CN113952262B - Preparation method and application of boat-fruited sterculia seed extract - Google Patents
Preparation method and application of boat-fruited sterculia seed extract Download PDFInfo
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- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
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Abstract
The invention discloses a preparation method and application of a boat-fruited sterculia seed extract. The boat-fruited sterculia seed extract is prepared by the following steps: pulverizing semen Scaphii Lychnophori, mixing with water, steaming at certain temperature under certain pressure, and filtering to obtain semen Scaphii Lychnophori extract. The semen Scaphii Lychnophori extract obtained by the preparation method has improved polysaccharide yield. The boat-fruited sterculia seed extract prepared by the method is applied to skin, can improve the roughness of the skin and has the effect of immediately pulling and tightening the skin. The method is simple, is easy to realize industrial production, solves the problems of low yield and difficult filtration of the polysaccharide extracted from the boat-fruited sterculia seed in the prior art, and has higher application value.
Description
Technical Field
The invention relates to a preparation method and application of a boat-fruited sterculia seed extract.
Background
Boat-fruited sterculia seed, which is the mature seed of a plant of Pinna genus of Sterculiaceae family, has obvious effects of lowering blood pressure, moistening throat and reducing phlegm, and is used as a traditional medicine-food dual-purpose medicinal material for clearing heat from throat and benefiting throat. Its history of use is recorded in Bencao Shi Yi (supplement to materia Medica), which is called Annan Zi. Modern scientific researches show that the seed coat of scaphium scaphigerum contains polysaccharide components such as galactose, pentose and the like, in addition, active components such as fat-sea weed, tannin, phenolic acid, amino acid and the like, and calcium and magnesium microelements, and the polysaccharide is a functional component of the seed coat, and has the functions of resisting inflammation, treating bacillary dysentery and inhibiting the formation of calcium oxalate crystals.
At present, relevant reports about the active ingredients of the scaphium scaphigerum are mainly focused on the polysaccharide ingredients of the scaphium scaphigerum, and the extraction and preparation processes are mostly a solvent hot dipping method, an enzyme method, an ultrasonic auxiliary method and a microwave auxiliary method. The existing extraction and preparation method for the boat-fruited sterculia seed has the problems of low yield of active polysaccharide, difficult filtration and the like.
Disclosure of Invention
Based on the defects of the prior art, the invention aims to solve the problems of improving the extraction rate of the active polysaccharide substance of the scaphium scaphigerum, reducing the viscosity index of the polysaccharide and providing the preparation process of the active polysaccharide of the scaphium scaphigerum with high extraction rate, thereby fully utilizing the extract of the scaphium scaphigerum.
The technical problem to be solved by the invention is realized by the following technical scheme:
pulverizing semen Scaphii Lychnophori, mixing with water, extracting at certain temperature under certain pressure, and filtering to obtain semen Scaphii Lychnophori extract.
According to the invention, the extraction temperature is 110-135 ℃.
According to the invention, the pressure is 0.11-0.19 MPa.
According to the invention, the extraction time is 0.5-3.0 h.
According to some preferred embodiments of the present invention, the extraction temperature is 110 to 128 ℃, the extraction pressure is 0.11 to 0.17 MPa, and the extraction time is 1.0 to 2.0 hours.
According to still further preferred embodiments of the present invention, the extraction temperature is 121 ℃, the pressure conditions are 0.13 MPa, and the extraction time is 1.0 h.
According to the invention, the mass ratio of the boat-fruited sterculia seed to the water is 1: 20-1: 80.
According to the invention, the mass ratio of the boat-fruited sterculia seed to the water is 1: 20.
According to the invention, the used boat-fruited sterculia seed is dry boat-fruited sterculia seed, which is crushed and then passes through a 24-40 mesh sieve;
according to the invention, the water used is preferably deionized water.
In another aspect, the invention provides a boat-fruited sterculia seed extract obtained by the preparation method and a composition containing the boat-fruited sterculia seed extract.
