CN116004319A - Preparation method and application of papermulberry fruit oil with high linoleic acid content - Google Patents
Preparation method and application of papermulberry fruit oil with high linoleic acid content Download PDFInfo
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- CN116004319A CN116004319A CN202310279209.5A CN202310279209A CN116004319A CN 116004319 A CN116004319 A CN 116004319A CN 202310279209 A CN202310279209 A CN 202310279209A CN 116004319 A CN116004319 A CN 116004319A
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- papermulberry fruit
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- papermulberry
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention belongs to the technical field of cosmetics and medicines, and particularly relates to application of papermulberry fruit oil with high linoleic acid content in cosmetics. The preparation method provided by the invention comprises the following steps: parching fructus Broussonetiae, and squeezing to obtain fructus Broussonetiae crude oil; the stir-frying temperature is less than or equal to 60 ℃; heating and mixing the papermulberry fruit crude oil and the acid clay, and standing to obtain a mixture; the standing temperature is more than or equal to 60 ℃; filtering the mixture through a membrane to obtain the papermulberry fruit oil. The invention adopts a mechanical squeezing method, cold-presses at the squeezing temperature of less than or equal to 60 ℃, does not damage the molecular structure of unsaturated fatty acid, can better retain the unsaturated fatty acid active ingredients of papermulberry fruit in oil, and improves the content of unsaturated fatty acid; and secondly, the preparation method provided by the invention does not need high-temperature distillation and solvent removal, is simple and low in cost, and can prepare the unsaturated fatty acid papermulberry fruit oil with the functions of resisting inflammation and allergy, relieving, moisturizing, brightening and whitening and resisting photoaging.
Description
Technical Field
The invention belongs to the technical field of cosmetics and medicines, and particularly relates to a preparation method and application of papermulberry fruit oil with high linoleic acid content.
Background
The fructus Broussonetiae is dry mature fruit of Broussonetia papyrifera of Moraceae. Fructus Broussonetiae has sweet and cold nature, no toxicity, and has effects of replenishing kidney essence, nourishing yin, removing liver fire for improving eyesight, inducing diuresis for removing edema, etc., and is commonly used for treating liver-kidney yin deficiency, bone steaming hectic fever, night sweat and nocturnal emission, dizziness, nebula, edema and fullness, dysuria, etc. Clinically, fructus Broussonetiae is mainly used for treating senile dementia, chronic hepatitis C, liver cirrhosis, chronic nephritis, ophthalmic diseases, infertility, alopecia areata, etc.
The traditional extraction and purification method of papermulberry fruit oil comprises the steps of extracting papermulberry fruit which is crushed and sieved by using organic solvents such as petroleum ether and the like, filtering a solution which is subjected to cold leaching or leakage by using a petroleum ether cold leaching method or a leakage method, concentrating and recovering the solvent to obtain brown papermulberry fruit oil; then adding papermulberry fruit oil onto silica gel column, respectively using solvents with different polarities such as: washing the column with diethyl ether, acetone, etc., and recovering solvent to obtain fructus Broussonetiae oil extract. Since the petroleum ether extracted grease contains impurities including pigments, volatile oil, small polar substances and saturated fatty acids, solvents with different polarities are needed for purification. The process has the advantages of poor selectivity of unsaturated fatty acid in papermulberry fruit, low content, easy existence of organic solvent residue and inapplicability to industrial production.
Chinese patent CN1605618A discloses a method for preparing and purifying plant linoleic acid, which comprises the following steps: the papermulberry fruit raw material is dried, crushed and sieved to obtain papermulberry fruit powder; CO 2 Preparing papermulberry fruit oil by circulating supercritical extraction: first, the system is prepared and fed; regulating the rotating speed, the flow speed and the vacuum degree, and distilling to remove low boiling components; when the molecular distillation device is at a certain temperature and vacuum degree, the speed of a rotor and the flow rate of papermulberry fruit oil from which low boiling point components are removed are regulated when the feed inlet is at a certain temperature, and crude linoleic acid is obtained by distillation; and when the molecular distillation device is at a certain temperature and vacuum degree, the speed of scraping the film by the rotor and the flow speed of crude linoleic acid are regulated at a certain temperature by the sample inlet, and unsaturated fatty acid linoleic acid pure product is obtained by distillation, so that organic solvent residues are avoided. But due to supercritical CO 2 Volatile oil, monoterpene substances and saturated fatty acid substances are extracted at the same time during the extraction, so that the subsequent distillation method is still needed to remove volatile substances, and the operation process is complicated.
Disclosure of Invention
The invention aims to provide a preparation method and application of papermulberry fruit oil with high linoleic acid content, and the extraction and purification method provided by the invention adopts a squeezing method to directly squeeze unsaturated fatty acid in papermulberry fruit, has high content of active ingredients and no organic solvent residue, has the effects of anti-inflammatory, relieving, whitening and anti-photoaging, and can be widely applied to daily chemical industry.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides application of papermulberry fruit oil in cosmetics, wherein the cosmetics comprise one or more of skin photoaging resisting cosmetics, moisturizing cosmetics, whitening cosmetics and anti-inflammatory and anti-allergic cosmetics; the preparation method of the papermulberry fruit oil comprises the following steps:
parching fructus Broussonetiae, and squeezing to obtain fructus Broussonetiae crude oil; the stir-frying temperature is less than or equal to 60 ℃;
heating and mixing the papermulberry fruit crude oil and acid clay, and standing to obtain a mixture; the standing temperature is more than or equal to 60 ℃;
filtering the mixture through a membrane to obtain the papermulberry fruit oil.
