present invention.

[0066] In addition, it should be understood that although the present specification is described according to implementation modes, not every implementation mode contains only one independent technical solution. This description of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment may also be appropriately combined to form other implementation modes that can be understood by those skilled in the art.

Claims

1. A process for extracting rosemary essential oil, characterized in that, The process for extracting rosemary essential oil comprises the steps: S1, cutting, crushing and fermenting rosemary to obtain pretreated rosemary; S2, mixing the pretreated rosemary with modified activated carbon, introducing humid air, and allowing to stand for adsorption; S3, desorbing the modified activated carbon to obtain rosemary essential oil; in, The modified activated carbon is hydroxypropyl cellulose or methacrylic acid modified activated carbon; The preparation method of the modified activated carbon comprises the following steps: L1. Add 4 parts of 200-mesh activated carbon and 0.5 parts of methacrylic acid to 100 parts of water, then add 0.01 parts of sodium persulfate, react at 70°C for 2 h under nitrogen atmosphere, centrifuge, wash and dry to obtain an intermediate product; L2. Add 5 parts of the intermediate product and 0.5 parts of hydroxypropyl cellulose to 50 parts of ethanol, ultrasonically treat for 2 hours, centrifuge and wash, press into a cube with a side length of 1 mm, and obtain modified activated carbon after drying.

2. The process for extracting rosemary essential oil according to claim 1, wherein: The rosemary is selected from rosemary leaves or twigs.

3. The process for extracting rosemary essential oil according to claim 1, wherein: The fermentation adopts one or more of lactic acid bacteria, yeast and mold.

4. The process for extracting rosemary essential oil according to claim 1, wherein: The fineness of the pulverization is 200-500 meshes.

5. The process for extracting rosemary essential oil according to claim 1, wherein: The humidity of the humid air is 30-60%.

6. The process for extracting rosemary essential oil according to claim 1, characterized in that: The static adsorption time is 24-48 h, and the temperature is 30-40°C.