According to the present invention, the composition comprises the scaphium scaphigerum extract and a dispersing agent.
According to the invention, the dispersant is one or more of trehalose, maltodextrin, beta-cyclodextrin and mannitol.
According to the invention, the dispersant is used in an amount of 10 to 45% by weight of the composition.
According to the invention, the composition is prepared by the following steps:
(1) the boat-fruited sterculia seed extract is decolored by adding 0.5-2.0% of active carbon;
(2) filtering the mixture;
(3) compounding the filtrate with dispersant, drying and sterilizing.
In the above method, the drying method is one of freeze drying, low-temperature vacuum drying or spray drying.
In the method, the sterilization method is Co60 sterilization.
In another aspect, the invention provides the use of the boat-fruited sterculia seed extract or boat-fruited sterculia seed composition in skin care products.
The invention has the beneficial effects that:
the boat-fruited sterculia seed extract obtained by the preparation process has the advantages that the yield of boat-fruited sterculia seed polysaccharide is improved, and the molecular weight of the polysaccharide and the viscosity of an aqueous solution are reduced compared with those of a normal-pressure boiling method. Solves the problems of the prior art that the scaphium scaphigerum polysaccharide has large molecular weight, is not easy to be absorbed by skin, has large viscosity and is difficult to filter. The obtained boat-fruited sterculia seed extract or the composition is applied to skin, can improve the roughness of the skin, has the effect of immediately pulling and tightening the skin and the moistening feeling, and has wide application prospect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the following will be briefly described.
FIG. 1 is a graph showing the molecular weight distribution of the extract of Sterculia Lychnophora obtained by atmospheric cooking of Sterculia Lychnophora;
FIG. 2 is a graph showing the molecular weight distribution of the boat-fruited sterculia seed extract obtained by the process of the present invention;
FIG. 3 shows the effect of the skin care product of boat-fruited sterculia seed extract on skin smoothness SEsm;
FIG. 4 shows the effect of the skin care product of boat-fruited sterculia seed extract obtained by the preparation method of the invention on the average roughness R3 of skin;
Fig. 5 is a graph showing the results of the skin firming and moisturizing effect evaluation of the boat-fruited sterculia seed composition obtained by the preparation method of the present invention.
Detailed Description
The invention is further illustrated below with reference to specific examples, to which, however, the invention is not restricted.
The experimental procedures described in the following examples, unless otherwise specified, have conventional procedures; the experimental materials and reagents are commercially available, unless otherwise specified.
In the following examples, the starting materials used: boat-fruited sterculia seed is purchased from Beijing Hoorendong drugstore.
The apparatus used in the present invention is shown in table 1.
TABLE 1 test apparatus
| Name (R) | Model number | Suppliers of goods |
| Vertical high-pressure steam sterilizing pot | LDZM-30L-II | Shanghai Shenan high-pressure sterilizer |
| Vacuum freeze drier | LGJ-30FD | Beijing Songyuan Huaxing science and technology development company |
Test method
1. Polysaccharide test method: testing the polysaccharide yield in the boat-fruited sterculia seed extract by adopting an alcohol precipitation and phenol-sulfuric acid method (reference standard: QB/T2488-;
2. the polysaccharide molecular weight test method comprises the following steps: gel Permeation Chromatography (GPC) is adopted to detect the molecular weight and distribution of polysaccharide in the boat-fruited sterculia seed extract. The GPC method is based on a size exclusion separation mechanism, integrating a differential refractive detector and a laser light scattering detector to analyze the molecular weight distribution.
The specific test method comprises the following steps:
preparation of standard solution: 93.0 mg oat glucan, 25 mL mobile phase (0.1 mol. L) was weighed -1 NaNO 3 Solution and 0.02% NaN 3 ) Fixing the volume, mixing uniformly and preparing into 3.72 mg/mL -1 Standard oat glucan mother liquor; weighing 900 μ L of oat dextran standard mother liquor, 2700 μ L of mobile phase, and making into 0.930 mg/mL -1 Standard solutions of oat glucan.
