Preparation method and application of mangnolia officinalis extract

Abstract

The invention belongs to the technical field of medicine extraction, and discloses a preparation method and application of a mangnolia officinalis extract. The preparation method is characterized by comprising the following steps: adding a weak base reagent into officinal magnolia bark coarse powder, freezing, and grinding; and adding a mixed solution of ethanol and ethyl acetate for ultrasonic extraction, carrying out solid-liquid separation, collecting a separation liquid, and removing a solvent from the separation liquid to prepare the magnolia officinalis extract. By adding the weak base reagent and freezing treatment, the damage to active substances in the mangnolia officinalis powder in the grinding process can be effectively reduced, the mangnolia officinalis raw material can be ground to be small in particle size, and the active components are not affected. And then the mangnolia officinalis powder with smaller particle size is extracted from the mangnolia officinalis by adopting a mixed solution of ethanol and ethyl acetate, and the proportion of the two solvents is controlled, so that the antibacterial effect and the oxidation resistance of the mangnolia officinalis extract can be remarkably improved.

Description

Technical Field

[0001] The invention belongs to the technical field of drug extraction, and particularly relates to a preparation method of a magnolia bark extract and application thereof. Background Art

[0002] Magnolia officinalis (scientific name: Magnolia officinalis) is a common Chinese medicinal material, belonging to the genus Magnolia of the Magnoliaceae family. Its bark, leaves and fruits can all be used as medicine, among which the bark is the most commonly used. Magnolia bark is called "Magnolia officinalis" in traditional Chinese medicine. It has the effects of drying dampness and resolving phlegm, promoting qi and relieving fullness. It is often used to treat symptoms such as chest and abdominal distension, vomiting and diarrhea, and phlegm and cough. The main components of Magnolia officinalis include volatile oils, alkaloids, phenolic compounds, etc., which give it pharmacological effects. In modern medical research, Magnolia officinalis has also been found to have multiple biological activities such as anti-inflammatory, antibacterial, and anti-tumor.

[0003] Magnolia bark extract is an extract preparation obtained by extracting Magnolia bark, which contains a variety of bioactive ingredients, such as magnolol and honokiol. As a traditional Chinese medicinal material, Magnolia bark has a long history and has long been recorded in Chinese medical classics. It is mainly used to treat symptoms such as dampness blocking the middle jiao and phlegm and dampness in the lungs. With the development of modern extraction technology, Magnolia bark extract is increasingly used in skin care products, medicine, health care products and other fields. For example, in the skin care industry, Magnolia bark extract can improve skin color and has the effects of moisturizing, detoxifying, anti-aging, skin whitening and anti-inflammatory. For example, it can promote blood circulation in the body, help remove free radicals, and inhibit cell peroxidation, thereby achieving an anti-aging effect; at the same time, the antioxidant properties of Magnolia bark extract enhance the skin's luster and help whiten the skin. In addition, the anti-inflammatory properties of Magnolia bark extract are also used in anti-acne skin care products.

[0004] There are various production processes for Magnolia bark extracts. Common extraction methods include decoction, alcohol extraction, supercritical fluid extraction, and microwave-assisted extraction. Antioxidant and antibacterial properties are two of the most important effects of Magnolia bark extracts. How to balance these two effects and prepare Magnolia bark extracts with high antioxidant and antibacterial properties is of great significance for its application. Summary of the invention

[0005] The present invention aims to solve at least one of the technical problems existing in the above-mentioned prior art. To this end, the present invention provides a preparation method of a Magnolia bark extract and its application. The Magnolia bark extract prepared by the present invention has high antioxidant and antibacterial properties, and can better meet the application in the fields of skin care products, medicines, health care products, etc.

[0006] A first aspect of the present invention provides a method for preparing a Magnolia bark extract.

[0007] Specifically, a method for preparing a Magnolia officinalis extract comprises the following steps: A weak base reagent is added to the coarse powder of Magnolia officinalis, and the powder is ground after being frozen; a mixed solution of ethanol and ethyl acetate is added for ultrasonic extraction, and a separated liquid is collected by solid-liquid separation, and the separated liquid is desolventized to obtain a Magnolia officinalis extract.

