Method for extracting water-soluble components from rosemary, method for preparing rosemary emulsion, rosemary emulsion and application

Abstract

The invention relates to a method for extracting water-soluble components from rosemary, a method for preparing rosemary emulsion, the rosemary emulsion and application, and belongs to the technical field of rosemary extraction. The method for extracting the water-soluble components comprises the following steps: sequentially extracting rosemary essential oil and carnosic acid in rosemary dry leaves by adopting a supercritical CO2 fluid extraction technology to obtain rosemary dry leaves I; the method comprises the following steps: sealing and soaking rosemary dry leaves I in 30-60wt% ethanol for 1-3 hours, then putting the rosemary dry leaves I into an extraction kettle, introducing CO2, keeping the pressure at 20-35MPa, the extraction temperature at 30-60 DEG C and the extraction time at 4-8 hours, and collecting extract liquor; the mass ratio of the rosemary dry leaves I to the ethanol is 1: (2-15); and carrying out solid-liquid separation on the extract, and drying to obtain the water-soluble rosemary extract. The activity of the water-soluble component extracted by the method is higher, and meanwhile, the rosemary emulsion with a finer and more stable wrapping effect is obtained by matching with the method for preparing the rosemary emulsion.

Description

Technical Field

[0001] The present invention relates to a method for extracting water-soluble components from rosemary, a method for preparing rosemary emulsion, the rosemary emulsion and applications thereof, and belongs to the technical field of rosemary extraction. Background Art

[0002] In rosemary extraction methods, there are many literatures on lipophilic antioxidants such as carnosic acid and carnosol, while there are few reports on water-soluble active components such as rosemary polysaccharides, flavonoids, and polyphenols. However, various chemical components such as polysaccharides, flavonoids, and phenolic acids in rosemary have different effects. Among them, the research on flavonoid components started earlier. So far, more than 30 flavonoid compounds have been isolated from rosemary, mainly including hesperetin, apigenin, cirsimaritin, etc., which have antibacterial, anti-inflammatory, antihypertensive, antioxidant, anti-cancer and other effects.

[0003] However, there are few research reports on components such as total rosemary polysaccharides and total flavonoids at present, and the extraction rates of these types of active components are relatively low.

[0004] At present, in order to enhance the penetration performance of efficacy components in the epidermis and dermis of the skin, significantly improve the bioavailability of efficacy components, and at the same time increase the product stability, microemulsion and nanoemulsion are usually used as carrier systems. Both microemulsion and nanoemulsion belong to nanoscale colloidal dispersions. However, because the particle size of nanoemulsion is larger and has a smaller surface area, less surfactant is required during formation. According to the evaluation of the safety of rosemary-related products, when the content of surfactant required is less, the potential toxicity of the entire emulsion system will be reduced relatively a lot. Therefore, compared with microemulsion, nanoemulsion is more suitable for adding to products.

[0005] Although nanoemulsion can improve the safety of rosemary-related products, when applying rosemary extract to the daily chemical field, there are still certain requirements for the odor and stability of the product. Among them, polysaccharides are prone to moisture absorption and decomposition, and substances such as carnosic acid have herbal odors, etc., so they are not suitable for direct application in daily chemical products. Therefore, it is of great significance to develop a nanoemulsion that can improve the stability and functionality of daily chemical products. Summary of the Invention

[0006] Aiming at the problems existing in the above-mentioned prior art, one of the purposes of the present invention is to provide a method for extracting water-soluble components from rosemary, and the water-soluble components extracted by this method have higher activity.

[0007] The second object of the present invention is to provide a method for preparing rosemary emulsion. In this method, the types and dosages of substances in the oil phase and the water phase, as well as the ratio of the oil phase to the water phase, simultaneously achieve a finer and more stable encapsulation effect through the microfluidic technology, significantly improving the stability and functionality of the rosemary emulsion. Further, this method has a simple process and is easy to industrialize.

[0008] The third object of the present invention is to provide a rosemary emulsion. This emulsion has excellent stability, can protect the (active ingredients such as carnosic acid and polysaccharides) in the rosemary extract, and reduce oxidation, deterioration, etc. during storage; in addition, the compounded emulsion can enhance the penetration performance of the active ingredients in the epidermis and dermis of the skin, significantly improving the bioavailability of the active ingredients.

[0009] The fourth object of the present invention is to provide the application of the rosemary emulsion in the daily chemical field. The rosemary emulsion provided by the present invention has excellent activity and stability and can be used in the daily chemical field.

[0010] To achieve the above objects, the first aspect of the present invention is to provide a method for extracting water-soluble components from rosemary, which method includes:

[0011] (1) Using supercritical CO2 fluid extraction technology to sequentially extract rosemary essential oil and carnosic acid from dried rosemary leaves to obtain dried rosemary leaves I;

[0012] (2) Sealing and soaking the dried rosemary leaves I in ethanol with a concentration of 30-60 wt% for 1-3 h, then loading them into an extraction kettle, introducing CO2 to maintain a pressure of 20-35 MPa, with an extraction temperature of 30-60 °C and a time of 4-8 h, and collecting the extraction solution; the mass ratio of the dried rosemary leaves I to ethanol is 1:2-15;

[0013] (3) After solid-liquid separation of the extraction solution, perform drying treatment to obtain water-soluble rosemary extract.