GPC analysis conditions: gel chromatography column: SUGAR KS-805 (8.0X 300 mm, 7 μm) SUGAR KS-803 (8.0X 300 mm, 6 μm); mobile phase: 0.1 mol. L -1 NaNO 3 Solution (containing 0.02% NaN) 3 ) (ii) a Flow rate of 0.8 mL/min -1 (ii) a Column temperature: 60 ℃; differential Refractometer (RID) detection temperature: 50 ℃; sample introduction volume: 100 μ L.
The standard curve for measuring oat glucan is Y =786302 XX-24604, X is the peak area, and Y is the polysaccharide content. And F is the final volume of the sample according to the dendrobium polysaccharide content (mg/g) = oat glucan standard curve multiplied by F/sample sampling mass.
3. Viscosity test method: reference is made to GB/T15357-2014 surfactant and detergent rotational viscometers for determining viscosity and flow properties of liquid products.
Example 1
Selecting appropriate amount of semen Scaphii Lychnophori, pulverizing, sieving with 24-40 mesh sieve (24 mesh sieve, 40 mesh sieve for use), adding deionized water at a ratio of 1:20 (m/m), decocting at 110 deg.C under 0.11 MPa for 1.0 h, and filtering to obtain semen Scaphii Lychnophori extract.
Example 2
Selecting appropriate amount of semen Scaphii Lychnophori, pulverizing, sieving with 24-40 mesh sieve (24 mesh sieve, 40 mesh sieve for use), adding deionized water at a ratio of 1:20 (m/m), decocting at 110 deg.C under 0.11 MPa for 1.5 hr, and filtering to obtain semen Scaphii Lychnophori extract.
Example 3
Selecting appropriate amount of semen Scaphii Lychnophori, pulverizing, sieving with 24-40 mesh sieve (24 mesh sieve, 40 mesh sieve for use), adding deionized water at a ratio of 1:20 (m/m), decocting at 110 deg.C under 0.11 MPa for 2.0 h, and filtering to obtain semen Scaphii Lychnophori extract.
Example 4
Selecting appropriate amount of semen Scaphii Lychnophori, pulverizing, sieving with 24-40 mesh sieve (24 mesh sieve, 40 mesh sieve for use), adding deionized water at a ratio of 1:20 (m/m), decocting at 121 deg.C under 0.13 MPa for 1.0 h, and filtering to obtain semen Scaphii Lychnophori extract.
Example 5
Selecting appropriate amount of semen Scaphii Lychnophori, pulverizing, sieving with 24-40 mesh sieve (24 mesh sieve, 40 mesh sieve for use), adding deionized water at a ratio of 1:20 (m/m), decocting at 128 deg.C and 0.17 MPa for 1.0 h, and filtering to obtain semen Scaphii Lychnophori extract.
Example 6
Selecting appropriate amount of semen Scaphii Lychnophori, pulverizing, sieving with 24-40 mesh sieve (24 mesh sieve, 40 mesh sieve for use), adding deionized water at a ratio of 1:30 (m/m), decocting at 110 deg.C under 0.11 MPa for 1.0 h, and filtering to obtain semen Scaphii Lychnophori extract.
Example 7
Selecting appropriate amount of semen Scaphii Lychnophori, pulverizing, sieving with 24-40 mesh sieve (24 mesh sieve, 40 mesh sieve for use), adding deionized water at a ratio of 1:40 (m/m), decocting at 110 deg.C under 0.11 MPa for 1.0 h, and filtering to obtain semen Scaphii Lychnophori extract.
Example 8
Selecting appropriate amount of semen Scaphii Lychnophori, pulverizing, sieving with 24-40 mesh sieve (24 mesh sieve, 40 mesh sieve for use), adding deionized water at a ratio of 1:60 (m/m), decocting at 110 deg.C under 0.11 MPa for 1.0 h, and filtering to obtain semen Scaphii Lychnophori extract.