Preferably, the membrane filtration comprises sequentially performing a first membrane filtration and a second membrane filtration;
the diameters of the filter membranes used for the first membrane filtration and the second membrane filtration are independently 1-5 mu m, and the pressures of the first membrane filtration and the second membrane filtration are independently 0.02-0.06 MPa.
Preferably, the stir-frying temperature is 40-60 ℃.
Preferably, the standing temperature is 60-80 ℃; the standing time is 20-30 min.
Preferably, the acid clay accounts for 1-4% of the papermulberry fruit crude oil by mass.
Preferably, the water content of the papermulberry fruit is 6-8%.
Preferably, in the anti-inflammatory and anti-allergic cosmetic, the effective mass percentage of the papermulberry fruit oil is 0.025-10%;
in the whitening cosmetic, the effective mass percentage of the papermulberry fruit oil is 0.0006-5%;
in the skin photoaging resistant cosmetic, the effective mass percentage of the papermulberry fruit oil is 0.003-5%.
The invention provides an anti-inflammatory and anti-sensitization cosmetic, which comprises papermulberry fruit oil and a cosmetic matrix; the preparation method of the papermulberry fruit oil comprises the following steps:
parching fructus Broussonetiae, and squeezing to obtain fructus Broussonetiae crude oil; the stir-frying temperature is less than or equal to 60 ℃;
heating and mixing the papermulberry fruit crude oil and acid clay, and standing to obtain a mixture; the standing temperature is more than or equal to 60 ℃;
filtering the mixture through a membrane to obtain the papermulberry fruit oil.
Preferably, the cosmetic base comprises cetostearyl alcohol, a nonionic sugar-based emulsifier, vitamin E, caprylic/capric triglyceride, 1, 3-butanediol, glycerol, ammonium acryloyldimethyl taurate, water, p-hydroxyacetophenone, and 1,2 hexanediol.
The invention provides application of papermulberry fruit oil in cosmetics, wherein the cosmetics comprise one or more of skin photoaging resisting cosmetics, moisturizing cosmetics, whitening cosmetics and anti-inflammatory and anti-allergic cosmetics; the preparation method of the papermulberry fruit oil comprises the following steps: parching fructus Broussonetiae, and squeezing to obtain fructus Broussonetiae crude oil; the stir-frying temperature is less than or equal to 60 ℃; heating and mixing the papermulberry fruit crude oil and the acid clay, and standing to obtain a mixture; the standing temperature is more than or equal to 60 ℃; filtering the mixture through a membrane to obtain the papermulberry fruit oil. The invention adopts a mechanical squeezing method, cold-presses at the squeezing temperature of less than or equal to 60 ℃, does not damage the molecular structure of unsaturated fatty acid, can better retain unsaturated fatty acid active ingredients with the functions of anti-inflammatory, anti-sensitization, relieving, moisturizing, brightening, whitening and resisting photoaging in papermulberry fruit oil, and improves the content of unsaturated fatty acid; secondly, the preparation method provided by the invention does not need high-temperature distillation and solvent removal, is simple and low in cost, and the prepared papermulberry seed oil is rich in unsaturated fatty acid; finally, the invention uses acid clay to decolorize papermulberry fruit crude oil, and uses the strong adsorption force of acid clay to adsorb pigment and other impurities in the oil, thereby achieving the purposes of improving the oil color and removing impurities, and also effectively removing trace metal ions and substances which can cause poisoning of hydrogenation catalyst in the oil. The results of the examples show that the linoleic acid content in the papermulberry fruit oil prepared by the preparation method provided by the invention is as high as 83.8%. The papermulberry fruit oil prepared by the preparation method disclosed by the technical scheme has obvious inhibition effect on TNF-alpha and NO, obvious inhibition effect on melanin secretion, and obvious inhibition effect on ROS expression, so that the papermulberry fruit oil prepared by the preparation method disclosed by the technical scheme has the effects of anti-inflammatory, relieving, whitening and resisting photoaging, and can be widely applied to the daily chemical industry.
Drawings
Fig. 1 is a flowchart of a preparation method of papermulberry fruit oil according to an embodiment of the present invention;
FIG. 2 shows the inhibition of TNF- α concentration by papermulberry fruit oil;
FIG. 3 shows the inhibition of NO by papermulberry fruit oil;
FIG. 4 is the effect of papermulberry fruit oil on B16-F10 cell viability;
FIG. 5 is the effect of papermulberry fruit oil on B16-F10 melanin secretion;
FIG. 6 is the effect of papermulberry seed oil on Hacat cell viability;
FIG. 7 is the effect of papermulberry fruit oil on ROS secretion;
FIG. 8 is the effect of papermulberry fruit oil on water activity at various times;
fig. 9 is a graph showing the effect of the papermulberry fruit oil moisturizing cream in eliminating red swelling.
