CN113797261A - Preparation method of camellia flower/leaf extract - Google Patents
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Abstract
The invention discloses a preparation method of a camellia japonica/leaf extract. Fresh camellia and/or camellia leaves are used as raw materials, and the extract is obtained through the working procedures of cleaning, crushing, ultrasonic-assisted extraction, concentration, refining and the like. Compared with the conventional extraction method, the preparation method is simple, convenient and quick, has controllable cost and is easy to realize batch production, and the flavone and polyphenol yield in the obtained extract is obviously improved, and the oxidation resistance is enhanced.
Description
Technical Field
The invention belongs to the technical field of natural product extraction, and particularly relates to a preparation method of a camellia/leaf extract.
Background
The camellia tree belongs to evergreen broad-leaved forest tree, also called camellia, camellia and winter resistance, and is one of ten major flowers in China; the camellia has wide distribution and is mainly produced in Zhejiang, Yunnan, Jiangxi, Sichuan and other places in China. The camellia seeds are a special pure natural high-grade oil material in China, the research and the utilization of camellia at present mainly focus on the aspects of camellia seeds, camellia seed meal and camellia seed shells, and the research and the utilization of camellia flowers and leaves are relatively less. The camellia is used as a reproductive organ of a camellia tree, integrates nutrient substances in the camellia, and is rich in various bioactive components such as protein, amino acid, reducing sugar, polysaccharide, polyphenol, flavone, anthocyanin, vitamin and the like; the camellia leaves are rich in bioactive components such as polyphenol, flavone, polysaccharide, triterpenoid saponin, steroid and the like. The active ingredients have the effects of resisting oxidation, reducing blood fat, reducing blood sugar, resisting tumor, moisturizing, whitening, detoxifying, healing sore, resisting bacteria and the like, and are widely used in the fields of food, health-care products and skin care products. Therefore, the camellia leaves with rich resources also have high utilization value.
Fresh plant material is usually dried by sun drying, oven drying or other drying methods to remove free water to obtain dry material, which is convenient for subsequent transportation, storage and utilization. However, in the drying process, factors such as high temperature, light, oxygen atmosphere and the like usually destroy the original bioactive components of the plants, so that the quality of the raw materials is reduced. In addition, the permeability of the dried plant cells is reduced after the free water is lost, which is not beneficial to the diffusion of the solvent and solute during the solvent extraction process, resulting in the reduction of the extraction efficiency. In order to improve the extraction efficiency, the dried raw material is usually subjected to moderate pulverization before extraction to reduce the particle size and increase the specific surface area, but pulverization and extraction of the raw material are usually performed stepwise. The above problems show that direct extraction of fresh plant material with minimized loss of active substances will result in higher bioactivity of the extracted product and thus greater advantage. Nowadays, developed transportation and convenient logistics enable the long-distance transportation of fresh plant raw materials, however, the supply of the fresh plant raw materials is limited by seasons, and the technical and cost challenges are still faced on how to solve the problem of long-time preservation of the fresh plant raw materials; for example, common physical preservation, i.e., low temperature preservation, such as refrigeration at 4 deg.C, freezing at-18 deg.C, and freezing at-80 deg.C. The plant cells still keep activity at 4 ℃, and nutrients or active substances are slowly consumed; freezing at-18 ℃ activates some biological enzymes such as polyphenol oxidase activity, resulting in rapid reduction of active substances; freezing at-80 ℃ can inhibit the activity of the biological enzyme, but the technical cost is higher.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to solve the problem of fresh-keeping extraction of fresh camellia and leaves, and provides a preparation method of a camellia/leaf extract. Aiming at the problems of low active ingredients of raw materials obtained by different drying modes and low extraction process efficiency, the invention adopts fresh camellia and leaves as raw materials and adopts a crushing extraction technology to realize full and rapid extraction while retaining active substances as much as possible; meanwhile, the ethanol aqueous solution with a certain concentration is used as an extraction solvent to play a role in sterilization and enzyme inhibition, so that the method can be regarded as green chemical fresh-keeping treatment, has less solvent consumption and is suitable for long-time preservation of a large quantity of materials.