Example 9
Selecting appropriate amount of semen Scaphii Lychnophori, pulverizing, sieving with 24-40 mesh sieve (24 mesh sieve, 40 mesh sieve for use), adding deionized water at a ratio of 1:80 (m/m), decocting at 110 deg.C under 0.11 MPa for 1.0 h, and filtering to obtain semen Scaphii Lychnophori extract.
Example 10
Selecting appropriate amount of semen Scaphii Lychnophori, pulverizing, sieving with 24-40 mesh sieve (24 mesh sieve, 40 mesh sieve for use), adding deionized water at a ratio of 1:20 (m/m), decocting at 110 deg.C under 0.11 MPa for 0.5 hr, and filtering to obtain semen Scaphii Lychnophori extract.
Example 11
Selecting appropriate amount of semen Scaphii Lychnophori, pulverizing, sieving with 24-40 mesh sieve (24 mesh sieve, 40 mesh sieve for use), adding deionized water at a ratio of 1:20 (m/m), decocting at 110 deg.C under 0.11 MPa for 3.0 h, and filtering to obtain semen Scaphii Lychnophori extract.
Example 12
Selecting appropriate amount of semen Scaphii Lychnophori, pulverizing, sieving with 24-40 mesh sieve (24 mesh sieve, 40 mesh sieve for use), adding deionized water at a ratio of 1:20 (m/m), decocting at 135 deg.C under 0.19 MPa for 1.0 h, and filtering to obtain semen Scaphii Lychnophori extract.
Comparative example 1 (atmospheric cooking technique)
Selecting appropriate amount of semen Scaphii Lychnophori, pulverizing, sieving with 24-40 mesh sieve (24 mesh sieve and 40 mesh sieve for use), adding deionized water at a ratio of 1:40 (m/m), steaming at 95-100 deg.C under normal pressure for 1.0 hr, and filtering to obtain semen Scaphii Lychnophori extract.
Comparative example 2
Selecting appropriate amount of semen Scaphii Lychnophori coarse powder, sieving with 24 mesh sieve, collecting the sieve, adding deionized water at a ratio of 1:20 (m/m), decocting at 110 deg.C under 0.11 Mpa for 1.0 hr, and filtering to obtain semen Scaphii Lychnophori extractive solution.
The experimental results are as follows:
taking a raw material boat-fruited sterculia seed, taking water as an extraction solvent, extracting by the processes of examples and comparative examples, and testing the yield of polysaccharide in an extracting solution, wherein the test results are as follows:
TABLE 2 polysaccharide yield in extract
The polysaccharide yield is taken as a research target, micro-pressure extraction preparation is adopted, and the influence of the granularity of raw materials, different material-liquid ratios, extraction time, extraction temperature and corresponding pressure on the target product polysaccharide is inspected. The inventor uses the same preparation process as the example 2, and only the crushed boat-fruited sterculia seed has different particle sizes (24 meshes, and the upper part of the dried sieve is taken), so that the particle size is larger (more than or equal to 24 meshes), and the yield of the polysaccharide is low (9.8%); when the particle size is smaller (< 40 meshes), the filtration is difficult and the industrialization is not easy to realize.
The data in table 2 show that the preferred preparation process is: the granularity of the boat-fruited sterculia seed is 24-40 meshes, the material-liquid ratio is 1:20-1:80 (m/m), the extraction time is 1.0-2.0 h, the micro-pressure extraction temperature is 110-.
The extract of boat-fruited sterculia seed obtained in example 4 was freeze-dried, and the physicochemical indices of the boat-fruited sterculia seed extract were further examined.
GPC measurement of molecular weight and distribution: 1.00 g of Sterculia Lychnophora extract was accurately weighed, dissolved in deionized water to prepare a 1% aqueous solution, and analyzed for polysaccharide molecular weight and distribution by GPC gel chromatography.
