A method for preparing chamomile extract, the product and its application
By employing mixed solvent and macroporous resin purification technology, the problem of low total flavonoid yield and purity in chamomile extract has been solved, achieving efficient and low-cost extraction and purification, which is suitable for cosmetic applications.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-01
- Publication Date
- 2026-04-03
AI Technical Summary
Existing chamomile extraction methods result in low yields and purity of total flavonoids, making it difficult to meet the oil-control and anti-inflammatory requirements in cosmetics.
A mixed solvent extraction process was adopted, in which chamomile powder was refluxed and extracted with a solution of disodium ethylenediaminetetraacetate and Tween 80 in ethanol. The filter residue was then extracted again with a mixed solution of ethanol, ethyl acetate and water, and purified by AB-8 macroporous resin. The extraction parameters were optimized to improve the content and purity of total flavonoids.
It significantly improved the dissolution rate and purity of total flavonoids in chamomile extract, reduced preparation costs, simplified the operation process, reduced resource waste, and improved extraction efficiency.
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Figure CN120661414B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of plant active ingredient extraction technology, specifically relating to a method for preparing chamomile extract, the product, and its application. Background Technology
[0002] Chamomile is an annual herbaceous plant belonging to the Asteraceae family, and is one of the oldest, most widely used, and best-documented medicinal plants in the world. Currently, the main varieties of chamomile are German chamomile (Matricaria chamomilia L.) and Roman chamomile (Chamaemelum nobile L.). Chamomile possesses a variety of biological properties, such as antioxidant, anti-inflammatory, antibacterial, antifungal, antiparasitic, insecticidal, antidepressant, anti-allergic, antidiabetic, anticancer, and analgesic effects. Therefore, chamomile is widely used in both traditional Chinese medicine and Western medicine to treat various diseases, such as infections, neuropsychiatric disorders, respiratory diseases, gastrointestinal diseases, and liver diseases. It can be used both internally and externally. Chamomile has been approved as a surfactant and preservative in many countries and is widely used in medicine, veterinary medicine, food engineering, and plant quarantine control.
[0003] Currently, there is a lot of research on the preparation methods of chamomile extract, which can be mainly divided into traditional extraction methods and innovative extraction methods. Traditional extraction methods include steam distillation, organic solvent extraction, and cold pressing; innovative extraction methods include supercritical fluid extraction, subcritical extraction, ultrasonic-assisted extraction, microwave-assisted extraction, and real-time controlled vacuum extraction.
[0004] Among them, steam distillation is currently the most commonly used extraction process. The equipment is simple and the operation is convenient. It mainly utilizes the control and regulation of steam pressure. For example, Chinese patent CN115887516A discloses a chamomile extract for treating rhinitis, which is prepared by the following steps: (1) Take the wet stamens of chamomile flowers and perform steam distillation to obtain the distilled product; (2) Place the distilled product in a sealed alcoholization tank and control the temperature and humidity to alcoholize it to obtain an alcoholized liquid; (3) Filter the alcoholized liquid to obtain a crude product to obtain a filtrate; (4) Concentrate and evaporate the filtrate under low temperature and reduced pressure, retain the aqueous solution, enrich the flavonoids and bisabolol compounds in the aqueous solution to obtain a concentrated solution; (5) Vacuum dry the concentrated solution obtained in step (4) to obtain the chamomile extract. This invention uses a pure plant extraction method to retain the natural effective components flavonoids, chamomile blue hydrocarbons and α-bisabolol to the greatest extent, without containing other impurities. The above-mentioned chamomile extract can be used to prepare a treatment for rhinitis, or as an effective ingredient in rhinitis drugs, to better synergistically treat rhinitis.
[0005] For example, Chinese patent CN116570639A discloses a method for extracting and purifying total flavonoids from chamomile. The method includes the following steps: drying, pulverizing, and sieving fresh chamomile; placing the chamomile powder in a supercritical CO2 apparatus for extraction to remove lipid-soluble compounds, obtaining supercritically extracted chamomile powder; subjecting the chamomile powder to ultrasonic-assisted extraction, followed by vacuum filtration to obtain a crude extract of total chamomile flavonoids; loading the crude extract onto a macroporous resin column for purification of the total chamomile flavonoids; and rotary evaporating and freeze-drying the purified chamomile flavonoids to obtain the purified total chamomile flavonoid product. This invention combines supercritical CO2 and ultrasonic-assisted extraction technologies, and after multiple optimizations of the extraction method, obtains the optimal extraction parameters. It also efficiently and environmentally friendly removes lipid-soluble substances from chamomile, effectively improving the purification efficiency of total chamomile flavonoids and showing good prospects for industrial production.