Detailed Description
The invention provides application of papermulberry fruit oil in cosmetics, which is characterized in that the cosmetics comprise one or more of anti-skin photoaging cosmetics, moisturizing cosmetics, whitening cosmetics and anti-inflammatory and anti-allergic cosmetics; the preparation method of the papermulberry fruit oil comprises the following steps:
parching fructus Broussonetiae, and squeezing to obtain fructus Broussonetiae crude oil; the stir-frying temperature is less than or equal to 60 ℃;
heating and mixing the papermulberry fruit crude oil and acid clay, and standing to obtain a mixture; the standing temperature is more than or equal to 60 ℃;
filtering the mixture through a membrane to obtain the papermulberry fruit oil.
In the present invention, all preparation materials/components are commercially available products well known to those skilled in the art unless specified otherwise.
The invention stir-fries fructus Broussonetiae and presses to obtain fructus Broussonetiae crude oil; the stir-frying temperature is less than or equal to 60 ℃.
In the invention, the water content of the papermulberry fruit is preferably 6-8%, more preferably 7%.
In the invention, the temperature of stir-frying is preferably 40-60 ℃, more preferably 60 ℃.
In the invention, the heat preservation time of stir-frying is preferably 5-8 min, more preferably 6min.
In the invention, the stir-frying is preferably performed in an oil press.
In the present invention, the pressing is preferably performed in an oil press.
In the present invention, the pressing pressure is preferably 30MPa.
After obtaining the fructus Broussonetiae crude oil, heating and mixing the fructus Broussonetiae crude oil and the acid clay, and standing to obtain a mixture; the standing temperature is more than or equal to 60 ℃.
In the invention, the acid clay accounts for 1-4% of the papermulberry fruit crude oil by mass, and more preferably 1.5-3%.
In the present invention, the temperature of the mixing is preferably 60 to 80 ℃, more preferably 70 ℃. In the present invention, the mixing is preferably performed under stirring conditions, and the present invention has no particular requirement for the specific trial process of the stirring.
In the present invention, the temperature of the standing is preferably 60 to 80 ℃, more preferably 70 ℃.
In the invention, the standing heat preservation time is preferably 20-30 min, more preferably 30min.
After the mixture is obtained, the invention filters the mixture through a membrane to obtain the papermulberry fruit oil.
In the invention, the mixture is preferably cooled to 25 ℃ for the membrane filtration.
In the present invention, the membrane filtration includes sequentially performing a first membrane filtration and a second membrane filtration.
In the present invention, the diameter of the filter membrane used for the first membrane filtration is preferably 1 to 5 μm, more preferably 2 to 4 μm. In the present invention, the pressure of the first membrane filtration is preferably 0.02 to 0.06mpa, more preferably 0.03 to 0.05mpa.
In the present invention, the diameter of the filter membrane used for the second membrane filtration is preferably 1 to 5 μm, more preferably 2 to 4 μm. In the present invention, the pressure of the second membrane filtration is preferably 0.02 to 0.06mpa, more preferably 0.03 to 0.05mpa.
The invention provides papermulberry fruit oil prepared by the preparation method. In the invention, the acid value of the papermulberry fruit oil is preferably 11.9-12.2 mg/g; the peroxide value is 0.012-0.064 g/100g; in the papermulberry fruit oil, the linoleic acid content is up to 83.8%.
In the anti-inflammatory and anti-allergic cosmetic, the effective mass percentage of the papermulberry fruit oil is preferably 0.025-10%.
In the whitening cosmetic, the effective mass percentage of the papermulberry fruit oil is preferably 0.0006-5%.
In the anti-skin photoaging cosmetic, the effective mass percentage of the papermulberry fruit oil is preferably 0.003-5%.
The invention provides an anti-inflammatory and anti-sensitization cosmetic, which comprises papermulberry fruit oil and a cosmetic matrix; the preparation method of the papermulberry fruit oil comprises the following steps:
parching fructus Broussonetiae, and squeezing to obtain fructus Broussonetiae crude oil; the stir-frying temperature is less than or equal to 60 ℃;
heating and mixing the papermulberry fruit crude oil and acid clay, and standing to obtain a mixture; the standing temperature is more than or equal to 60 ℃;
filtering the mixture through a membrane to obtain the papermulberry fruit oil.
In the present invention, the preparation method of the papermulberry fruit oil is the same as the preparation method of the papermulberry fruit oil described above, and will not be described in detail herein.
In the present invention, the cosmetic base includes cetostearyl alcohol, a nonionic sugar-based emulsifier, vitamin E, caprylic/capric triglyceride (GTCC), 1, 3-butylene glycol, glycerin, ammonium acryloyldimethyl taurate, water, p-hydroxyacetophenone, and 1,2 hexanediol.
In the present invention, the water is preferably deionized water.
In the present invention, the nonionic sugar-based emulsifier is particularly preferably M68.
In the invention, the anti-inflammatory and anti-allergic cosmetic provided by the invention comprises the following components in percentage by mass:
1% of cetostearyl alcohol, 1% of nonionic glycosyl emulsifier, 0.5% of vitamin E, 6% of GTCC, 0.5% of papermulberry fruit oil, 3% of 1, 3-butanediol, 6% of glycerol, 0.7% of ammonium acryloyldimethyl taurate, 0.2% of p-hydroxyacetophenone, 0.5% of 1, 2-hexanediol and the balance of water.