TABLE 3 physicochemical Properties of Sterculia Lychnophora extract
The polysaccharide component in the boat-fruited sterculia seed is extracted by a micro-pressure extraction technology, the polysaccharide yield is improved by 81.5%, the polysaccharide molecular weight distribution is reduced by 1 order of magnitude, meanwhile, the viscosity of a 2% aqueous solution is reduced to 1/2 of the viscosity under the same concentration of a normal-pressure decocting method, the problems that the polysaccharide has large molecular weight, is not easy to be absorbed by skin, the viscosity index is reduced, and the problems of large viscosity and difficult filtration in process preparation are solved.
Skin care efficacy test
1. Preparation method of semen Scaphii Lychnophori extract composition
Adding 1.5 percent of activated carbon into the boat-fruited sterculia seed extract obtained in the example 4 for decolorization, filtering, compounding with 36 percent of mannitol, freeze-drying the filtrate, and sterilizing by Co60 to obtain the boat-fruited sterculia seed extract composition.
Sample preparation
According to the formulation of table 4, the boat-fruited sterculia seed extract compositions prepared in the above example 4 and comparative example 1 were prepared into samples to be tested, respectively, and skin care efficacy test was performed.
TABLE 4 formula of sample to be tested and preparation process
The preparation process comprises the following steps:
(1) heating the phase A raw material to 80 ℃, and uniformly mixing for later use;
(2) stirring and cooling, adding the B-phase raw material at 60 ℃, and stirring uniformly;
(3) stirring and cooling, adding the C-phase raw material below 40 ℃, and stirring uniformly;
(4) stirring and cooling, discharging at 38 ℃, and adding the phase D.
3. Skin roughness test
The roughness was measured with a Visioscan VC98 image analyzer. The results are expressed by detecting the change rate of skin smoothness parameter SEsm and the change rate of average wrinkle depth R3; wherein: the SEsm index may characterize the degree of smoothness of the skin, with the smaller the value, the smoother the skin. The R3 index indicates the mean wrinkle depth, the smaller the R3 value, the less rough the skin, according to the skin wrinkle-roughness index meaning.
Wherein:
and (3) a formula for calculating the smoothness parameter SEsm change rate (%) shown in the formula (1).
In formula (1):S 0 -skin base data acquisition without sample application;Sn-the value collected at each time point after sample smearing.
The average wrinkle depth R3 change rate (%) is calculated as shown in formula (2).
In the formula (2):R 0 -skin base data acquisition without sample application;Rn-the value collected at each time point after sample smearing.
(1) Volunteer screening
Dry skin is the case when the age is 28-60 years old.
(2) Test method
Selecting 24 volunteers, and dividing into experimental group and control group, wherein the experimental group uses skin care sample containing 2% of semen Scaphii Lychnophori extract composition prepared in example 4; control group 1 used a skin care sample containing 2% of the boat-fruited sterculia seed extract composition prepared in comparative example 1; the control group 2 was coated with a formulation base which was the same as the sample to be tested except that no sterculia lychnophora extract composition was added); each group had 8 persons.
The volunteers applied the samples to the test area twice a day in the morning and in the evening, and the improvement effect of the samples on the skin roughness was evaluated by testing the smoothness parameter SEsm of the skin surface and the average wrinkle depth R3 before (0 w), after 1w, 2w, and 4 w.
(3) Test results
The difference of each index of a single product before and after use is analyzed by a Dunnett analysis method in STATISTICA software if the data are in normal distribution, a rank sum test in SPSS software if the data are in abnormal distribution, and the difference between two products at the same time point is analyzed by a t test.