[0006] However, the content of active ingredients in chamomile extract obtained by existing extraction methods cannot meet the requirements, especially the yield and purity of total flavonoids are relatively low. Therefore, it is necessary to develop a preparation method for chamomile extract that can better improve the extraction efficiency of total flavonoids. Summary of the Invention
[0007] In view of the shortcomings of the existing technology, the present invention aims to provide a method for preparing chamomile extract. The present invention uses a mixed solvent extraction process to extract the effective components of chamomile, which can significantly increase the content of total flavonoids in the extract. The obtained chamomile extract can enhance the oil-controlling, anti-inflammatory and soothing effects of cosmetics.
[0008] To achieve the above objectives, the present invention adopts the following technical solution:
[0009] On one hand, the present invention provides a method for preparing chamomile extract, comprising the following steps:
[0010] (1) Take dried chamomile raw material, remove impurities, and then pulverize it to obtain chamomile powder;
[0011] (2) Add solvent A to the obtained chamomile powder, soak at room temperature, then reflux to extract, filter, and obtain filtrate A and filter residue;
[0012] (3) Add solvent B to the filter residue obtained in step (2), reflux and extract again, filter, and obtain filtrate B;
[0013] (4) Combine filtrate A and filtrate B, then make up to 500 mL with 90% ethanol, let stand at 4℃ for 24 h, then centrifuge at 6000 r / min for 3 min, filter and take the filtrate, make up to 500 mL with 90% ethanol to obtain crude extract; concentrate the crude extract to obtain concentrated solution, pass the concentrated solution through macroporous resin adsorption, elute to obtain eluent, concentrate the eluent again, dry to obtain chamomile extract.
[0014] Solvent A mentioned in step (2) above is an ethanol solution containing disodium ethylenediaminetetraacetate and Tween 80;
[0015] The mass ratio of disodium ethylenediaminetetraacetate (EDTA) to Tween 80 is 1:5-7; preferably, the mass ratio of disodium EDTA to Tween 80 is 1:6.
[0016] During the implementation of this invention, it was discovered that mixing disodium ethylenediaminetetraacetate and Tween 80 and then adding them to ethanol for chamomile extraction can improve the dissolution of flavonoids.
[0017] Because Tween 80 can promote the rupture of plant cell walls, thereby increasing the extraction rate of active ingredients; in addition, as a nonionic hydrophilic surfactant, Tween can increase the solubility of poorly soluble or insoluble organic matter in water, allowing flavonoids to dissolve better.
[0018] However, during the implementation of this invention, it was unexpectedly discovered that mixing disodium EDTA and Tween 80 at a mass ratio of 1:3-6 and then adding them to low-concentration ethanol for extraction of chamomile powder significantly improved the dissolution of flavonoids. It is speculated that the reason is that mixing disodium EDTA and Tween 80 can significantly increase the solubility of flavonoids. On the one hand, disodium EDTA can play an antioxidant role, making the flavonoids stable during the extraction process. On the other hand, disodium EDTA can enhance the effect of Tween 80, improving its solubilizing effect.
[0019] The total mass of the disodium ethylenediaminetetraacetate and Tween 80 is 1-2% of the total mass of the chamomile powder; preferably 1.8%.
[0020] The volume fraction of the ethanol solution described in step (2) above is 50-70%; preferably 60%.
[0021] Furthermore, during the implementation of this invention, it was discovered that adding disodium ethylenediaminetetraacetate and Tween 80 to the extraction solvent can more effectively dissolve flavonoids under relatively low ethanol concentration conditions, thereby reducing the ethanol concentration and thus lowering the preparation cost. In addition, the addition of disodium ethylenediaminetetraacetate can achieve better solubilization effect with a relatively low amount of surfactant.
[0022] The volume-to-mass ratio of solvent A to chamomile powder in step (2) above is 20-40 mL: 1 g; preferably 30 mL: 1 g.
[0023] The soaking time in step (2) above is 10-20 hours; preferably 12 hours.