[0014] The innovation of the present invention lies in first extracting the oil-soluble antibacterial and antioxidant components, rosemary essential oil and carnosic acid, from rosemary through supercritical CO2 fluid extraction technology, and then extracting water-soluble components, mainly polysaccharides and polyphenols, etc., through ethanol-CO2 extraction method. The extraction temperature by the ethanol extraction method is low, which can effectively improve the activity of the water-soluble components.

[0015] In a preferred embodiment, in step (2), the mass fraction of ethanol used for soaking the dry rosemary leaves I is 40-60 wt%; and the mass ratio of the dry rosemary leaves I to ethanol is 1:8-12. The inventors found that under these preferred conditions, the extraction effect is better. If the ethanol dosage is too low, the extraction of water-soluble components is incomplete or insufficient, resulting in a low extraction rate.

[0016] In a preferred embodiment, the extraction temperature is 45-60 °C. The inventors of the present invention found that under these preferred conditions, water-soluble components with higher activity can be obtained. When the temperature is higher than 60 °C, the active components of water-soluble substances will be reduced or inactivated, and when the temperature is lower than 45 °C, the extraction of water-soluble substances is not sufficient enough.

[0017] In a preferred embodiment, the temperature of the drying treatment is 50-60 °C, and the time is 3-8 h.

[0018] It should be noted that the present invention has no special requirements for the solid-liquid separation method, and conventional methods in the art can be used. Exemplarily, the supernatant of the extraction solution can be concentrated, allowed to stand, and centrifuged.

[0019] In a preferred embodiment, the steps of extracting rosemary essential oil from dry rosemary leaves by supercritical CO2 fluid extraction technology include:

[0020] The dry rosemary leaves are crushed and sieved and then loaded into the extraction kettle. CO2 is introduced to maintain a pressure of 4-6 MPa, and static extraction is carried out for 0.5-1 h. Then, the pressure of the extraction kettle is adjusted to 10-30 MPa, the temperature is 35-60 °C, and supercritical CO2 is introduced for continuous cyclic extraction for 2-4 h. The pressure in the first separation kettle is controlled at 4-6 MPa, and the temperature is 30-50 °C to separate out rosemary essential oil.

[0021] In a preferred embodiment, the pressure of the extraction kettle is 15-18 MPa, and the temperature is 40-50 °C.

[0022] In a preferred embodiment, the steps of extracting carnosic acid from dry rosemary leaves by supercritical CO2 fluid extraction technology include:

[0023] The rosemary dry leaves from which rosemary essential oil has been extracted are sealed and soaked in ethanol at 20-50 wt% for 1-3 h, then loaded into the extraction kettle. CO2 is introduced to maintain a pressure of 8-12 MPa, and static extraction is carried out for 1-2 h. Then, the pressure of the extraction kettle is adjusted to 22-50 MPa and the temperature is adjusted to 40-70 °C. Supercritical CO2 is introduced for continuous cyclic extraction for 2-4 h. The entrainer is ethanol at 50-80 wt%, and the addition amount each time is 0.2-0.5 times that of the rosemary dry leaves, with the addition frequency of once per hour. The pressure in separation kettle 1 is controlled at 8-15 MPa and the temperature at 35-55 °C; the pressure in separation kettle 2 is 4-6 MPa and the temperature is 30-40 °C, and the pressure in the rectifying column is 4-15 MPa and the temperature is 30-50 °C. The extraction liquids in separation kettle 1, separation kettle 2 and the rectifying column are collected respectively to obtain carnosic acid;

[0024] The mass ratio of the rosemary dry leaves from which rosemary essential oil has been extracted to ethanol at 20-50 wt% is 1:0.3-0.6.

[0025] In a more preferred embodiment, the rosemary dry leaves from which rosemary essential oil has been extracted are sealed and soaked in ethanol at 20-30 wt% for 1-3 h, then loaded into the extraction kettle. CO2 is introduced to maintain a pressure of 8-12 MPa, and static extraction is carried out for 1-2 h. Then, the pressure of the extraction kettle is adjusted to 22-50 MPa and the temperature is adjusted to 40-70 °C. Supercritical CO2 is introduced for continuous cyclic extraction for 2-4 h. The entrainer is ethanol at 50-60 wt%, and the addition amount each time is 0.2-0.3 times that of the rosemary dry leaves, with the addition frequency of once per hour. The pressure in separation kettle 1 is controlled at 8-15 MPa and the temperature at 35-55 °C; the pressure in separation kettle 2 is 4-6 MPa and the temperature is 30-40 °C, and the pressure in the rectifying column is 4-15 MPa and the temperature is 30-50 °C. The extraction liquids in separation kettle 1, separation kettle 2 and the rectifying column are collected respectively to obtain carnosic acid;