[0008] In some embodiments, the coarse magnolia bark powder is a magnolia bark powder obtained by passing through a 10-40 mesh sieve, such as a 10 or 20 mesh sieve. There is no particular requirement for the particle size of the coarse magnolia bark powder, but it should not be too fine. Because if an inappropriate crushing and grinding method is used to obtain ultrafine magnolia bark powder, a large amount of active ingredients will be lost, thereby affecting the antioxidant and antibacterial properties of the final extract.

[0009] Preferably, the weak base reagent includes at least one of sodium carbonate, potassium carbonate, borax, calcium carbonate, sodium bicarbonate, and potassium bicarbonate.

[0010] Preferably, the amount of the weak base reagent added is 0.5%-8% of the mass of the Magnolia bark powder; further preferably, the amount of the weak base reagent added is 0.5%-5% of the mass of the Magnolia bark powder.

[0011] Preferably, the temperature of the freezing treatment is -20°C to -5°C, and the time of the freezing treatment is 10 min-40 min; further preferably, the temperature of the freezing treatment is -18°C to -8°C, and the time of the freezing treatment is 10 min-30 min.

[0012] Preferably, the grinding process is grinding to a particle size D90 of 25 μm-80 μm; further preferably, the grinding process is grinding to a particle size D90 of 25 μm-60 μm.

[0013] Preferably, the mixed solution of ethanol and ethyl acetate contains ethanol and ethyl acetate; the mass ratio of the ethanol to the ethyl acetate is 1:(0.2-5); further preferably, the mass ratio of the ethanol to the ethyl acetate is 1:(0.25-4); more preferably, the mass ratio of the ethanol to the ethyl acetate is 1:(0.6-1.5).

[0014] Preferably, the ultrasonic extraction process is carried out at a temperature of 40°C-55°C and an ultrasonic power of 100W-200W for 30min-60min; further preferably, the ultrasonic extraction process is carried out at a temperature of 40°C-50°C and an ultrasonic power of 120W-180W for 40min-60min.

[0015] A second aspect of the present invention provides a Magnolia bark extract.

[0016] Specifically, a Magnolia bark extract is prepared by the above preparation method.

[0017] The third aspect of the present invention provides the use of the above-mentioned Magnolia Bark Extract.

[0018] Specifically, the above-mentioned Magnolia bark extract is used in the preparation of skin care products, medicines or health care products.

[0019] Compared with the prior art, the beneficial effects of the present invention are as follows: The preparation method of the Magnolia officinalis extract provided by the present invention comprises the following steps: firstly adding a weak base reagent to the Magnolia officinalis coarse powder, grinding the Magnolia officinalis coarse powder after freezing treatment; and then adding a mixed solution of ethanol and ethyl acetate for ultrasonic extraction. The addition of the weak base reagent and freezing treatment can effectively reduce the damage to the active substances in the Magnolia officinalis powder during the grinding process, and the Magnolia officinalis raw material can be ground to a smaller particle size without affecting the active ingredients. Then, the Magnolia officinalis coarse powder with a smaller particle size is extracted from the Magnolia officinalis coarse powder using a mixed solution of ethanol and ethyl acetate, and the ratio of the two solvents is controlled, so that the antibacterial effect and antioxidant property of the Magnolia officinalis coarse extract can be significantly improved. DETAILED DESCRIPTION

[0020] In order to make the technical scheme of the present invention more clearly understood by those skilled in the art, the following embodiments are listed for illustration. It should be pointed out that the following embodiments do not limit the protection scope of the present invention.

[0021] Unless otherwise specified, the raw materials, reagents or devices used in the following examples can be obtained from conventional commercial sources or by existing known methods.