[0024] The reflux extraction temperature in step (2) above is 70-80℃, and the extraction time is 1-2 hours.
[0025] Solvent B mentioned in step (3) above is a mixed solution of ethanol, ethyl acetate and water; the volume ratio of ethanol, ethyl acetate and water is 60-70:20-30:10-20;
[0026] Preferably, the volume ratio of ethanol, ethyl acetate and water is 60:20:20, 70:20:10, 60:30:10, 65:25:10, 62:23:15 or 67:20:13;
[0027] More preferably, the volume ratio of ethanol, ethyl acetate and water is 70:20:10.
[0028] The reflux extraction temperature in step (3) above is 80-90℃, and the extraction time is 2-3 hours.
[0029] The volume-to-mass ratio of solvent B and filter residue in step (3) above is 10-25 mL:1 g; preferably 15 mL:1 g.
[0030] In the implementation process, this invention uses a mixed solution of ethanol, ethyl acetate and water as the extraction solvent to re-extract the filter residue. By controlling the volume ratio of the three to 60-70:20-30:10-20, the remaining flavonoid components in the filter residue are better and more fully dissolved. By using mixed solvents of different polarities, various flavonoid components in plants can be better dissolved, thereby improving the extraction efficiency.
[0031] The macroporous resin mentioned in step (4) above is AB-8 resin.
[0032] The elution conditions are as follows: the sample volume is 6 BV, the sample flow rate is 4 mL / min, the eluent is a 50% ethanol solution, the eluent flow rate is 4 mL / min, the eluent volume is 5 BV, and elution is stopped when the eluent becomes colorless, thus obtaining the eluent.
[0033] This invention uses AB-8 macroporous resin to purify the extract, which improves the purity of total flavonoids while ensuring the yield of total flavonoids, significantly improving the extraction efficiency. Furthermore, the macroporous resin can be continuously regenerated and reused, reducing resource waste.
[0034] As a preferred embodiment, the method for preparing the chamomile extract includes the following steps:
[0035] (1) Take dried chamomile raw material, remove impurities, and pulverize it to 1-2 mm to obtain chamomile powder;
[0036] (2) Add solvent A to the obtained chamomile powder, soak at room temperature for 12 hours, then reflux extract at 80°C for 1.5 hours, filter, and obtain filtrate A and filter residue;
[0037] Solvent A is an ethanol solution with a volume fraction of 60% containing disodium ethylenediaminetetraacetate (EDTA) and Tween 80, wherein the mass ratio of EDTA to Tween 80 is 1:6, and the total mass of EDTA and Tween 80 is 1.8% of the total mass of chamomile powder; the volume-to-mass ratio of solvent A to chamomile powder is 30 mL: 1 g.
[0038] (3) Add solvent B to the filter residue obtained in step (2), reflux and extract again at 90°C for 2.5 hours, filter, and obtain filtrate B;
[0039] The solvent B is a mixed solution of ethanol, ethyl acetate and water in a volume ratio of 70:20:10; the mass-volume ratio of the filter residue to solvent B is 1g:15mL.
[0040] (4) Combine filtrate A and filtrate B, then make up to 500 mL with 90% ethanol, let stand at 4℃ for 24 h, then centrifuge at 6000 r / min for 3 min, filter and take the filtrate, make up to 500 mL with 90% ethanol to obtain crude extract; concentrate the crude extract to obtain concentrated solution, pass the concentrated solution through AB-8 macroporous resin for adsorption, eluent after elution, concentrate the eluent again, dry to obtain chamomile extract.
[0041] On the other hand, the present invention also provides a chamomile extract prepared by the above preparation method.
[0042] Furthermore, the present invention also provides the application of the chamomile extract prepared by the above preparation method in the preparation of cosmetic raw materials or cosmetics.
[0043] In another aspect, the present invention provides a cosmetic ingredient comprising chamomile extract prepared by the above method, a solvent, and a preservative; wherein the solvent is propylene glycol.
[0044] In another aspect, the present invention also provides a cosmetic product, which includes chamomile extract prepared by the above method or the above cosmetic raw materials.
[0045] The cosmetic products mentioned are serums, essence creams, eye creams, or face creams.