[0026] The mass ratio of the rosemary dry leaves from which rosemary essential oil has been extracted to ethanol at 20-30 wt% is 1:0.3-0.4. The preferred alcohol addition amount and concentration are more conducive to the extraction of carnosic acid in the natural state and prepare for supercritical extraction. Excessive addition amount is easy to adsorb and saturate, which is not conducive to the loading of the extraction kettle; high alcohol concentration will extract carnosic acid and it is easy to be oxidized in the air. At the same time, the preferred alcohol entrainer addition amount and concentration can prevent more impurity components from being extracted, and adding in batches is for extracting in small amounts and multiple times, which is conducive to improving the extraction efficiency and the purity of the active ingredient.

[0027] In a preferred embodiment, the extraction liquid of the rectifying column is concentrated under reduced pressure to obtain carnosic acid I; the extraction liquids in separation kettle 1 and separation kettle 2 are combined, then subjected to membrane separation filtration, washing and concentration to obtain a concentrated liquid. The pH value of the concentrated liquid is adjusted to 3.5-5, and n-hexane is added for reverse extraction, and then vacuum drying is carried out to obtain carnosic acid II.

[0028] In a preferred embodiment, combining the carnosic acid I and the carnosic acid II gives carnosic acid.

[0029] It should be noted that the present invention has no special requirements for the nanofiltration membrane for membrane separation, the acid used to adjust the pH value, and the amount of n-hexane, and those known in the art can be used.

[0030] The present invention also provides a method for preparing a rosemary emulsion, which method comprises:

[0031] S1: Preparing an oil phase: First mixing carnosic acid and vegetable oil to obtain Material I, and then second mixing the Material I with a surfactant and a co-surfactant to obtain an oil phase;

[0032] The mass ratio of the carnosic acid to the vegetable oil is 1:12 - 20;

[0033] And,

[0034] Preparing an aqueous phase: Dissolving a water-soluble rosemary extract in water to obtain an aqueous phase; the concentration of the water-soluble rosemary extract is 15 - 30 wt%; the water-soluble rosemary extract is the water-soluble rosemary extract prepared by the method according to any one of claims 1 - 4;

[0035] S2: Preparing a single-coated rosemary emulsion: After adding the aqueous phase to the oil phase and mixing, emulsifying at 18000 - 22000 r / min to obtain a coarse emulsion, and then circulating the coarse emulsion in a dynamic high-pressure microfluidic homogenizer 3 - 6 times to obtain a single-coated rosemary emulsion;

[0036] Based on the total amount of the oil phase and the oil phase, the amount of the oil phase is 75 - 95 wt%, and the amount of the aqueous phase is 5 - 25 wt%.

[0037] By introducing the water-soluble rosemary extract obtained by the foregoing extraction method, through the synergistic effect between various substances, and at the same time by regulating the ratio of the oil phase and the aqueous phase, the microfluidic technology not only achieves a finer and more stable encapsulation effect, but also prepares a nano rosemary emulsion with excellent stability and functionality.

[0038] In a preferred embodiment, based on the total amount of the oil phase and the oil phase, the amount of the oil phase is 80 - 95 wt%, and the amount of the aqueous phase is 5 - 20 wt%.

[0039] In a preferred embodiment, first mix carnosic acid and alcohol, heat to 40 - 60 °C, and after the carnosic acid is dissolved, then first mix with vegetable oil. After mixing, stir to evaporate the alcohol, and filter, take the filtrate to obtain Material I.

[0040] In a preferred embodiment, after the water-soluble rosemary extract is dissolved in water, it is filtered, and the filtrate is taken to obtain an aqueous phase.

[0041] In a preferred embodiment, the vegetable oil is selected from at least one of soybean oil, sunflower oil, corn oil, peanut oil, rapeseed oil, and palm oil.

[0042] In a preferred embodiment, the surfactant is selected from at least one of Tween 20, Tween 60, Tween 80, Span 20, Span 80, Span 85, mono- and diglycerides, glyceryl stearate, and lecithin.

[0043] In a preferred embodiment, the co-surfactant is selected from at least one of ethanol, propylene glycol, and polyethylene glycol.

[0044] In a preferred embodiment, based on the total amount of Material I, surfactant, co-surfactant, and aqueous phase, the amount of Material I is 50-60 wt%, the amount of the surfactant is 10-20 wt%, the amount of the co-surfactant is 10-15 wt%, and the amount of the aqueous phase is 5-20 wt%.

[0045] In a preferred embodiment, in step S1, the temperature for dissolving the water-soluble rosemary extract in water is 40-60 °C.

[0046] In a preferred embodiment, in step S2, the emulsification time is 3-5 min, and the pressure of the dynamic high-pressure microfluidic homogenizer is 40-60 MPa.