The technical solutions provided by the present invention are described in detail below with reference to the drawings and examples for further illustrating the present invention, but they should not be construed as limiting the scope of the present invention.
Example 1
Weighing 2-5 g of untreated papermulberry fruit medicinal material (purchased from Kunming self-honest traditional Chinese medicine) into a constant-weight flat bottle, precisely weighing, opening a bottle cover, drying at 105 ℃ for 5 hours, covering the bottle cover, placing the bottle cover in a dryer, cooling for 30 minutes, precisely weighing, drying at the temperature for 1 hour, cooling, weighing until the difference between two continuous weighing is not more than 5 mg. According to the weight loss, the water content in the test sample is calculated to be 7 percent (refer to the second method drying method of the third part (2015 edition) general rule 0823 of Chinese pharmacopoeia).
According to the preparation process shown in fig. 1, papermulberry fruit medicinal materials with the water content of 7% are selected and placed in a small oil press, a low-temperature pressing mode is selected and stir-fried for 6min at the temperature of 60 ℃, pressing (the pressing pressure is 30 MPa) is carried out to obtain pressed papermulberry fruit crude oil, the oil yield is calculated, and the relation between the water content and the oil yield in the embodiment is shown in table 1; the relation among the stir-frying temperature, the stir-frying time and the oil yield in this example is shown in Table 2.
Table 1 relation between water content and oil yield of papermulberry fruit medicinal material in example 1
TABLE 2 relation between stir-frying temperature, stir-frying time and oil yield in example 1
Placing cold pressed fructus Broussonetiae crude oil in a dry clean container, heating to 70deg.C, adding acid clay with 2% of crude oil quality, stirring, maintaining at 70deg.C for 30min, and naturally cooling to 25deg.C; the papermulberry fruit oil cooled to room temperature is placed on a positive pressure filter for filtration, and the first filtration is carried out: (the filtration mode is positive pressure filtration, the diameter of a filter membrane is 1-5 mu m, the pressure is 0.02-0.06 MPa, the filtered papermulberry fruit base oil is subpackaged, the papermulberry fruit oil is obtained, the acid value and the peroxide value of the papermulberry fruit oil prepared in the embodiment are calculated and tested, and the obtained test results are shown in Table 3.
TABLE 3 acid value and peroxide value of Broussonetia papyrifera seed oil prepared in example 1
Example 2
Weighing 2-5 g of untreated papermulberry fruit medicinal material (purchased from Kunming self-honest traditional Chinese medicine) into a constant-weight flat bottle, precisely weighing, opening a bottle cover, drying at 105 ℃ for 5 hours, covering the bottle cover, placing the bottle cover in a dryer, cooling for 30 minutes, precisely weighing, drying at the temperature for 1 hour, cooling, weighing until the difference between two continuous weighing is not more than 5 mg. According to the weight loss, the water content in the test sample is calculated to be 7 percent (refer to the second method drying method of the third part (2015 edition) general rule 0823 of Chinese pharmacopoeia).
According to the preparation process shown in fig. 1, papermulberry fruit medicinal materials with the water content of 7% are selected and put into a small oil press, and the papermulberry fruit crude oil is obtained by squeezing (the squeezing pressure is 30 MPa) after the papermulberry fruit medicinal materials are stir-fried for 6min at the temperature of 60 ℃ in a low-temperature squeezing mode.
Placing cold pressed fructus Broussonetiae crude oil in a dry clean container, heating to 80deg.C, adding acid clay with mass of 1% of crude oil, stirring, keeping at 80deg.C, standing for 10min, and naturally cooling to 25deg.C; the papermulberry fruit oil cooled to room temperature is placed on a positive pressure filter for filtration, and the first filtration is carried out: (the filtration mode is positive pressure filtration, the filter membrane is 1-5 mu m, the pressure is 0.02-0.06 MPa, the filtered papermulberry fruit base oil is subpackaged, the papermulberry fruit oil is obtained, the acid value and the peroxide value of the papermulberry fruit oil prepared in the embodiment are calculated and tested, and the obtained test results are shown in Table 4.
TABLE 4 acid value and peroxide value of Broussonetia papyrifera seed oil prepared in example 2
Example 3
Weighing 2-5 g of untreated papermulberry fruit medicinal material (purchased from Kunming self-honest traditional Chinese medicine) into a constant-weight flat bottle, precisely weighing, opening a bottle cover, drying at 105 ℃ for 5 hours, covering the bottle cover, placing the bottle cover in a dryer, cooling for 30 minutes, precisely weighing, drying at the temperature for 1 hour, cooling, weighing until the difference between two continuous weighing is not more than 5 mg. According to the weight loss, the water content in the test sample is calculated to be 7 percent (refer to the second method drying method of the third part (2015 edition) general rule 0823 of Chinese pharmacopoeia).
According to the preparation process shown in fig. 1, papermulberry fruit medicinal materials with the water content of 7% are selected and put into a small oil press, and the papermulberry fruit crude oil is obtained by squeezing (the squeezing pressure is 30 MPa) after the papermulberry fruit medicinal materials are stir-fried for 6min at the temperature of 60 ℃ in a low-temperature squeezing mode.