The results of the smoothness parameter SEsm test (fig. 3) show that the smoothness parameter SEsm is reduced by 23% from the initial value after using the sample of the boat-fruited sterculia seed extract composition containing 2% of example 4 for 4 weeks, which is higher than the sample of the boat-fruited sterculia seed extract composition containing 2% of comparative example 1 (-14.3%), and the change rate of the formula matrix (-7.7%), which shows that the 2% boat-fruited sterculia seed extract composition can effectively improve the smoothness of the skin, and has significant difference compared with the control group (see (b))p<0.05）。
The average wrinkle depth R3 test results (FIG. 4) showed that the average wrinkle depth R3 was reduced by 38% from the initial value after using the composition comprising 2% of the extract of Sterculia Lychophora according to example 4 for 4 consecutive weeks, which was superior to the composition comprising 2% of the extract of Sterculia Lychophora prepared according to comparative example 1 (-25.6%), and the change rate of the formula base (-14.1%), indicating that the 2% extract of Sterculia Lychophora was effective in improving the skin roughness, and showed significant difference compared to the formula base group (see (b) (FIG. 4))p<0.05）。
4. Skin firming and moisturizing test
(1) Volunteer selection
60 volunteers were selected.
(2) Test method
Volunteers were randomly divided into 3 groups of 20 persons, the first group using a sample containing 2% of the boat-fruited sterculia seed extract composition prepared in example 4, the second group using a sample containing 2% of the boat-fruited sterculia seed extract composition prepared in comparative example 1, and the third group using a formula base not containing the boat-fruited sterculia seed extract composition, the rest being the same, and the effects were evaluated by applying to the skin around the canthus, and feeding back the skin lifting, tightening, and moisturizing effects using questionnaires.
(3) Test results
The results (fig. 5) show that more than 80% of the volunteers fed back the composition sample containing 2% of the extract of scaphium scaphigerum prepared in example 4 had a skin-tightening feeling and a moisturizing feeling, and the effect was superior to that of the comparative example.
Claims (5)
1. A method for preparing a boat-fruited sterculia seed extract comprises the following steps: pulverizing semen Scaphii Lychnophori, mixing with water, extracting at certain temperature under certain pressure, and filtering to obtain semen Scaphii Lychnophori extract;
the extraction temperature is 121 ℃, the pressure condition is 0.13 MPa, the extraction time is 1.0 h, and the addition ratio of the crushed boat-fruited sterculia seeds to the deionized water is 1: 20.
2. a skin care composition comprising the scaphium scaphigerum extract of claim 1 and a dispersing agent which is one or more of trehalose, maltodextrin, beta-cyclodextrin and mannan.
3. The composition according to claim 2, wherein the dispersant is present in an amount ranging from 10 to 45% by weight relative to the total weight of the composition.
4. The composition of claim 2, wherein the composition is prepared by:
(1) the scaphium scaphigerum extract of claim 1 is decolored by adding 0.5 to 2.0 percent of activated carbon;
(2) filtering the mixture;
(3) Compounding the filtrate with dispersant, drying and sterilizing.
5. Use of the extract of scaphium scaphigerum as claimed in claim 1 or the composition as claimed in any one of claims 2 to 4 for the preparation of a skin care product.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000247829A (en) * | 1999-02-24 | 2000-09-12 | Mikimoto Pharmaceut Co Ltd | Cosmetic, unregulated drug, medicine and food |
| CN101372514A (en) * | 2007-08-21 | 2009-02-25 | 光明乳业股份有限公司 | Scaphium scaphigerum polysaccharide, preparation and use thereof |
| CN110585302A (en) * | 2019-10-16 | 2019-12-20 | 佳木斯大学 | Traditional Chinese medicine combined granular tea for treating chronic pharyngitis and preparation method thereof |
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2020
- 2020-08-31 CN CN202010892090.5A patent/CN113952262B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000247829A (en) * | 1999-02-24 | 2000-09-12 | Mikimoto Pharmaceut Co Ltd | Cosmetic, unregulated drug, medicine and food |
| CN101372514A (en) * | 2007-08-21 | 2009-02-25 | 光明乳业股份有限公司 | Scaphium scaphigerum polysaccharide, preparation and use thereof |
| CN110585302A (en) * | 2019-10-16 | 2019-12-20 | 佳木斯大学 | Traditional Chinese medicine combined granular tea for treating chronic pharyngitis and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 胖大海水溶性多糖的提取;周郑坤等;《西北林学院学报》;20060730;第129-131页 * |
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