The purpose of the invention is realized by the following technical scheme:
the invention relates to a preparation method of a fresh camellia flower/leaf extract, which comprises the following steps:
s1, picking fresh camellia and/or camellia leaves as raw materials, cleaning, draining and then shredding;
s2, taking fresh camellia flower filaments and/or camellia leaf filaments, adding 40-80% ethanol water solution in volume fraction, and crushing to obtain camellia flower and/or camellia leaf feed liquid;
s3, taking the feed liquid of the camellia and/or the camellia leaves, supplementing an ethanol water solution to ensure that the total weight ratio of the fresh camellia and/or the camellia leaves to the ethanol water solution reaches 1 (4-10), and carrying out ultrasonic extraction;
s4, filtering after extraction is finished to obtain clear filtrate and filter residue, adding an ethanol water solution, carrying out ultrasonic extraction on the filter residue according to the material-liquid ratio of 1 (4-10), and combining the two filtrates after filtering;
s5, continuously concentrating the obtained filtrate to enable the weight of the obtained concentrated solution to be 1/(6-10) of the weight of the original extraction filtrate, adding ethanol to enable the mass fraction of the ethanol to reach 60-80%, and refrigerating at 4 ℃ for 1-2 days;
s6, filtering to remove insoluble substances to obtain clear filtrate, and then carrying out reduced pressure concentration to remove ethanol to obtain a fresh camellia flower/leaf extract.
In step S1, the precut filaments are beneficial to subsequent crushing, and a feed liquid with narrower particle size distribution is obtained.
In step S2, the weight ratio of fresh camellia flower filaments and/or camellia leaves filaments to the ethanol aqueous solution is 1 (2-5).
As an embodiment of the present invention, when the raw materials are fresh camellia and camellia leaves, in step S2, fresh camellia filaments and camellia leaves filaments are respectively crushed to obtain a camellia liquid and a camellia leaf liquid, and the liquid and liquid are combined.
In an embodiment of the present invention, in step S2, the crushing conditions are 3000-10000 rpm, 0.5-2 minutes for camellia filaments, and 5-10 minutes for camellia leaves.
As an embodiment of the present invention, the crushing is performed in a crushing apparatus, the existing crushing apparatus can realize high rotation speed of the crushing blade, the crushing process can be completed within several minutes, and the crushing and the extraction are performed simultaneously due to the addition of the solvent. The ethanol water solution is used as an extraction solvent, and has the functions of sterilization and enzyme inhibition, so that the crushed feed liquid can be stored for a long time without great influence on active ingredients.
As an embodiment of the present invention, in step S3, the additional ethanol aqueous solution has the same volume fraction as the ethanol aqueous solution in step S2. The yield of the extraction in two times is higher than that of the extraction in one time by using the same solvent.
In one embodiment of the present invention, in the steps S3 and S4, the ultrasonic extraction is performed at 30 to 70 ℃ and 300 to 700W for 0.5 to 2.0 hours.
As an embodiment of the present invention, when the raw material contains camellia leaves, the step S4, after combining the filtrates, further includes: concentrating the filtrate at 45 deg.C under reduced pressure until the concentrated solution has no ethanol taste, refrigerating the obtained concentrated solution at 4 deg.C for 12-24 hr, and filtering to remove precipitate to obtain clear filtrate. The fresh camellia leaf extract contains more chlorophyll, and the chlorophyll is precipitated by utilizing the property that the chlorophyll is difficult to dissolve in water. Since camellia does not contain chlorophyll, if only camellia is used as a raw material, the step is not needed.
As an embodiment of the invention, the reduced pressure concentration is carried out at 35-55 ℃.
As an embodiment of the present invention, the ethanol aqueous solution added in step S4 has the same volume fraction as that of the ethanol aqueous solution added in step S2.
As one embodiment of the present invention, in step S4, the amount of the aqueous ethanol solution added is the total amount of the aqueous ethanol solutions added in the first two times.