Placing cold pressed fructus Broussonetiae crude oil in a dry clean container, heating to 80deg.C, adding acid clay with 3% crude oil quality, stirring, standing at 80deg.C for 10min, and naturally cooling to 25deg.C; the papermulberry fruit oil cooled to room temperature is placed on a positive pressure filter for filtration, and the first filtration is carried out: (the filtration mode is positive pressure filtration, the filter membrane is 1-5 mu m, the pressure is 0.02-0.06 MPa, the filtered papermulberry fruit base oil is subpackaged, the papermulberry fruit oil is obtained, the acid value and the peroxide value of the papermulberry fruit oil prepared in the embodiment are calculated and tested, and the obtained test results are shown in Table 5.
TABLE 5 acid value and peroxide value of Broussonetia papyrifera seed oil prepared in example 3
Comparative example 1
Weighing 2-5 g of untreated papermulberry fruit medicinal materials (purchased from Kunming self-honest traditional Chinese medicines) into a constant-weight flat bottle, precisely weighing, opening a bottle cover, drying at 105 ℃ for 5 hours, covering the bottle cover, placing the bottle cover in a dryer, cooling for 30 minutes, precisely weighing, drying at the temperature for 1 hour, cooling, weighing until the difference between two continuous weighing is not more than 5 mg; according to the weight loss, the water content in the test sample is calculated to be 4 percent (refer to the second method drying method of the third part (2015 edition) general rule 0823 of Chinese pharmacopoeia).
In the comparative example, papermulberry fruit medicinal materials with the water content of 4% are selected in a small oil press, a low-temperature squeezing mode is selected, stir-frying is carried out for 6min at the temperature of 60 ℃, squeezing (the squeezing pressure is 30 MPa) is carried out, so that squeezed papermulberry fruit crude oil is obtained, the oil yield is calculated, and the relation between the water content and the oil yield is obtained as shown in table 6.
TABLE 6 relationship between moisture and oil yield in comparative example 1
Comparative example 2
Weighing 2-5 g of untreated papermulberry fruit medicinal material (purchased from Kunming self-honest traditional Chinese medicine) into a constant-weight flat bottle, precisely weighing, opening a bottle cover, drying at 105 ℃ for 5 hours, covering the bottle cover, placing the bottle cover in a dryer, cooling for 30 minutes, precisely weighing, drying at the temperature for 1 hour, cooling, weighing until the difference between two continuous weighing is not more than 5 mg. According to the weight loss, the water content in the test sample is calculated to be 10 percent (refer to the second method drying method of the third part (2015 edition) general rule 0823 of Chinese pharmacopoeia).
Selecting fructus Broussonetiae with water content of 10% in small oil press, parching at 60deg.C for 6min, squeezing (pressure of 30 MPa) to obtain crude fructus Broussonetiae oil, and calculating oil content to obtain water content and oil yield relationship shown in Table 7.
TABLE 7 relation between moisture and oil yield in comparative example 2
Comparative example 3
Weighing 2-5 g of untreated papermulberry fruit medicinal material (purchased from Kunming self-honest traditional Chinese medicine) into a constant-weight flat bottle, precisely weighing, opening a bottle cover, drying at 105 ℃ for 5 hours, covering the bottle cover, placing the bottle cover in a dryer, cooling for 30 minutes, precisely weighing, drying at the temperature for 1 hour, cooling, weighing until the difference between two continuous weighing is not more than 5 mg. According to the weight loss, the water content in the test sample is calculated to be 7 percent (refer to the second method drying method of the third part (2015 edition) general rule 0823 of Chinese pharmacopoeia).
Selecting fructus Broussonetiae with water content of 7% in a small oil press, parching at 120deg.C for 30min, squeezing (30 MPa pressure) to obtain fructus Broussonetiae crude oil, and calculating oil yield to obtain the relationship among parching temperature, parching time and oil yield in this comparative example as shown in Table 8.
TABLE 8 relation between stir-frying temperature, stir-frying time and oil yield in comparative example 3
Example 4
The papermulberry fruit oil prepared in example 1 was prepared into a cream according to the mass ratio of table 9.
Table 9 raw materials and mass% of the cream of example 4
The preparation method comprises the following steps:
cetostearyl alcohol, M68, vitamin E, GTCC and papermulberry fruit oil prepared in example 1 are mixed to obtain phase a.
Mixing 1, 3-butanediol, glycerol, ammonium acryloyldimethyl taurate and deionized water to obtain phase B.
P-hydroxyacetophenone and 1,2 hexanediol were mixed to give phase C.
Mixing the phase A, the phase B and the phase C to obtain the face cream.
Test example 1
In order to verify the safety and effectiveness of the papermulberry fruit oil obtained in the invention, the papermulberry fruit oil obtained in example 1 is selected for research.
1. Fatty acid content determination
1.1 Experimental methods and conditions
Reference is made to GB5009.168-2016 "determination of fatty acids in food", third method.
Chromatographic conditions: (1) capillary chromatography column: polydihydropropyl siloxane strong polar stationary phase, column length: 100mm, 0.25mm in inner diameter and 0.2 mu m in film thickness; injector temperature: 270 ℃; temperature during detection period: 280 ℃; programming temperature: the initial temperature is 100 ℃ and lasts for 13min; carrier gas: nitrogen gas; split ratio: 100:1; sample volume is 1.0 mu L; the detection conditions should satisfy the theoretical plate number (n) of at least 2000/m and the degree of separation (R) of at least 1.25.