[0047] In a preferred embodiment, the method further includes preparing the single-coated rosemary emulsion into a double-coated rosemary emulsion, and the specific steps include:

[0048] Using a mixture of porous starch and β-cyclodextrin as the wall material and the single-coated rosemary emulsion prepared in step S2 as the core material, emulsifying the wall material and the core material at a temperature of 40-55 °C and a rotation speed of 18,000-22,000 r / min for 3-5 min to obtain a double-coated rosemary emulsion. The inventor found that in this preferred case, it is more capable of suppressing the herbaceous odor of substances such as carnosic acid.

[0049] In a more preferred embodiment, the mass ratio of the amount of porous starch to β-cyclodextrin is 1:0.8-1.2; the mass ratio of the amount of the core material to the wall material is 10:0.8-1.2.

[0050] The present invention also provides a rosemary emulsion prepared by the method for preparing a rosemary emulsion described above.

[0051] The present invention also provides the application of the aforementioned rosemary emulsion in the daily chemical field.

[0052] Compared with the prior art, the present invention has at least the following advantages:

[0053] (1) The traditional method mainly uses water extraction to extract water-soluble components from rosemary. However, the extraction temperature of this method is high, which will cause the active components in the water-soluble substances to be inactivated. In the present invention, first, the oil-soluble antibacterial and antioxidant components, rosemary essential oil and carnosic acid, in rosemary are extracted by supercritical CO2 fluid extraction technology, and then the water-soluble components are extracted by ethanol-CO2 extraction method, so as to obtain water-soluble extracts with higher activity and more content. This water-soluble component can absorb ultraviolet rays, prevent the formation of oxygen free radicals, and at the same time prevent the decline of the skin immune system and keratinocytes, and has the effects of repairing the skin and delaying aging, further enhancing the antibacterial, antioxidant and other anti-aging effects of the product.

[0054] (2) Compared with the conventional microemulsion process, the subsequent compounding operation or temperature change of the product will damage its internal structure. The present invention adopts the microjet technology to achieve a finer and more stable encapsulation effect, which can significantly improve the subsequent product compounding, long-term storage, temperature adaptability, etc. of this product, and the nanoemulsion provided by the present invention can further enhance the stability and functionality of the rosemary emulsion.

[0055] (3) The present invention adopts a double coating method. On the basis of single coating, different outer coating matrices can be adapted according to the subsequent compounding requirements of customers, increasing the possibility of product compounding. In addition, it can further inhibit the herbaceous odor generated by substances such as carnosic acid. BRIEF DESCRIPTION OF THE DRAWINGS

[0056] Figure 1 It is a test result diagram of the oilification of the emulsion prepared in each example. DETAILED DESCRIPTION OF THE INVENTION

[0057] The endpoints and any values disclosed in this text are not limited to the exact ranges or values. These ranges or values should be understood to include values close to these ranges or values. For numerical ranges, the endpoints of each range, between the endpoints of each range and individual point values, and between individual point values can be combined with each other to obtain one or more new numerical ranges, and these numerical ranges should be regarded as specifically disclosed in this text.

[0058] The following further describes the present invention in conjunction with specific embodiments, but the protection scope of the present invention is not limited to the following specific embodiments. Obviously, the embodiments described below are only a part of the embodiments, and all other embodiments obtained by those skilled in the art without creative efforts still fall within the protection scope of the present invention.

[0059] Unless otherwise specified, all kinds of raw materials, reagents, instruments, and equipment used in the present invention can be obtained through market purchase or can be prepared by existing methods.

[0060] The preparation examples of the present invention are used to extract carnosic acid and water-soluble rosemary extract.

[0061] Preparation Example 1

[0062] (1) Extract rosemary essential oil: Weigh 1 kg of dried rosemary leaves, crush them and pass through a 60-mesh sieve, load them into the extraction kettle, introduce CO2 to maintain a pressure of 5 MPa, set the flow rate to 15 kg / h, perform static extraction for 0.75 h, then adjust the pressure of the extraction kettle to 17 MPa and the temperature to 45 °C, introduce supercritical CO2 for continuous circulation extraction for 3 h, control the pressure in separator kettle 1 to be 5 MPa and the temperature to be 40 °C to separate out rosemary essential oil, and obtain 43.6 g of rosemary essential oil;