Compared with the prior art, the invention has the following beneficial effects:
1. fresh camellia flowers and leaves are used as raw materials, so that the loss of active substances caused in the conventional drying process is avoided, and meanwhile, the fresh camellia leaves are more beneficial to rapid extraction;
2. by using an in-situ crushing and extracting technology, the crushing and the extraction of the raw materials are carried out simultaneously, the crushing is quick, and the method is suitable for the large-scale treatment of the fresh flowers and leaves;
3. the ethanol solution is used as an extraction solvent, has the functions of sterilizing and inhibiting enzyme, can realize long-time preservation of the crushed feed liquid, and has little influence on active ingredients.
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Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 shows DPPH free radical scavenging ratio IC of camellia japonica flower leaf extract50The value is obtained.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
Fresh camellia flowers are taken, washed by clean water, drained and cut into threads to obtain fresh flower threads, and the water content is 87.2 percent measured by an oven method (105 ℃). Putting 25g of flower silk into a blade type crushing device, adding 100g of ethanol water solution with volume fraction of 60%, starting the device, and crushing for 1 minute at the rotating speed of 8000 rpm to obtain flower particle dispersion liquid. Transferring the obtained feed liquid into a beaker, supplementing 100g of ethanol aqueous solution with the volume fraction of 60%, and ultrasonically extracting for 1.5 hours at the temperature of 50 ℃ and the power of 420W. And after extraction, carrying out vacuum filtration to obtain clear filtrate and filter residue, collecting the filter residue, adding 200g of ethanol aqueous solution with the volume fraction of 60%, and carrying out ultrasonic extraction at 50 ℃ for 1.5 hours at the power of 420W. And carrying out vacuum filtration again, combining filtrates obtained by two-time extraction, concentrating to 50g at 45 ℃ under reduced pressure, adding 75g of absolute ethyl alcohol, refrigerating for 2 days at 4 ℃, filtering to obtain clear filtrate, and concentrating under reduced pressure again to remove the ethanol to obtain 45g of camellia extract.
Example 2
Fresh picked camellia leaves are taken, washed by clear water, drained and cut into threads to obtain fresh leaf threads, and the water content is 52.2 percent measured by an oven method (105 ℃). And (3) putting 30g of cut tobacco into blade type crushing equipment, adding 120g of ethanol water solution with the volume fraction of 60%, starting the equipment, and crushing for 5 minutes at the rotating speed of 8000 rpm to obtain fresh leaf particle dispersion liquid. Transferring the obtained feed liquid into a beaker, supplementing 120g of ethanol aqueous solution with the volume fraction of 60%, and ultrasonically extracting for 1.5 hours at the temperature of 50 ℃ and the power of 420W. And after extraction, carrying out vacuum filtration to obtain clear filtrate and filter residue, collecting the filter residue, adding 240g of ethanol aqueous solution with the volume fraction of 60%, and carrying out ultrasonic extraction at 50 ℃ for 1.5 hours at the power of 420W. And (4) carrying out suction filtration again under reduced pressure, and combining filtrates obtained by two extractions to obtain 389g in total. Concentrating the filtrate at 45 deg.C under reduced pressure until no ethanol smell, refrigerating at 4 deg.C for 15 hr, and filtering to obtain clear filtrate. Concentrating under reduced pressure to 56g, adding 84g anhydrous ethanol, refrigerating at 4 deg.C for 2 days, filtering to obtain clear filtrate, concentrating under reduced pressure again to remove ethanol to obtain folium Camelliae Japonicae extract 71 g.
Example 3
The same fresh flower silk 47.1g as in example 1 was taken and subjected to the same crushing conditions to prepare a flower granule dispersion; the weight of the 60% by volume aqueous ethanol solution added during the disruption was 188.4 g.
12.9g of the same fresh leaf shreds as in example 2 were taken and used to prepare a dispersion of fresh leaf particles under the same crushing conditions. The weight of the 60% by volume aqueous ethanol solution added during the disruption was 51.6 g.