1.3 Experimental procedure
5g of a uniform sample is weighed, the sample is transferred into a 250mL flat-bottomed flask, about 100mg of pyrogallic acid is added, a few zeolite particles are added, 2mL of ethanol aqueous solution with the volume percentage of 95% is added, and the mixture is uniformly mixed. 8mL of 2% sodium hydroxide methanol solution is added, the mixture is connected with a reflux condenser, reflux is carried out on the mixture in a water bath at 80 ℃ until oil drops disappear, 7mL of 15wt% boron trichloride methanol solution is added from the upper end of the reflux condenser, reflux is continued for 2min in the water bath at 80 ℃, the reflux condenser is flushed with a small amount of water, heating is stopped, a beaker is taken off from the water bath, and the mixture is rapidly cooled to room temperature. Accurately adding 20mL of n-heptane, shaking for 2min, adding saturated sodium chloride aqueous solution, standing for layering, sucking about 5mL of the upper n-heptane extraction solution, adding about 4g of anhydrous sodium sulfate into a 25mL test tube, shaking for 1min, standing for 5min, and sucking the upper solution into a sample bottle to be measured.
1.4 test results
According to the fatty acid content test result C18:2n-6C, the linoleic acid content was 83.8%.
Test example 2
Example 1 Effect of papermulberry seed oil on mouse macrophage inflammatory factor
1. Reagent preparation
1.1 LPS: LPS was prepared to a concentration of 200. Mu.g/mL with PBS and dispensed into 1.5mL centrifuge tubes at 100. Mu.L/tube and stored at-20℃for further use.
1.2 Positive control sample (dexamethasone sodium phosphate): precisely weighing a proper amount of dexamethasone sodium phosphate reference substance, preparing a DMEM basic culture medium into a concentration of 0.1mg/mL, and filtering and sterilizing with a 0.22 mu m filter membrane for later use.
1.3 Papermulberry fruit oil: proper amount of papermulberry fruit oil is measured by a pipette, prepared into a solution with 10 weight percent by DMSO, then diluted into a solution with 0.1 weight percent by DMEM basic culture, and subjected to gradient dilution.
2 experimental procedure
After 24h of cell plating, sample treatment and LPS stimulation are carried out, MTT is carried out after 24h, cell viability is measured, and NO and TNF-alpha content is measured.
2.1MTT assay for determining the effect of drugs on LPS-stimulated macrophage viability
2.1.1 cell Density was adjusted to 8X10 based on the results of the counting 4 cell/mL, cells were inoculated into 96-well plates at a volume of 200. Mu.L per well, and returned to the incubator for incubation (37 ℃,5% CO) 2 ）。
2.1.2 The drug addition treatment is shown in Table 10.
Table 10 medicated handling packet case
After 24 hours, the 96-well plate was removed, the old medium was discarded, the sample was added according to the procedure of Table 10, 4 wells per concentration were returned to the incubator (37 ℃,5% CO) 2 ) Continuing to culture; taking out the 96-well plate after 24 hours, collecting cell supernatant of each treatment group, centrifuging at 2000rpm for 10 minutes, collecting supernatant, preserving at-20 ℃, taking out before use, thawing, and avoiding repeated freeze thawing.
2.2 MTT method for testing cell viability
After taking out the cell supernatant, 200. Mu.L of basal medium and 20. Mu.L of MTT (5 mg/mL) were added again to each well, the mixture was returned to the incubator for further culture for 4 hours, then the liquid in the well was discarded, 150. Mu.L of DMSO was added, and after shaking for 10 minutes, absorbance was measured at 490nm wavelength.
2.3ELISA method for determining TNF-alpha concentration
Taking out the kit and the sample to be tested, placing the kit and the sample to be tested at room temperature for use, and performing test operation strictly according to the instruction of the kit.
2.4 Griess reagent method for measuring concentration of NO
The Griess Reagent I and Griess Reagent II in the kit are taken out 30min before the test, and the kit is used after being placed at room temperature, and the test operation is strictly performed according to the instruction of the kit.
3 results of experiments
MTT assay of cell viability
Table 11 shows the results of MTT assay cell viability of papermulberry fruit oil prepared in example 1
As shown in table 11, each sample had no significant effect on LPS-stimulated macrophage viability.
3.2 ELISA method for determining inhibition of papermulberry fruit oil to TNF-alpha
TABLE 12 inhibition of TNF-alpha by papermulberry seed oil prepared in EXAMPLE 1
As shown in FIG. 2, TNF-. Alpha.concentration was significantly elevated after LPS stimulation (NC) compared to the Blank Control (BC) *** P is less than 0.001), dexamethasone (100 mug/mL) can obviously inhibit the secretion of TNF-alpha ### P < 0.001), indicating that the current stimulation condition is effective; the papermulberry fruit oil with the concentration of 0.05wt% and 0.025wt% has obvious inhibition effect on TNF-alpha secreted by macrophage Raw264.7 cells caused by LPS.