[0022] Example 1 A method for preparing a Magnolia officinalis extract comprises the following steps: Weigh 20g of coarse Magnolia officinalis powder that has passed through a 20-mesh sieve and place it in a triangular flask, add 0.2g of weak alkaline reagent sodium carbonate (1%), then freeze it at -10°C for 15 minutes, grind it to a powder particle size D90 of 40μm (detected by a particle size analyzer, the same below); then add a mixed solution of ethanol and ethyl acetate (the mass ratio of ethanol to ethyl acetate is 3:2) at a solid-liquid ratio of 1:10 (g / mL), and ultrasonicate for 45min at a temperature of 50°C (ultrasonic power of 150W). After extraction, filter it while hot and collect the separated liquid, wash the filter residue with a mixed solution of ethanol and ethyl acetate, filter it, repeat 3 times, and combine the separated liquid obtained after filtration. Finally, the combined separated liquid is evaporated by rotary evaporation to remove the solvent to obtain Magnolia officinalis extract.

[0023] Example 2 A method for preparing a Magnolia officinalis extract comprises the following steps: Weigh 20g of coarse powder of Magnolia officinalis passed through a 20-mesh sieve and place it in a triangular flask, add 0.2g of weak alkaline reagent sodium carbonate (1%), then freeze it at -10℃ for 15 minutes, grind it to a powder particle size D90 of 40μm (detected by a particle size analyzer, the same below); then add a mixed solution of ethanol and ethyl acetate (the mass ratio of ethanol to ethyl acetate is 2:3) at a solid-liquid ratio of 1:10 (g / mL), ultrasonicate for 45min at a temperature of 50℃ (ultrasonic power is 150W), filter it while hot after extraction and collect the separated liquid, wash the filter residue with a mixed solution of ethanol and ethyl acetate, filter it, repeat 3 times, and combine the separated liquid obtained after filtration. Finally, the combined separated liquid is evaporated by rotary evaporation to remove the solvent to obtain Magnolia officinalis extract.

[0024] Example 3 A method for preparing a Magnolia officinalis extract comprises the following steps: Weigh 20g of coarse Magnolia officinalis powder that has passed through a 20-mesh sieve and place it in a triangular flask, add 0.2g of weak alkaline reagent sodium carbonate (1%), then freeze it at -10°C for 15 minutes, grind it to a powder particle size D90 of 40μm (detected by a particle size analyzer, the same below); then add a mixed solution of ethanol and ethyl acetate (the mass ratio of ethanol to ethyl acetate is 1:4) at a solid-liquid ratio of 1:10 (g / mL), and ultrasonicate for 45min at a temperature of 50°C (ultrasonic power of 150W). After extraction, filter it while hot and collect the separated liquid, wash the filter residue with a mixed solution of ethanol and ethyl acetate, filter it, repeat 3 times, and combine the separated liquids obtained after filtration. Finally, the combined separated liquids are evaporated by rotary evaporation to remove the solvent to obtain Magnolia officinalis extract.

[0025] Example 4 A method for preparing a Magnolia officinalis extract comprises the following steps: Weigh 20g of coarse powder of Magnolia officinalis passed through a 20-mesh sieve and place it in a triangular flask, add 0.2g of weak alkaline reagent sodium carbonate (1%), then freeze it at -10℃ for 15 minutes, grind it to a powder particle size D90 of 40μm (detected by a particle size analyzer, the same below); then add a mixed solution of ethanol and ethyl acetate (the mass ratio of ethanol to ethyl acetate is 4:1) at a solid-liquid ratio of 1:10 (g / mL), ultrasonicate for 45min at a temperature of 50℃ (ultrasonic power is 150W), filter it while hot after extraction and collect the separated liquid, wash the filter residue with a mixed solution of ethanol and ethyl acetate, filter it, repeat 3 times, and combine the separated liquid obtained after filtration. Finally, the combined separated liquid is evaporated by rotary evaporation to remove the solvent to obtain Magnolia officinalis extract.