Mixing the two dispersions, adding 240g of ethanol aqueous solution with volume fraction of 60%, and ultrasonically extracting at 50 ℃ for 1.5 hours at the power of 420W. And after extraction, carrying out vacuum filtration to obtain clear filtrate and filter residue, collecting the filter residue, adding 480g of ethanol aqueous solution with the volume fraction of 60%, and carrying out ultrasonic extraction at 50 ℃ for 1.5 hours at the power of 420W. The mixture was again filtered under reduced pressure and the filtrates from the two extractions were combined to give a total of 805 g. Concentrating the filtrate at 45 deg.C under reduced pressure until no ethanol smell, refrigerating at 4 deg.C for 15 hr, and filtering to obtain clear filtrate. Concentrating under reduced pressure to 115g, adding 172.5g anhydrous ethanol, refrigerating at 4 deg.C for 2 days, filtering to obtain clear filtrate, concentrating under reduced pressure again to remove ethanol to obtain folium Camelliae Japonicae extract 102 g.
Example 4
As a comparative example of example 3, the fresh flower particle dispersion and the fresh leaf particle dispersion were combined, and then refrigerated at 4 ℃ for 3 months, followed by the same procedure, to obtain 102g of a camellia leaf extract.
Example 5
Putting 47.1g of fresh flower filaments which are the same as in example 1 into blade type crushing equipment, adding 140g of ethanol water solution with the volume fraction of 40%, starting the equipment, and crushing for 2 minutes at the rotating speed of 4000 revolutions per minute to obtain fresh flower particle dispersion liquid;
12.9g of fresh leaf shreds which are the same as those in the example 2 are taken and put into a blade type crushing device, 40g of ethanol water solution with the volume fraction of 40 percent is added, the device is started, and the fresh leaf shreds are crushed for 10 minutes at the rotating speed of 4000 revolutions per minute to obtain the fresh leaf particle dispersion liquid.
And combining the two dispersions, supplementing 180g of 40% ethanol aqueous solution by volume fraction, and ultrasonically extracting at the temperature of 30 ℃ for 2.0 hours at the power of 350W. And after extraction, carrying out vacuum filtration to obtain clear filtrate and filter residue, collecting the filter residue, adding 360g of 40% ethanol aqueous solution by volume fraction, and carrying out ultrasonic extraction at 30 ℃ for 2.0 hours at the power of 350W. And carrying out suction filtration again under reduced pressure, and combining filtrates obtained by two extractions to obtain a total of 590 g. Concentrating the filtrate at 45 deg.C under reduced pressure until no ethanol smell, refrigerating at 4 deg.C for 15 hr, and filtering to obtain clear filtrate. Concentrating under reduced pressure to 95g, adding 380g anhydrous ethanol, refrigerating at 4 deg.C for 2 days, filtering to obtain clear filtrate, concentrating under reduced pressure again to remove ethanol to obtain folium Camelliae Japonicae extract 80 g.
Example 6
Putting 47.1g of fresh flower filaments which are the same as in example 1 into blade type crushing equipment, adding 220g of ethanol water solution with volume fraction of 80%, starting the equipment, and crushing for 1.5 minutes at the rotating speed of 6000 revolutions per minute to obtain fresh flower particle dispersion liquid;
12.9g of fresh leaf shreds which are the same as those in the example 2 are taken and put into a blade type crushing device, 60g of ethanol water solution with the volume fraction of 80 percent is added, the device is started, and the fresh leaf shreds are crushed for 6.5 minutes at the rotating speed of 6000 revolutions per minute to obtain fresh leaf particle dispersion liquid.
And combining the two dispersions, supplementing 320g of 80% ethanol aqueous solution, and ultrasonically extracting at the temperature of 60 ℃ for 0.5 hour under the power of 560W. And after extraction, carrying out vacuum filtration to obtain clear filtrate and filter residue, collecting the filter residue, adding 600g of 80% ethanol aqueous solution by volume fraction, and carrying out ultrasonic extraction at 60 ℃ for 0.5 hour at the power of 560W. The mixture was again filtered under reduced pressure and the filtrates from the two extractions were combined to give a total of 955 g. Concentrating the filtrate at 45 deg.C under reduced pressure until no ethanol smell, refrigerating at 4 deg.C for 15 hr, and filtering to obtain clear filtrate. Concentrating under reduced pressure to 105g, adding 380g anhydrous ethanol, refrigerating at 4 deg.C for 2 days, filtering to obtain clear filtrate, concentrating under reduced pressure again to remove ethanol to obtain folium Camelliae Japonicae extract 91 g.