[0063] (2) Extract carnosic acid: Release the pressure of the extraction kettle after extracting the essential oil, take out the rosemary powder, add 0.4 times 25 wt% ethanol, mix evenly, seal and soak for 3 h, then load it into the extraction kettle, introduce CO2 to maintain a pressure of 10 MPa, perform static extraction for 1.5 h, then adjust the pressure of the extraction kettle to 30 MPa and the temperature to 50 °C, introduce supercritical CO2 for continuous circulation extraction for 4 h, where the entrainer is 55 wt% ethanol, the addition amount each time is 0.25 times that of the dried rosemary leaves, and the addition frequency is once per hour, control the pressure in separator kettle 1 to be 10 MPa and the temperature to be 40 °C; the pressure in separator kettle 2 to be 5 MPa and the temperature to be 35 °C, and the pressure in the rectification column to be 8 MPa and the temperature to be 40 °C. Collect the extraction liquids in separator kettle 1, separator kettle 2, and the rectification column respectively. Vacuum concentrate the extraction liquid in the rectification column to obtain 4.3 g of carnosic acid I; Combine the extraction liquids collected from separator kettle 1 and separator kettle 2, pass them through a nanofiltration membrane with a molecular weight cut-off of 300 - 500, reduce the pressure and concentrate to recover half of the solvent to obtain a concentrated liquid, adjust the pH = 4 with hydrochloric acid, add 5 times n-hexane for reverse extraction, combine the extraction liquids and vacuum concentrate to obtain 5.9 g of carnosic acid II; Combine carnosic acid I and carnosic acid II to obtain carnosic acid A;

[0064] (3) Extract water-soluble components: Release the pressure of the extraction kettle after extracting carnosic acid, take out the rosemary powder, add 55 wt% alcohol with a mass 11 times that of the dried rosemary leaves, seal and soak for 2 h, then load it into the extraction kettle, set the extraction temperature to 60 °C, introduce CO2 to maintain a pressure of 30 MPa, continue to extract for 5 h, collect the extraction liquid, centrifuge 3 times, concentrate the supernatant, let it stand, centrifuge again, and place it in an oven at 60 °C to dry for 5 h to obtain 153.8 g of water-soluble rosemary extract A containing rosemary polysaccharide, polyphenol, etc.

[0065] Preparation Example 2

[0066] (1) Extraction of rosemary essential oil: Weigh 1 kg of dried rosemary leaves, crush them and sieve through a 60-mesh sieve. Load them into the extraction kettle, introduce CO2 to maintain a pressure of 4 MPa, set the flow rate at 15 kg / h, perform static extraction for 1 h. Then adjust the pressure in the extraction kettle to 18 MPa and the temperature to 50 °C, and introduce supercritical CO2 for continuous cyclic extraction for 3 h. Control the pressure in separator kettle 1 at 4 MPa and the temperature at 50 °C to separate the rosemary essential oil; 44.3 g of rosemary essential oil is obtained.

[0067] (2) Extraction of carnosic acid: Depressurize the extraction kettle after extracting the essential oil, take out the rosemary powder, add 0.4 times of 30 wt% ethanol, mix evenly, seal and soak for 3 h, introduce CO2 to maintain a pressure of 8 MPa, perform static extraction for 2 h. Then adjust the pressure in the extraction kettle to 40 MPa and the temperature to 50 °C, and introduce supercritical CO2 for continuous cyclic extraction for 2.5 h. The entrainer is 55 wt% ethanol, and the addition amount each time is 0.3 times that of the dried rosemary leaves, with the addition frequency of once per hour. Control the pressure in separator kettle 1 at 12 MPa and the temperature at 40 °C; the pressure in separator kettle 2 at 6 MPa and the temperature at 30 °C, and the pressure in the rectifying column at 8 MPa and the temperature at 45 °C. Collect the extraction liquids in separator kettle 1, separator kettle 2 and the rectifying column respectively. Vacuum-concentrate the extraction liquid in the rectifying column to obtain 4.9 g of carnosic acid I; Combine the extraction liquids collected from separator kettle 1 and separator kettle 2, pass them through a nanofiltration membrane with a molecular weight cut-off of 300 - 500, and concentrate under reduced pressure to recover half of the solvent to obtain a concentrated liquid. Adjust the pH = 4 with hydrochloric acid, add 5 times of n-hexane for reverse extraction, combine the extraction liquids and vacuum-concentrate to obtain 6.1 g of carnosic acid II; Combine carnosic acid I and carnosic acid II to obtain carnosic acid B.

[0068] (3) Extraction of water-soluble components:

[0069] Depressurize the extraction kettle after extracting carnosic acid, take out the rosemary powder, add 60 wt% alcohol with a mass 10 times that of the dried rosemary leaves, seal and soak for 3 h, then load it into the extraction kettle. Set the extraction temperature at 50 °C, introduce CO2 to maintain a pressure at 25 MPa, continue extraction for 8 h, collect the extraction liquid, centrifuge 3 times, concentrate the supernatant, let it stand, centrifuge again, and dry in an oven at 60 °C for 5 h to obtain 142.1 g of water-soluble rosemary extract B containing rosemary polysaccharide, polyphenol, etc.

[0070] Preparation Example 3

[0071] This preparation example is carried out by referring to a similar method as in Preparation Example 1. The difference is that in step (3), 55 wt% alcohol with a mass 7 times that of the dried rosemary leaves is added to the rosemary powder to obtain 118.2 g of water-soluble rosemary extract C containing rosemary polysaccharide, polyphenol, etc.