3.3 Griess reagent method for determining inhibition of papermulberry fruit oil on NO
TABLE 13 inhibition of NO by papermulberry seed oil prepared in EXAMPLE 1
As shown in FIG. 3, the concentration of NO was significantly increased after LPS stimulation (NC) compared with the blank control group (BC) *** P is less than 0.001), dexamethasone (100 mug/mL) can obviously inhibit NO secretion ## P is less than 0.01), which indicates that the stimulation condition is effective; the papermulberry fruit oil with the concentration of 0.05wt% has obvious inhibition effect on NO secreted by macrophage Raw264.7 cells caused by LPS.
Test example 3
Example 1 inhibition experiment of Broussonetia papyrifera seed oil on melanin
1. Reagent preparation
1.1 Alpha arbutin: precisely weighing a proper amount of alpha-arbutin reference substance, preparing into 200 mug/mL concentration with RPMI-1640 basic culture medium, and filtering and sterilizing with 0.22 mu m filter membrane for later use.
1.2 Kojic acid: precisely weighing a proper amount of kojic acid reference substance, preparing into a basic culture medium with RPMI-1640, filtering with a 0.22 μm filter membrane, and sterilizing.
1.3 Papermulberry fruit oil: proper amount of papermulberry fruit oil is measured by a pipette, prepared into 10% solution by DMSO, then diluted into 0.1wt% solution by DMEM basic culture, and subjected to gradient dilution.
2. Experimental procedure
2.1MTT method for testing cell viability
Taking logarithmic growth phase cells, and adjusting cell concentration to 3.5X10 5 cell/mL was inoculated in 96-well plates at 200. Mu.L per well at 37℃with 5% CO 2 Culturing in an incubator for 24 hours until the cells adhere to the wall. Preparing samples into a certain concentration by using RPMI-1640 basal medium, respectively setting an experiment group (0.1%, 0.05%,0.025%,0.0125%,0.00625%, 0.003125%), a normal control group and a zeroing group, removing the culture solution, adding the RPMI-1640 basal medium or samples with different concentrations according to the test group, setting 3 compound holes at each concentration, setting 200 mu L of each hole, and placing the mixture back into an incubator for incubation for 24 hours. After 24h, the 96-well plate was removed, 20. Mu.L of MTT (5 mg/mL PBS solution) was added to each well, the culture was continued for 4h, after the completion of the culture, the supernatant was aspirated, 150. Mu.L of DMSO was added to each well, shaking was conducted for 10min under light-shielding conditions, and the absorbance was measured at 490 nm.
The test results are shown in FIG. 4, and FIG. 4 shows the effect of papermulberry seed oil on B16-F10 cell viability. As can be seen from fig. 4: when the concentration of the papermulberry fruit oil is less than or equal to 0.003125%, the cell activity is more than 90%, the papermulberry fruit oil is taken as the maximum safe concentration, and different concentrations are selected within the concentration range of less than or equal to 0.003125% for the next experiment.
2.2 Experiments for melanin inhibition
Taking logarithmic growth phase cells, and adjusting cell concentration to 1x10 5 cell/mL, cells were inoculated into 6-well plates at a volume of 2mL per well, and returned to the incubator for incubation (37 ℃,5% CO) 2 ). Selecting proper concentration as the concentration to be measured of the experimental group sample according to the cell viability test result; experiments were performed using beta-arbutin (200. Mu.g/mL) and kojic acid (100. Mu.g/mL) as positive controls. After 24h, 6-well plates were removed, old medium was discarded, cells were washed with PBS, and then loaded in 3 duplicate wells per concentration per group. Taking out 6-well plate 24 hr after administration, discarding supernatant, washing with PBS for 2 times, adding 500 μl of pancreatin to each well, blowing cells to resuspension after 1min, transferring cell suspension into centrifuge tube, centrifuging at 1000rpm for 10min, discarding supernatant, adding 200 μl of 1mol/L sodium hydroxide solution to each tube, standing in 80deg.C water bath for 1 hr, vortex mixing, taking 150 μl of each well in 96-well plate, and measuring absorbance value (O) at 405nm wavelength with 1mol/L sodium hydroxide solution as blankD）。
Test results: FIG. 5 shows the effect of papermulberry fruit oil on B16-F10 melanin secretion
TABLE 14 Effect of papermulberry fruit oil prepared in example 1 on B16-F10 melanin secretion
Compared with the negative control group (NC), the positive control group (beta-arbutin and kojic acid) treated cells have obviously reduced content of melanin secretion (P is less than 0.01), which indicates that the experimental condition is effective; the content of melanin secreted by 0.0006% of treated cells of the papermulberry fruit oil is obviously reduced (P is less than 0.01), which indicates that the papermulberry fruit oil can play a role in whitening to a certain extent by reducing the synthesis of melanin.
Test example 4
EXAMPLE 1 preparation of Broussonetia papyrifera seed oil secretion inhibition experiment on UVB keratinocyte skin photoaging model
1. Reagent preparation
1.1 Positive control sample (vitamin E): accurately weighing a proper amount of vitamin E reference substance, and preparing into 200 mug/mL concentration with MEM basic culture medium for later use.
1.2 Papermulberry fruit oil: proper amount of papermulberry fruit oil is measured by a pipette, prepared into 10% solution by DMSO, then diluted into 0.03% solution by DMEM basic culture, and subjected to gradient dilution.