[0046] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0047] (1) During the implementation of this invention, it was discovered that mixing disodium EDTA and Tween 80 and adding them to ethanol for chamomile extraction can improve the dissolution of flavonoids. Unexpectedly, it was also found that mixing disodium EDTA and Tween 80 at a mass ratio of 1:3-6 and adding them to ethanol for chamomile powder extraction significantly improved the dissolution of flavonoids. The reason for this is speculated to be that the mixture of disodium EDTA and Tween 80 significantly increases the solubility of flavonoids. On the one hand, disodium EDTA has an antioxidant effect, ensuring the stability of flavonoids during extraction; on the other hand, disodium EDTA can enhance the solubilizing effect of Tween 80. Furthermore, an unexpected discovery during the implementation of this invention is that the extraction method described in this invention does not require pre-defatting treatment and does not affect the total dissolution rate of flavonoids. The operation is simple, time-saving, and labor-saving.
[0048] (2) Adding disodium ethylenediaminetetraacetate and Tween 80 to the extraction solvent can make the flavonoid components dissolve more effectively under the condition of relatively low ethanol concentration, thereby reducing the concentration of ethanol and thus reducing the preparation cost; in addition, the addition of disodium ethylenediaminetetraacetate can make the surfactant achieve better solubilization effect with relatively low addition amount.
[0049] (3) In this invention, a mixed solution of ethanol, ethyl acetate and water is used as the extraction solvent to extract the filter residue again. By controlling the volume ratio of the three to be 60-70:20-30:10-20, the remaining flavonoid components in the filter residue are better and more fully dissolved. By using mixed solvents of different polarities, various flavonoid components in plants can be better dissolved, thereby improving the extraction efficiency. This invention uses a two-stage extraction process to make the effective components in plants more fully extracted and reduce resource waste.
[0050] (4) By using AB-8 macroporous resin to purify the extract, the present invention improves the purity of total flavonoids while ensuring the yield of total flavonoids, significantly improving the extraction efficiency. Furthermore, the macroporous resin can be continuously regenerated and reused, reducing resource waste. Attached Figure Description
[0051] Figure 1 This is the standard curve for rutin solution.
[0052] The absorbance measured by rutin was used to establish a regression equation: y = 1.41x - 0.042, R0 2=0.9996, indicating that rutin showed a good linear relationship with absorbance within the range of mass concentrations set in the experiment. Detailed Implementation
[0053] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the tables in the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.
[0054] The following examples and comparative examples of the present invention are shown to provide a more detailed description of the compositions of the present invention, but the present invention is not limited thereto.
[0055] The present invention does not limit the source of the raw materials used. Unless otherwise specified, the raw materials used in the present invention are all commercially available products in this technical field.
[0056] Example 1: A method for preparing chamomile extract
[0057] Includes the following steps:
[0058] (1) Take dried chamomile raw material, remove impurities, and pulverize it to 1-2 mm to obtain chamomile powder;
[0059] (2) Add solvent A to 10g of chamomile powder, soak at room temperature for 12 hours, then reflux extract at 80℃ for 1.5 hours, filter, and obtain filtrate A and filter residue;
[0060] Solvent A is an ethanol solution with a volume fraction of 60% containing disodium ethylenediaminetetraacetate (EDTA) and Tween 80, wherein the mass ratio of EDTA to Tween 80 is 1:6, and the total mass of EDTA and Tween 80 is 1.8% of the total mass of chamomile powder; the volume-to-mass ratio of solvent A to chamomile powder is 30 mL: 1 mg.
[0061] (3) Add solvent B to the filter residue obtained in step (2), reflux and extract again at 90°C for 2.5 hours, filter, and obtain filtrate B;
[0062] The solvent B is a mixed solution of ethanol, ethyl acetate and water in a volume ratio of 70:20:10; the mass-volume ratio of the filter residue to solvent B is 1g:15mL.
[0063] (4) Combine filtrate A and filtrate B, then make up to 500 mL with 90% ethanol, let stand at 4°C for 24 h, then centrifuge at 6000 r / min for 3 min, filter and take the filtrate, make up to 500 mL with 90% ethanol to obtain crude extract; concentrate the crude extract to obtain concentrated solution, pass the concentrated solution through AB-8 macroporous resin for adsorption, eluent after elution, concentrate the eluent again, freeze dry to obtain chamomile extract.