[0026] Example 5 A method for preparing a Magnolia officinalis extract comprises the following steps: Weigh 20g of coarse Magnolia officinalis powder that has passed through a 20-mesh sieve and place it in a triangular flask, add 0.3g of weak alkaline reagent sodium bicarbonate (1.5%), then freeze it at -8°C for 15 minutes, grind it to a powder particle size D90 of 50μm (detected by a particle size analyzer, the same below); then add a mixed solution of ethanol and ethyl acetate (the mass ratio of ethanol to ethyl acetate is 3:2) at a solid-liquid ratio of 1:15 (g / mL), and ultrasonicate for 40min at a temperature of 55°C (ultrasonic power of 140W). After extraction, filter it while hot and collect the separated liquid, wash the filter residue with a mixed solution of ethanol and ethyl acetate, filter it, repeat 3 times, and combine the separated liquid obtained after filtration. Finally, the combined separated liquid is evaporated by rotary evaporation to remove the solvent to obtain Magnolia officinalis extract.

[0027] Example 6 A method for preparing a Magnolia officinalis extract comprises the following steps: Weigh 20g of coarse powder of Magnolia officinalis passed through a 20-mesh sieve and place it in a triangular bottle, add 0.3g of weak alkaline reagent borax (1.0%), then freeze it at -8℃ for 12 minutes, grind it to a powder particle size D90 of 40μm (detected by a particle size analyzer, the same below); then add a mixed solution of ethanol and ethyl acetate (the mass ratio of ethanol to ethyl acetate is 3:2) at a solid-liquid ratio of 1:20 (g / mL), ultrasonicate for 40min at a temperature of 50℃ (ultrasonic power is 150W), filter it while hot after extraction and collect the separated liquid, wash the filter residue with a mixed solution of ethanol and ethyl acetate, filter it, repeat 3 times, and combine the separated liquid obtained after filtration. Finally, the combined separated liquid is evaporated by rotary evaporation to remove the solvent to obtain Magnolia officinalis extract.

[0028] Comparative Example 1 A method for preparing a Magnolia officinalis extract comprises the following steps: Weigh 20g of coarse powder of Magnolia officinalis passed through a 20-mesh sieve and place it in a triangular flask, add 0.2g of weak alkaline reagent sodium carbonate (1%), then freeze it at -10℃ for 15 minutes, grind it to a powder particle size D90 of 40μm (detected by a particle size analyzer, the same below); then add ethanol at a solid-liquid ratio of 1:10 (g / mL), ultrasonicate for 45min at a temperature of 50℃ (ultrasonic power of 150W), filter it while hot after extraction and collect the separated liquid, wash the filter residue with a mixed solution of ethanol and ethyl acetate, filter it, repeat 3 times, and combine the separated liquid obtained after filtration. Finally, the combined separated liquid is evaporated by rotary evaporation to remove the solvent to obtain Magnolia officinalis extract.

[0029] Comparative Example 2 A method for preparing a Magnolia officinalis extract comprises the following steps: Weigh 20g of coarse powder of Magnolia officinalis passed through a 20-mesh sieve and place it in a triangular flask, add 0.2g of weak alkaline reagent sodium carbonate (1%), then freeze it at -10℃ for 15 minutes, grind it to a powder particle size D90 of 40μm (detected by a particle size analyzer, the same below); then add ethyl acetate at a solid-liquid ratio of 1:10 (g / mL), ultrasonicate for 45min at a temperature of 50℃ (ultrasonic power of 150W), filter it while hot after extraction and collect the separated liquid, wash the filter residue with a mixed solution of ethanol and ethyl acetate, filter it, repeat 3 times, and combine the separated liquid obtained after filtration. Finally, the combined separated liquid is evaporated by rotary evaporation to remove the solvent to obtain Magnolia officinalis extract.