Comparative example 1
As a comparative example of example 3, fresh flowers and leaves were dried in the sun, ground and passed through a 60-mesh sieve, and the moisture content of the dried flower powder was 9.2% and the moisture content of the dried leaf powder was 9.7% as measured by an oven method (105 ℃). Taking 6.64g of dry flower powder and 6.83g of dry leaf powder, uniformly mixing, adding 46.53g of pure water (water is added to reach the same moisture as that of fresh flower leaves), and uniformly stirring. Then 480g of ethanol water solution with the volume fraction of 60 percent is added, ultrasonic extraction is carried out for 1.5 hours at the temperature of 50 ℃ and the power of 420W, the filter residue is extracted once again under the same extraction condition after filtration, and the two filtrates are combined to total 811 g. Concentrating the filtrate at 45 deg.C under reduced pressure until no ethanol smell, refrigerating at 4 deg.C for 15 hr, and filtering to obtain clear filtrate. Concentrating under reduced pressure to 115g, adding 172.5g anhydrous ethanol, refrigerating at 4 deg.C for 2 days, filtering to obtain clear filtrate, concentrating under reduced pressure again to remove ethanol to obtain folium Camelliae Japonicae extract 102 g.
Comparative example 2
As a comparative example to example 3, fresh flowers and leaves were dried under vacuum at 60 ℃ and ground to pass through a 60 mesh sieve, and the moisture content of the dried flower powder was 7.0% and the moisture content of the dried leaf powder was 6.2% as measured by the oven method (105 ℃). Taking 6.48g of dried flower powder and 6.57g of dried leaf powder, uniformly mixing, then adding 46.95g of pure water, and uniformly stirring. Then 480g of ethanol water solution with the volume fraction of 60 percent is added, ultrasonic extraction is carried out for 1.5 hours at the temperature of 50 ℃ and the power of 420W, the filter residue is extracted once again under the same extraction condition after filtration, and 813g of the two filtrates are combined. Concentrating the filtrate at 45 deg.C under reduced pressure until no ethanol smell, refrigerating at 4 deg.C for 15 hr, and filtering to obtain clear filtrate. Concentrating under reduced pressure to 115g, adding 172.5g anhydrous ethanol, refrigerating at 4 deg.C for 2 days, filtering to obtain clear filtrate, concentrating under reduced pressure again to remove ethanol to obtain folium Camelliae Japonicae extract 102 g.
Comparative example 3
As a comparative example of example 3, a fresh flower granule dispersion and a fresh leaf granule dispersion were combined, and 720g of an aqueous ethanol solution having a volume fraction of 60% was added thereto, and ultrasonic extraction was performed at 50 ℃ and a power of 420W for 3.0 hours, followed by vacuum filtration to obtain 819g of a filtrate. Then, the same operation is carried out to obtain 102g of camellia flower leaf extract.
Comparative example 4
As a comparative example of example 2, the filtrates were combined after extraction twice in the same manner, amounting to 389g, and the filtrate was directly concentrated under reduced pressure to 56g, followed by addition of 84g of absolute ethanol, cold storage at 4 ℃ for 2 days, filtration to give a clear filtrate, and concentration under reduced pressure again to remove ethanol, to give 71g of camellia leaf extract.
Comparative example 5
As a comparative example of example 1, freshly picked camellia was taken, washed with clean water, drained and cut into fresh filaments with a moisture of 87.2% as measured by the oven method (105 ℃). Taking 25g of filament, adding 400g of ethanol water solution with volume fraction of 60%, and ultrasonically extracting at 50 ℃ for 1.5 hours at the power of 420W. Filtering to obtain clear filtrate after extraction, and concentrating under reduced pressure to remove ethanol to obtain flos Camelliae Japonicae extract 50 g.
Effect verification experiment 1
The contents of total flavonoids and total phenols in the camellia flower leaf extract obtained in the above examples are respectively determined by spectrophotometry.