[0064] The elution conditions are as follows: the sample volume is 6 BV, the sample flow rate is 4 mL / min, the eluent is a 50% ethanol solution, the eluent flow rate is 4 mL / min, the eluent volume is 5 BV, and elution is stopped when the eluent becomes colorless, thus obtaining the eluent.
[0065] Example 2: A method for preparing chamomile extract
[0066] Includes the following steps:
[0067] (1) Take dried chamomile raw material, remove impurities, and pulverize it to 1-2 mm to obtain chamomile powder;
[0068] (2) Add solvent A to 10g of chamomile powder, soak at room temperature for 10 hours, then reflux extract at 80℃ for 2 hours, filter, and obtain filtrate A and filter residue;
[0069] The solvent A is an ethanol solution with a volume fraction of 50% containing disodium ethylenediaminetetraacetate and Tween 80, the mass ratio of disodium ethylenediaminetetraacetate and Tween 80 is 1:5, and the total mass of disodium ethylenediaminetetraacetate and Tween 80 is 1% of the total mass of chamomile powder; the volume mass ratio of solvent A to chamomile powder is 40mL:1g.
[0070] (3) Add solvent B to the filter residue obtained in step (2), reflux and extract again at 80°C for 3 hours, filter, and obtain filtrate B;
[0071] The solvent B is a mixed solution of ethanol, ethyl acetate and water in a volume ratio of 60:20:20; the mass-volume ratio of the filter residue to solvent B is 1 mg: 25 mL.
[0072] (4) Combine filtrate A and filtrate B, then make up to 500 mL with 90% ethanol, let stand at 4°C for 24 h, then centrifuge at 6000 r / min for 3 min, filter and take the filtrate, make up to 500 mL with 90% ethanol to obtain crude extract; concentrate the crude extract to obtain concentrated solution, pass the concentrated solution through AB-8 macroporous resin for adsorption, eluent after elution, concentrate the eluent again, freeze dry to obtain chamomile extract.
[0073] The elution conditions are as follows: the sample volume is 6 BV, the sample flow rate is 4 mL / min, the eluent is a 50% ethanol solution, the eluent flow rate is 4 mL / min, the eluent volume is 5 BV, and elution is stopped when the eluent becomes colorless, thus obtaining the eluent.
[0074] Example 3: A method for preparing chamomile extract
[0075] Includes the following steps:
[0076] (1) Take dried chamomile raw material, remove impurities, and pulverize it to 1-2 mm to obtain chamomile powder;
[0077] (2) Add solvent A to 10g of chamomile powder, soak at room temperature for 20 hours, then reflux extract at 70℃ for 1 hour, filter, and obtain filtrate A and filter residue;
[0078] Solvent A is an ethanol solution with a volume fraction of 70% containing disodium ethylenediaminetetraacetate (EDTA) and Tween 80, wherein the mass ratio of EDTA to Tween 80 is 1:7, and the total mass of EDTA and Tween 80 is 2% of the total mass of chamomile powder; the volume mass ratio of solvent A to chamomile powder is 20 mL: 1 mg.
[0079] (3) Add solvent B to the filter residue obtained in step (2), reflux and extract again at 85°C for 2 hours, filter, and obtain filtrate B;
[0080] The solvent B is a mixed solution of ethanol, ethyl acetate and water in a volume ratio of 60:30:10; the mass-volume ratio of the filter residue to solvent B is 1 mg: 10 mL.
[0081] (4) Combine filtrate A and filtrate B, then make up to 500 mL with 90% ethanol, let stand at 4°C for 24 h, then centrifuge at 6000 r / min for 3 min, filter and take the filtrate, make up to 500 mL with 90% ethanol to obtain crude extract; concentrate the crude extract to obtain concentrated solution, pass the concentrated solution through AB-8 macroporous resin for adsorption, eluent after elution, concentrate the eluent again, freeze dry to obtain chamomile extract.
[0082] The elution conditions are as follows: the sample volume is 6 BV, the sample flow rate is 4 mL / min, the eluent is a 50% ethanol solution, the eluent flow rate is 4 mL / min, the eluent volume is 5 BV, and elution is stopped when the eluent becomes colorless, thus obtaining the eluent.
[0083] Comparative Example 1
[0084] The difference from Example 1 is that only Tween 80 is used as the surfactant in step (2), while the rest is the same as in Example 1.