[0030] Comparative Example 3 A method for preparing a Magnolia officinalis extract comprises the following steps: Weigh 20g of coarse powder of Magnolia officinalis passed through a 20-mesh sieve and place it in a triangular flask, add 0.2g of weak alkaline reagent sodium carbonate (1%), then freeze it at -10℃ for 15 minutes, grind it to a powder particle size D90 of 40μm (detected by a particle size analyzer, the same below); then add a mixed solution of ethanol and ethyl acetate (the mass ratio of ethanol to ethyl acetate is 10:1) at a solid-liquid ratio of 1:10 (g / mL), ultrasonicate for 45min at a temperature of 50℃ (ultrasonic power is 150W), filter it while hot after extraction and collect the separated liquid, wash the filter residue with a mixed solution of ethanol and ethyl acetate, filter it, repeat 3 times, and combine the separated liquid obtained after filtration. Finally, the combined separated liquid is evaporated by rotary evaporation to remove the solvent to obtain Magnolia officinalis extract.

[0031] Comparative Example 4 A method for preparing a Magnolia officinalis extract comprises the following steps: Weigh 20g of coarse Magnolia officinalis powder that has passed through a 20-mesh sieve and place it in a triangular bottle, then freeze it at -10°C for 15 minutes, grind it to a powder particle size D90 of 40μm (detected by a particle size analyzer, the same below); then add a mixed solution of ethanol and ethyl acetate (the mass ratio of ethanol to ethyl acetate is 3:2) at a solid-liquid ratio of 1:10 (g / mL), and ultrasonicate for 45min at a temperature of 50°C (ultrasonic power of 150W). After extraction, filter it while hot and collect the separated liquid, wash the filter residue with a mixed solution of ethanol and ethyl acetate, filter it, repeat 3 times, and combine the separated liquids obtained after filtration. Finally, the combined separated liquids are evaporated by rotary evaporation to remove the solvent to obtain Magnolia officinalis extract.

[0032] Product effect testing 1. Determination of antibacterial ability, the specific process is as follows: (1) Under aseptic conditions, transfer the test strain Staphylococcus aureus to the corresponding test tube slant culture medium, culture it in a constant temperature incubator at 37°C for 24 hours, and then refrigerate it at 4°C for later use; and select individual colonies from them for test tube slant culture, and transfer each type to multiple test tubes for later use; (2) Take the cultured strain slant, add 10 mL of sterile water, gently scrape the bacterial moss with an inoculating loop, and shake to make a concentration of about 10 6 cfu / mL bacterial suspension; (3) Pour 15 mL of the culture medium that has been melted and cooled to 50°C into a sterile culture dish and condense it; use a sterile pipette to transfer 100 μL onto the culture medium, then spread it evenly and set aside; (4) Dissolving the Magnolia officinalis extract prepared in each of the Examples and Comparative Examples in 15 times (by mass) ethanol to prepare a Magnolia officinalis extract solution; (5) The antibacterial ability was determined by the filter paper method commonly used in antibacterial experiments. The specific method is as follows: Punch the qualitative filter paper into 6mm small discs with a hole puncher, place them in a culture dish, and sterilize them at 121℃ for 0.5h. Soak the sterilized filter paper in the Magnolia officinalis extract solution under aseptic operation conditions, and take them out after soaking for 2h. Place the soaked filter paper on the prepared bacteria-containing plates, three pieces per dish plus one blank. Culture them at 37℃ for 24h, observe the growth of the colonies, and measure the diameter of the inhibition zone. The larger the diameter of the inhibition zone of the extract against Staphylococcus aureus, the stronger the antibacterial property of the extract.

[0033] 2. Determination of free radical scavenging activity using the DPPH method (1) Dissolving the Magnolia officinalis extract prepared in each embodiment and comparative example in 10 times (by mass) ethanol, and diluting the mixture in a certain ratio to obtain Magnolia officinalis extract solutions of various dilution ratios; (2) Take 0.5 mL of Magnolia officinalis extract solution and add 2.5 mL of DPPH ethanol solution (8.516×10 -5 mol / L), and the absorbance was measured at 517 nm after 14 hours. The free radical scavenging rate was calculated as follows: Free radical scavenging rate = (Aj-Ai) / Aj Where: Aj---the absorbance of 2.5mL DPPH ethanol solution plus 0.5mL ethanol solvent; Ai---the absorbance of 2.5mL DPPH ethanol solution plus 0.5mL Magnolia officinalis extract solution; EC 50 The value of (the sample concentration when scavenging 50% of DPPH free radicals).