[0072] Comparative Preparation Example 1

[0073] Step (1) is the same as Preparation Example 1;

[0074] Step (2) is the same as Preparation Example 1;

[0075] Step (3): Depressurize the extraction kettle that has extracted carnosic acid, take out the rosemary powder, add boiling water with a mass 11 times that of the dry rosemary leaves, and extract for 5 h to obtain 1167.6 g of water-soluble rosemary extract containing rosemary polysaccharides, polyphenols, etc., namely D.

[0076] The examples of the present invention are used to prepare rosemary emulsion.

[0077] Example 1

[0078] S1: Prepare the oil phase: Dissolve 40 g of oil-soluble carnosic acid A in alcohol, heat to 50 °C and stir continuously. After complete dissolution, add 580 g of soybean oil, stir well and then evaporate the alcohol, and filter to obtain the filtrate; obtain Material I.

[0079] Then take 550 g of Material I, 150 g of Tween 20 and 150 g of propylene glycol, stir and mix them well to form a mixed solution, thus forming the oil phase.

[0080] S2: Prepare the water phase: Weigh 35 g of water-soluble rosemary extract A, dissolve it in 115 g of water, heat to 60 °C and stir continuously until completely dissolved, then filter to obtain the filtrate, thus forming the water phase.

[0081] S3: Prepare the single-coated rosemary emulsion: Slowly add the water phase to the oil phase, emulsify with a high-speed disperser (20000 r / min, 4 min) to obtain a crude emulsion, and then circulate the crude emulsion through a dynamic high-pressure microfluidic homogenizer at 60 MPa for 4 times to obtain a single-coated nanoemulsion, cool it to room temperature and set it aside for use.

[0082] S4: Prepare the double-coated rosemary emulsion: Take 100 g of the single-coated nanoemulsion as the core material, and take 500 g of porous starch and 500 g of β-cyclodextrin as the wall materials, and emulsify with a high-speed disperser at 50 °C (20000 r / min, 4 min) to obtain a secondary-coated emulsion.

[0083] Example 2

[0084] S1: Prepare the oil phase: Dissolve 32 g of oil-soluble carnosic acid B in alcohol, heat to 50 °C and stir continuously. After complete dissolution, add 617 g of soybean oil, stir well and then evaporate the alcohol, and filter to obtain the filtrate; obtain Material I.

[0085] Then take 600 g of Material I, 140 g of Tween 20 and 140 g of propylene glycol, stir and mix them well to form a mixed solution, thus forming the oil phase.

[0086] S2: Prepare the aqueous phase: Weigh 33 g of water-soluble rosemary extract B and dissolve it in 87 g of water. Heat the solution to 60 °C and continuously stir until it is fully dissolved. Then, filter the solution and collect the filtrate to form the aqueous phase.

[0087] S3: Prepare the single-coated rosemary emulsion: Slowly add the aqueous phase to the oil phase and emulsify it with a high-speed disperser (20000 r / min, 4 min) to obtain a crude emulsion. Then, circulate the crude emulsion through a dynamic high-pressure microfluidizer at 60 MPa for 4 times to obtain a single-coated nanoemulsion. Cool the nanoemulsion to room temperature and set it aside for use.

[0088] S4: Prepare the double-coated rosemary emulsion: Take 100 g of the single-coated nanoemulsion as the core material and 530 g of porous starch and 470 g of β-cyclodextrin as the wall materials. Emulsify them with a high-speed disperser at 50 °C (20000 r / min, 4 min) to obtain a secondary-coated emulsion.

[0089] Example 3

[0090] Step S1 is the same as that in Example 1;

[0091] Step S2 is carried out by referring to a similar method in Example 1. The difference is that the water-soluble rosemary extract A is replaced with an equal mass of water-soluble rosemary extract C;

[0092] Step S3 is the same as that in Example 1;

[0093] Step S4 is the same as that in Example 1 to obtain a secondary-coated emulsion.

[0094] Example 4

[0095] S1: Prepare the oil phase: Take 40 g of oil-soluble carnosic acid A and dissolve it in alcohol. Heat the solution to 50 °C and continuously stir. After complete dissolution, add 580 g of soybean oil, stir well, evaporate the alcohol, filter the solution, and collect the filtrate to obtain Material I.

[0096] Then, take 500 g of Material I and mix it well with 150 g of Tween 20 and 100 g of propylene glycol to form a mixed solution, which is the oil phase.

[0097] S2: Prepare the aqueous phase: Weigh 58.25 g of water-soluble rosemary extract A and dissolve it in 191.75 g of water. Heat the solution to 60 °C and continuously stir until it is fully dissolved. Then, filter the solution and collect the filtrate to form the aqueous phase.

[0098] Step S3 is the same as that in Example 1;

[0099] Step S4 is the same as that in Example 1 to obtain a secondary-coated emulsion.