The principle of measuring the total flavone is as follows: reducing flavone in neutral or alkalescent condition in the presence of sodium nitrite, adding aluminium nitrate for complexing to generate chelate, adding sodium hydroxide solution to open the ring of flavone compound to generate 2-hydroxy chalcone for developing color, and having maximum absorption peak at 500nm wavelength and according with beer's law of quantitative analysis.
The principle of the determination of total phenols is as follows: folin-ciocalteu oxidizes-OH groups in polyphenol and shows blue color, the maximum absorption wavelength lambda is 765nm, and gallic acid is used as a calibration standard to quantify polyphenol.
The yield was then calculated according to the following formula:
in the formula (I), the compound is shown in the specification,
c is the concentration of total flavone or total phenol, and the unit is mg/g;
m is the mass of the camellia flower leaf extract obtained in each example, and the unit is g;
m1 is the mass of the flower in g;
m2 is the dry weight of the leaves in g;
w1 is flower moisture in%;
w2 is the moisture of the leaves in%.
The measurement and calculation results are shown in table 1.
TABLE 1 Total Flavonoids, Total phenols concentration and yield in Camellia japonica leaf extract
As can be seen from Table 1, in example 3 in which fresh flowers and fresh leaves were used as the starting materials, the yields of total flavonoids and total phenols were higher than in comparative example 1 in which dried flowers and dried leaves obtained by air-drying were used as the starting materials, and in comparative example 2 in which dried flowers and dried leaves obtained by vacuum drying were used as the starting materials.
The results of example 4 show that after the fresh flower particle dispersion and the fresh leaf particle dispersion are combined and refrigerated at 4 ℃ for 3 months, the subsequent same operations are carried out, the yield of the obtained total flavonoids and the total phenols of the extract is only slightly reduced, and the feed liquid after being crushed can be preserved for a long time.
The results of comparative example 3 show that with the same total solvent dosage and total extraction time, the extraction of active substances is not sufficient in a single extraction, the yield of total flavonoids is 9.47 percent lower than that of the two extractions, and the yield of total phenols is 26.75 percent lower.
The results of comparative example 5 show that the extraction of active substances is not sufficient because the filaments are not subjected to high-speed crushing and are extracted once, and compared with example 1, the yield of total flavonoids is reduced by 13.88%, and the yield of total phenols is reduced by 35.76%.
Effect verification experiment 2
The related research shows that DPPH free radical clearance rate and hydroxyl free radical clearance rate are in a positive correlation with each other, so that one of the characteristics of the antioxidant capacity can be selected.
1, 1-diphenyl-2-trinitrophenylhydrazine (DPPH) is a stable long-life free radical, and the ethanol solution of the radical is dark purple and has strong absorption near 520 nm. In the presence of free radical scavengers, the light absorption of the DPPH ethanol solution is reduced due to its one-electron pairing. The degree of discoloration of the DPPH ethanol solution is linear with the number of electrons it receives, and thus the ability of the test sample to scavenge free radicals, i.e., the magnitude of antioxidant activity, can be evaluated.
Determination of IC corresponding to the DPPH radical scavenging half of the Camellia japonica leaf extracts obtained in example 3, comparative example 1 and comparative example 250The results are shown in FIG. 1. As can be seen, the IC of example 350The value is the smallest, and the antioxidant capacity is the strongest.
Effect verification experiment 3
Maximum absorption peaks of chlorophyll a and chlorophyll b in red light region are 663nm and 645nm respectively, and the concentrations of chlorophyll a, chlorophyll b and total chlorophyll are calculated according to the following formulas by the reference method:
Ca＝12.7A663–2.69A645
Cb＝22.9A645–4.68A663
Ct＝20.2A645+8.02A663
in the formula, Ca is the concentration of chlorophyll a, Cb is the concentration of chlorophyll b, and Ct is the total chlorophyll concentration, and the unit is mg/L; a. the663And A645The absorbance of the test solution at 663nm and the absorbance at 645nm are respectively.
The chlorophyll concentrations of the extracts obtained in example 2 and comparative example 4 are shown in table 2.