[0085] Comparative Example 2
[0086] The difference from Example 1 is that the mass ratio of disodium ethylenediaminetetraacetate and Tween 80 in step (2) is 1:3, while the rest is the same as in Example 1.
[0087] Comparative Example 3
[0088] The difference from Example 1 is that the solvent B mentioned in step (3) is only an ethanol solution with a volume fraction of 70%, and the rest is the same as in Example 1.
[0089] Comparative Example 4
[0090] The difference from Example 1 is that in step (3), solvent B is a mixed solution of ethanol, ethyl acetate and water in a volume ratio of 70:10:20, and the rest is the same as in Example 1.
[0091] Effect detection:
[0092] 1. Detection of total flavonoid content in chamomile
[0093] The following results were obtained using the method disclosed in section 2.2.3 of the master's thesis, "Extraction, Separation and Skin Care Efficacy Study of Total Flavonoids from Chamomile, South China University of Technology, Qiu Zhi":
[0094] The total flavonoids in chamomile were measured using the Al(NO3)3-NaNO2-NaOH colorimetric method.
[0095] The principle is that the ortho-dihydroxyl structure in the flavonoid molecule is related to Al 3+ A complexation reaction occurs, and the resulting complex dissolves in an alkaline solution containing NaNO2, at which point the solution turns brick red.
[0096] Detection method:
[0097] Take 1 mL of the crude extract obtained in step (4) of Examples 1-3 and Comparative Examples 1-4, add 0.5 mL of 50 g / L sodium nitrite solution, shake well, let stand for 6 min, then add 0.5 mL of 100 g / L aluminum nitrate solution, shake well, let stand for 6 min, add 4 mL of 40 g / L sodium hydroxide solution, add water to make up to 10 mL, let stand for 15 min, and measure its absorbance at 510 nm. Using rutin as a standard, plot a regression curve with rutin mass concentration as the x-axis and absorbance as the y-axis (see Appendix). Figure 1 The concentration of total flavonoids in the crude chamomile extract was calculated using a standard curve (calculated as an equivalent rutin concentration), and the total flavonoid extraction rate was calculated using formula (1):
[0098]
[0099] In the formula:
[0100] C: Total flavonoid concentration (mg / mL) in the colorimetric tube calculated from the standard curve;
[0101] V: Volume of crude chamomile extract (mL);
[0102] N: The dilution factor of the crude extract after it is added to the colorimetric tube;
[0103] m: Mass of chamomile powder (g).
[0104] The calculation results are shown in Table 1 below.
[0105] Table 1
[0106] Total flavonoid extraction yield Example 1 4.34% Example 2 4.28% Example 3 4.26% Comparative Example 1 2.85% Comparative Example 2 3.21% Comparative Example 3 3.56% Comparative Example 4 3.83%
[0107] According to the test results in Table 1 above, the preparation method of chamomile extract provided by this invention, by adding disodium ethylenediaminetetraacetate and Tween 80 to the extraction solvent and controlling their mass ratio to 1:5-7, allows for more effective dissolution of flavonoids under relatively low ethanol concentration conditions. Furthermore, using a mixed solution of ethanol, ethyl acetate, and water as the extraction solvent for re-extraction of the filter residue further improves the dissolution of remaining flavonoids. By employing mixed solvents of different polarities, various flavonoids in the plant can be better dissolved, thereby increasing the extraction rate of total chamomile flavonoids to above 4.2%. The method does not require pre-degreasing treatment, is simple to operate, and saves time and effort. Changing the type or ratio of surfactant in Comparative Examples 1-2, and changing the type or volume percentage of solvent B in Comparative Examples 3-4, will affect the extraction efficiency of total chamomile flavonoids to some extent, reducing the extraction rate.
[0108] 2. Purity test of total flavonoids in chamomile
[0109] The purity of total flavonoids is calculated using formula (2):
[0110]
[0111] m: Total flavonoid content (mg) calculated based on the data in Table 1;
[0112] M: Mass (mg) of the chamomile extract obtained in step (4).
[0113] The calculation results are shown in Table 2 below.