[0100] Example 5

[0101] Step S1 is the same as that in Example 1;

[0102] Step S2 is the same as that in Example 1;

[0103] S3: Preparation of single-coated rosemary emulsion: Gradually add the water-soluble mixture to the oil-soluble mixture while stirring to obtain a rosemary microemulsion.

[0104] Comparative Example 1

[0105] Step S1 is the same as that in Example 1;

[0106] Step S2 is carried out by referring to a method similar to that in Example 1. The difference is that the water-soluble rosemary extract A is replaced with an equal mass of water-soluble rosemary extract D-1;

[0107] Step S3 is the same as that in Example 1;

[0108] Step S4 is the same as that in Example 1 to obtain a double-coated emulsion.

[0109] Comparative Example 2

[0110] Step S1 is the same as that in Example 1;

[0111] S2: Preparation of the aqueous phase: Weigh 150 water to form the aqueous phase.

[0112] Step S3 is the same as that in Example 1;

[0113] Step S4 is the same as that in Example 1 to obtain a double-coated emulsion.

[0114] Test Example

[0115] Perform a water solubility content test on the water-soluble rosemary extract prepared in the above preparation examples. The test results are shown in Table 1.

[0116] Perform an oil oxidation test on the emulsion prepared in the above examples. The test instrument is: Metrohm Oxidation Stability Tester 892. Determine the induction time (Induction Period, IP) of the oxidation process by continuously monitoring the change in conductivity, that is, the time period from the start of oxidation to the rapid increase in oxidation products.

[0117] The test conditions are a temperature of 110 °C, a calibration temperature of 1.5 °C, an air flow rate of 20 L / h, a sample weighing of 5 g, 60 ml of deionized water, and a sample addition amount of 200 ppm. The test results are shown in Table 2 and Figure 1 .

[0118] Table 1

[0119] Total polysaccharide (wt%) Total polyphenol (wt%) Total flavonoid (wt%) Total amount (wt%) Preparation Example 1 9.69％ 2.23％ 3.82％ 15.74 Preparation Example 2 9.33％ 2.86％ 4.21％ 16.4 Preparation Example 3 8.65％ 1.96％ 3.65％ 14.26 Comparative Preparation Example 1 10.4％ 0.75％ 1.07％ 12.22

[0120] Table 2

[0121] Induction time / h Blank control 5.08 Example 1 14.99 Example 2 14.66 Example 3 14.60 Example 4 14.29 Example 5 13.83 Comparative Example 1 11.79 Comparative Example 2 9.70

[0122] As can be seen from Table 1, when extracting water-soluble rosemary extract by the method provided by the present invention, the total amount extracted is more. From Table 2 and Figure 1 it can be seen that the induction time of the emulsion oxidation process provided by the present invention is more than 13 h, indicating that the rosemary emulsion prepared by using the water-soluble rosemary extract provided by the present invention as the raw material of the rosemary emulsion and in combination with the preparation method of the present application has excellent antioxidant properties and stability.

[0123] The preferred embodiments of the present invention have been described in detail above. However, the present invention is not limited thereto. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solutions of the present invention, including any other suitable combination of each technical feature. These simple modifications and combinations should also be regarded as the content disclosed by the present invention and fall within the protection scope of the present invention.

Claims

1. A method for extracting water-soluble components from rosemary, characterized in that: The method comprises the following steps: (1) Using supercritical CO2 fluid extraction technology to sequentially extract rosemary essential oil and carnosic acid from dry rosemary leaves to obtain dry rosemary leaves I; (2) Sealing and soaking the dry rosemary leaves I in ethanol with a concentration of 30 - 60 wt% for 1 - 3 h, then loading them into an extraction kettle, introducing CO2 to maintain a pressure of 20 - 35 MPa, with an extraction temperature of 30 - 60 °C and a time of 4 - 8 h, and collecting the extraction solution; the mass ratio of the dry rosemary leaves I to ethanol is 1:2 - 15; (3) Separating the solid and liquid of the extraction solution and then performing a drying treatment to obtain a water-soluble rosemary extract.

2. The method for extracting water-soluble components from rosemary according to claim 1, characterized in that: In step (2), the mass fraction of ethanol used for soaking the dry rosemary leaves I is 50 - 60 wt%; and the mass ratio of the dry rosemary leaves I to ethanol is 1:8 - 12; and / or, the extraction temperature is 45 - 60 °C.

3. A method for extracting water-soluble components from rosemary according to claim 1 or 2, characterized in that: The steps of using supercritical CO2 fluid extraction technology to extract rosemary essential oil from dry rosemary leaves include: After the dry rosemary leaves are crushed and sieved, they are loaded into an extraction kettle, CO2 is introduced to maintain a pressure of 4 - 6 MPa, and static extraction is carried out for 0.5 - 1 h. Then, the pressure of the extraction kettle is adjusted to 10 - 30 MPa, the temperature is 35 - 60 °C, and supercritical CO2 is introduced for continuous cyclic extraction for 2 - 4 h. The pressure in separation kettle I is controlled at 4 - 6 MPa, and the temperature is 30 - 50 °C to separate out rosemary essential oil; Preferably, the pressure of the extraction kettle is 15 - 18 MPa, and the temperature is 40 - 50 °C.