[0034] Use EC 50The size of EC is a measure of the sample's ability to scavenge free radicals. 50 The larger the value, the smaller its free radical scavenging ability.

[0035] The test results of the antibacterial effect and free radical scavenging ability of the Magnolia officinalis extracts prepared in various embodiments and comparative examples are shown in Table 1.

[0036] Table 1 Group Diameter of inhibition zone (cm) <![CDATA[EC 50 (μg / mL)]]> Example 1 3.9 2.25 Example 2 3.7 2.31 Example 3 2.9 2.87 Example 4 3.3 2.55 Example 5 3.4 2.42 Example 6 3.2 2.47 Comparative Example 1 2.1 3.56 Comparative Example 2 2.4 3.96 Comparative Example 3 2.6 3.04 Comparative Example 4 3.0 2.93 As shown in Table 1, the antibacterial effect and antioxidant property of the Magnolia officinalis extract prepared by the embodiment of the present invention are significantly better than those of the comparative example. By extracting Magnolia officinalis with a mixed solution of ethanol and ethyl acetate, and controlling the ratio of the two solvents, the antibacterial effect and antioxidant property of the Magnolia officinalis extract can be significantly improved. Analysis of Example 1 and Comparative Examples 1 and 2 shows that when ethanol or ethyl acetate is used alone as an extraction solvent, the prepared extract cannot simultaneously have high antibacterial property and antioxidant property. When ethanol is used for extraction, its antibacterial effect is not as good as that of ethyl acetate extraction, but its antioxidant property is slightly better than that of the Magnolia officinalis extract extracted with ethyl acetate. Analysis of Example 1 and Comparative Example 4 shows that when no weak alkaline reagent is added before freezing treatment, the grinding process will inactivate more active ingredients, which will directly affect the antibacterial effect and antioxidant property of the Magnolia officinalis extract.

Claims

1. A method for preparing a Magnolia officinalis extract, characterized in that: The following steps are involved: A weak base reagent is added to the coarse powder of Magnolia officinalis, and the powder is ground after being frozen; a mixed solution of ethanol and ethyl acetate is added for ultrasonic extraction, and a separated liquid is collected by solid-liquid separation, and the separated liquid is desolventized to obtain a Magnolia officinalis extract.

2. The preparation method according to claim 1, characterized in that: The weak base reagent includes at least one of sodium carbonate, potassium carbonate, borax, calcium carbonate, sodium bicarbonate, and potassium bicarbonate.

3. The preparation method according to claim 1 or 2, characterized in that: The amount of the weak base reagent added is 0.5%-8% of the mass of the Magnolia officinalis crude powder.

4. The preparation method according to claim 3, characterized in that: The temperature of the freezing treatment is -20°C to -5°C, and the time of the freezing treatment is 10 min to 40 min.

5. The preparation method according to claim 3, characterized in that: The grinding process is to grind to a particle size D90 of 25 μm-80 μm.

6. The preparation method according to any one of claims 1, 2, 4 and 5, characterized in that: The mixed solution of ethanol and ethyl acetate contains ethanol and ethyl acetate; the mass ratio of the ethanol to the ethyl acetate is 1:(0.2-5).

7. The preparation method according to claim 6, characterized in that: The mass ratio of the ethanol to the ethyl acetate is 1:(0.25-4).

8. The preparation method according to claim 6, characterized in that: The ultrasonic extraction process is to extract the product for 30 minutes to 60 minutes at a temperature of 40° C. to 55° C. and an ultrasonic power of 100W to 200W.

9. A Magnolia Bark Extract, characterized in that Prepared by the preparation method described in any one of claims 1 to 8.

10. Use of the Magnolia officinalis extract according to claim 9 in the preparation of skin care products, medicines or health care products.