[0114] Table 2
[0115] Flavonoid purity Example 1 55.62% Example 2 53.48% Example 3 54.06% Comparative Example 1 45.15% Comparative Example 2 48.86% Comparative Example 3 50.51% Comparative Example 5 51.64%
[0116] According to the test results in Table 2 above, the chamomile extracts prepared by the methods in Examples 1-3 have a relatively high content of total flavonoids. Therefore, during the purification process with large-pore resin, a higher purity of total flavonoids can be obtained at a higher elution rate, resulting in a purity of over 53% for the total chamomile flavonoids. In contrast, the total flavonoid content in the chamomile extracts in Comparative Examples 1-4 was relatively low during the preparation process, leading to greater interference during elution and resulting in a lower purity of the final total chamomile flavonoids compared to Examples 1-3.
[0117] Obviously, the described embodiments are only individual embodiments of the present invention, and not all embodiments. All other implementations obtained by those skilled in the art based on the embodiments of the present invention without inventive effort are within the protection scope of the present invention.
Claims
1. A method for preparing chamomile extract, characterized in that: Includes the following steps: (1) Take dried chamomile raw material, remove impurities, and then pulverize it to obtain chamomile powder; (2) Add solvent A to the obtained chamomile powder, soak at room temperature, then reflux to extract, filter, and obtain filtrate A and filter residue; (3) Add solvent B to the filter residue obtained in step (2), reflux and extract again, filter, and obtain filtrate B; (4) Combine filtrate A and filtrate B, concentrate them, adsorb them through macroporous resin, elute them to obtain eluent, concentrate the eluent again, dry it to obtain chamomile extract; Solvent A is an ethanol solution containing disodium ethylenediaminetetraacetate and Tween 80, wherein the mass ratio of disodium ethylenediaminetetraacetate to Tween 80 is 1:5-7; and the volume fraction of the ethanol solution is 50-70%. The solvent B is a mixed solution of ethanol, ethyl acetate and water, wherein the volume ratio of ethanol, ethyl acetate and water is 60-70:20-30:10-20.
2. The preparation method according to claim 1, characterized in that: The total mass of the disodium ethylenediaminetetraacetate and Tween 80 is 1-2% of the total mass of the chamomile powder.
3. The preparation method according to claim 1, characterized in that: The volume-to-mass ratio of solvent A to chamomile powder in step (2) is 20-40 mL: 1 g.
4. The preparation method according to any one of claims 1-3, characterized in that: Includes the following steps: (1) Take dried chamomile raw material, remove impurities, and pulverize it to 1-2 mm to obtain chamomile powder; (2) Add solvent A to the obtained chamomile powder, soak at room temperature for 12 hours, then reflux extract at 80°C for 1.5 hours, filter to obtain filtrate A and filter residue; Solvent A is an ethanol solution with a volume fraction of 60% containing disodium ethylenediaminetetraacetate and Tween 80, the mass ratio of disodium ethylenediaminetetraacetate and Tween 80 is 1:6, and the total mass of disodium ethylenediaminetetraacetate and Tween 80 is 1.8% of the total mass of chamomile powder; the volume mass ratio of solvent A to chamomile powder is 30mL:1g. (3) Add solvent B to the filter residue obtained in step (2), reflux and extract again at 90°C for 2.5 hours, filter, and obtain filtrate B; The solvent B is a mixed solution of ethanol, ethyl acetate and water in a volume ratio of 70:20:10; the mass-volume ratio of the filter residue to solvent B is 1g:15mL. (4) Combine filtrate A and filtrate B, then make up to 500 mL with 90% ethanol, let stand at 4℃ for 24 h, then centrifuge at 6000 r / min for 3 min, filter and take the filtrate, make up to 500 mL with 90% ethanol to obtain crude extract; concentrate the crude extract to obtain concentrated solution, pass the concentrated solution through AB-8 resin adsorption, eluent after elution, concentrate the eluent again, dry to obtain chamomile extract.
5. Chamomile extract prepared by the preparation method according to any one of claims 1-3.
6. The use of the chamomile extract prepared by the preparation method according to any one of claims 1-3 in the preparation of cosmetic raw materials or cosmetics.
7. A cosmetic ingredient, characterized in that: The cosmetic raw materials include chamomile extract prepared by the preparation method according to any one of claims 1-3, a solvent, and a preservative; the solvent is propylene glycol.
8. A cosmetic product, characterized in that: The cosmetics mentioned above include chamomile extract prepared by the preparation method according to any one of claims 1-3 or the cosmetic raw material according to claim 7.
Citation Information
Patent Citations
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