4. The method for extracting water-soluble components from rosemary according to claim 1 or 3, characterized in that: The steps of using supercritical CO2 fluid extraction technology to extract carnosic acid from dry rosemary leaves include: The dry rosemary leaves from which rosemary essential oil has been extracted are sealed and soaked in ethanol with a concentration of 20 - 50 wt% for 1 - 3 h, then loaded into an extraction kettle, CO2 is introduced to maintain a pressure of 8 - 12 MPa, and static extraction is carried out for 1 - 2 h. Then, the pressure of the extraction kettle is adjusted to 22 - 50 MPa, the temperature is adjusted to 40 - 70 °C, and supercritical CO2 is introduced for continuous cyclic extraction for 2 - 4 h. The entrainer is ethanol with a concentration of 50 - 80 wt%, the amount added each time is 0.2 - 0.5 times that of the dry rosemary leaves, and the addition frequency is once per hour. The pressure in separation kettle I is controlled at 8 - 15 MPa, and the temperature is 35 - 55 °C; the pressure in separation kettle II is 4 - 6 MPa, and the temperature is 30 - 40 °C; the pressure in the rectification column is 4 - 15 MPa, and the temperature is 30 - 50 °C. The extraction solutions in separation kettle I, separation kettle II, and the rectification column are respectively collected to obtain carnosic acid; The mass ratio of the dry rosemary leaves from which rosemary essential oil has been extracted to 20 - 50 wt% ethanol is 1:0.3 - 0.

6.

5. A method for preparing rosemary emulsion, characterized in that: The method comprises the following steps: S1: Preparing an oil phase: First, mixing carnosic acid and vegetable oil to obtain material I, and then mixing the material I with a surfactant and a co-surfactant to obtain an oil phase; The mass ratio of carnosic acid to the vegetable oil is 1:12 - 20; And, Preparation of aqueous phase: Dissolve the water-soluble rosemary extract in water to obtain the aqueous phase; the concentration of the water-soluble rosemary extract is 15-30 wt%; the water-soluble rosemary extract is the water-soluble rosemary extract prepared by the method described in any one of claims 1-4; S2: Preparation of single-coated rosemary emulsion: After adding the aqueous phase to the oil phase and mixing, emulsify at 18000-22000 r / min to obtain a crude emulsion, and then circulate the crude emulsion 3-6 times in a dynamic high-pressure microfluidic homogenizer to obtain a single-coated rosemary emulsion; Based on the total amount of the oil phase and the oil phase, the amount of the oil phase is 75-95 wt%, and the amount of the aqueous phase is 5-25 wt%.

6. A method for preparing a rosemary emulsion according to claim 5, characterized in that: The vegetable oil is selected from at least one of soybean oil, sunflower oil, corn oil, peanut oil, rapeseed oil, and palm oil; And / or, the surfactant is selected from at least one of Tween 20, Tween 60, Tween 80, Span 20, Span 80, Span 85, mono- and diglycerides, glyceryl stearate, and lecithin; And / or, the co-surfactant is selected from at least one of ethanol, propylene glycol, and polyethylene glycol.

7. A method for preparing rosemary emulsion according to claim 5 or 6, characterized in that: Based on the total amount of Material I, surfactant, co-surfactant, and aqueous phase, the amount of Material I is 50-60 wt%, the amount of the surfactant is 10-20 wt%, the amount of the co-surfactant is 10-15 wt%, and the amount of the aqueous phase is 5-20 wt%; And / or, in step S1, the temperature for dissolving the water-soluble rosemary extract in water is 40-60 °C; And / or, in step S2, the emulsification time is 3-5 min, and the pressure of the dynamic high-pressure microfluidic homogenizer is 40-60 MPa.

8. A method for preparing a rosemary emulsion according to claim 5 or 6, characterized in that: This method further includes preparing the single-coated rosemary emulsion into a double-coated rosemary emulsion, and the specific steps include: Using the mixture of porous starch and β-cyclodextrin as the wall material, and the single-coated rosemary emulsion prepared in step S2 as the core material, emulsify the wall material and the core material at a temperature of 40-55 °C and a rotation speed of 18000-22000 r / min for 3-5 min to obtain a double-coated rosemary emulsion; Preferably, the mass ratio of the amount of porous starch to β-cyclodextrin is 1:0.8-1.2; the mass ratio of the amount of the core material to the wall material is 10:0.8-1.

2.

9. A rosemary emulsion prepared by the method for preparing a rosemary emulsion according to any one of claims 5-8.

10. Use of the rosemary emulsion according to claim 9 in the daily chemical field.

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