TABLE 2 chlorophyll concentration/mg. L of fresh Camellia japonica leaf extract-1
| Example one another | Ca | Cb | Ct |
| Example 2 | 0.589 | 1.116 | 1.714 |
| Comparative example 4 | 49.153 | 19.360 | 68.560 |
The data in table 2 show that the removal rate of chlorophyll a is about 98.8%, the removal rate of chlorophyll b is about 94.2%, and the removal rate of total chlorophyll is about 97.5% after the fresh camellia leaf extract is subjected to concentration and refrigeration, which indicates that the chlorophyll removal is relatively thorough.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (10)
1. A preparation method of a fresh camellia flower/leaf extract is characterized by comprising the following steps:
s1, picking fresh camellia and/or camellia leaves as raw materials, cleaning, draining and then shredding;
s2, taking fresh camellia flower filaments and/or camellia leaf filaments, adding 40-80% ethanol water solution in volume fraction, and crushing to obtain camellia flower and/or camellia leaf feed liquid;
s3, taking the feed liquid of the camellia and/or the camellia leaves, supplementing an ethanol water solution to ensure that the total weight ratio of the fresh camellia and/or the camellia leaves to the ethanol water solution reaches 1 (4-10), and carrying out ultrasonic extraction;
s4, filtering after extraction is finished to obtain clear filtrate and filter residue, adding an ethanol water solution, carrying out ultrasonic extraction on the filter residue according to the material-liquid ratio of 1 (4-10), and combining the two filtrates after filtering;
s5, continuously concentrating the obtained filtrate to enable the weight of the obtained concentrated solution to be 1/(6-10) of the weight of the original extraction filtrate, adding ethanol to enable the mass fraction of the ethanol to reach 60-80%, and refrigerating at 4 ℃ for 1-2 days;
s6, filtering to remove insoluble substances to obtain clear filtrate, and then carrying out reduced pressure concentration to remove ethanol to obtain a fresh camellia flower/leaf extract.
2. The method for preparing a fresh camellia/leaf extract as claimed in claim 1, wherein in step S2, the weight ratio of fresh camellia filaments and/or camellia leaves filaments to the ethanol aqueous solution is 1 (2-5).
3. The method for preparing a fresh camellia/leaf extract according to claim 1, wherein when the raw materials are fresh camellia and camellia leaf, in step S2, fresh camellia filament and camellia leaf filament are respectively crushed to obtain camellia feed liquid and camellia leaf feed liquid, and the feed liquids are combined.
4. The method for preparing a fresh camellia/leaf extract as claimed in claim 1 or 3, wherein in step S2, the crushing condition is that the rotation speed is 3000-10000 r/min, the camellia filaments are crushed for 0.5-2 min, and the camellia leaves are crushed for 5-10 min.
5. The method of claim 1, wherein the additional ethanol aqueous solution has the same volume fraction as the ethanol aqueous solution in step S2 in step S3.
6. The method for preparing a fresh camellia/leaf extract as claimed in claim 1, wherein in the steps S3 and S4, the ultrasonic extraction is performed at 30-70 ℃ and 300-700W for 0.5-2.0 hours.
7. The method for preparing a fresh camellia/leaf extract as claimed in claim 1, wherein when the raw material contains camellia leaves, the step S4 combining the filtrates further comprises: concentrating the filtrate at 45 deg.C under reduced pressure until the concentrated solution has no ethanol taste, refrigerating the obtained concentrated solution at 4 deg.C for 12-24 hr, and filtering to remove precipitate to obtain clear filtrate. If only camellia is used as a raw material, the step is not needed.
8. The method for preparing a fresh camellia/leaf extract as claimed in claim 1 or 7, wherein the concentration under reduced pressure is performed at 35-55 ℃.
9. The method of claim 1, wherein the ethanol aqueous solution added in step S4 has the same volume fraction as the ethanol aqueous solution added in step S2.
10. The method for preparing a fresh camellia/leaf extract as claimed in claim 1, wherein the amount of the aqueous ethanol solution added in step S4 is the total amount of the aqueous ethanol solutions added in the first two times.
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| CN114989318A (en) * | 2022-05-09 | 2022-09-02 | 孙芙蓉 | Moisturizing and whitening polysaccharide and application thereof in preparing moisturizing and whitening cosmetics |
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