2. Experimental procedure
2.1MTT method for testing cell viability
Taking Hacat keratinocyte in logarithmic phase, and adjusting cell concentration to 8×10 4 cell/mL was inoculated in 96-well plates at 200. Mu.L per well at 37℃with 5% CO 2 Culturing in an incubator for 24 hours until the cells adhere to the wall. Preparing samples into a certain concentration by using MEM basal medium, respectively setting an experimental group (0.03%, 0.015%,0.0075%,0.00375%,0.0018755%, 0.0009375%), a normal control group and a zeroing group, removing culture solution, adding the MEM basal medium or samples with different concentrations according to the experimental group, setting 3 compound holes for each concentration, and setting 2 holes for each hole00 μl was returned to the incubator and incubated for 24h. After 24h, the 96-well plate was removed, 20. Mu.L of MTT (5 mg/mL PBS solution) was added to each well, the culture was continued for 4h, after the completion of the culture, the supernatant was aspirated, 150. Mu.L of DMSO was added to each well, shaking was conducted for 10min under dark conditions, and the absorbance was measured at 490 nm.
The results of the experiment are shown in FIG. 6, and FIG. 6 shows the effect of papermulberry fruit oil prepared in example 1 on Hacat cell viability. As shown in fig. 6: the Broussonetia papyrifera seed oil is in the range of 0.001wt% to 0.03wt%, the activity of Hacat cells is more than 90%, and the concentration can be selected in the concentration range of less than or equal to 0.03% for the next experiment.
2.2 ROS detection
Taking logarithmic growth phase cells, and adjusting cell concentration to 1x10 5 cell/mL, cells were inoculated into 24-well plates at a volume of 1mL per well, and returned to the incubator for incubation (37 ℃,5% CO) 2 ). Selecting proper concentration as the concentration to be measured of the experimental group sample according to the cell viability test result; vitamin E (200. Mu.g/mL) was used as a positive control for the experiment. After 24h, the 24-well plate was removed, the cell culture supernatant was aspirated, 200. Mu.L of probe DCFH-DA at 37℃was added to each well and incubated for 30min in a 200w cell incubator after PBS washing, the DCFH-DA solution was discarded, the cells were washed 3 times with PBS, the cells were digested with pancreatin and collected into a 2mL centrifuge tube, centrifuged at 2500rpm for 10min, the supernatant was discarded, 300. Mu.L of the resuspended cells were added to each tube, 200. Mu.L of the resuspended cell suspension was added to a 96-well plate, and the fluorescence intensity was detected by a fluorescent microplate reader (incident light wavelength 525 nm, excitation light wavelength 488 nm). Results analysis, summarizing the ROS fluorescence intensity values for each group, and plotting using GraphPad Prism software, statistical analysis was performed between each group using T-test, # P<0.05 indicates that the difference in music is significant, ## P<0.01 indicates that the difference is significant, ### P<0.001 indicates that the difference is extremely remarkable.
The test results are shown in FIG. 7 and Table 15, wherein FIG. 7 shows the effect of papermulberry fruit oil prepared in example 1 on ROS secretion, and Table 15 shows the effect of papermulberry fruit oil prepared in example 1 on ROS secretion.
TABLE 15 Effect of papermulberry fruit oil prepared in example 1 on ROS secretion
As shown in FIG. 7 and Table 15, the UVB irradiation group (NC) showed an increase in ROS fluorescence intensity as compared to the control BC * P < 0.05), vitamin E (PC) (200. Mu.g/mL) can inhibit ROS expression # P < 0.05), indicating that the experimental conditions are valid; the concentration of the papermulberry fruit oil of 0.003 weight percent has an inhibition effect on ROS secreted by Hacat keratinocytes caused by UVB, and the difference has statistical significance # P＜0.05）。
Test example 5
Example 1 experiments on the moisturizing efficacy of Broussonetia papyrifera seed oil
The test area (area 3 cm. Times.3 cm) was marked with a marker in the forearms of both hands of the subject. Before the test, the test subject is still sitting for 20 minutes in a laboratory with the temperature of 20-22 ℃ and the relative humidity of 40-60%, and can not drink water and beverages. The forearm exposure was placed in a test condition and left relaxed. And testing the basic value of each area, then using a sample in a sample smearing area, using a matrix formula in a blank control area, and randomly distributing the sample smearing area and the blank control area in the left arm calibration area and the right arm calibration area. After using samples 2h, 4h, 6h, test areas were tested. The test period is that the test subjects are in rest state in a laboratory with the temperature of 20-22 ℃ and the relative humidity of 40-60%.
The results are shown in FIG. 8, and FIG. 8 shows the effect of different time periods on the oil-water activity of papermulberry fruit. As can be seen from fig. 8, the skin water activity is significantly increased after the papermulberry fruit oil is smeared compared with the paper mulberry fruit oil before the use, and the skin water tends to be stable after the use for 2 hours, 4 hours and 6 hours, which indicates that the papermulberry fruit oil has a certain moisturizing effect.
Test example 6
Example 4 preparation of the finished Broussonetia papyrifera cream formulated with Broussonetia papyrifera oil test for skin sensitization
1. Anti-sensitization test
20 subjects were selected and the persons participating in the trial were selected according to the subject inclusion criteria.
(1) Sensitizers: weighing a proper amount of histamine reagent, adding deionized water for dissolution, and preparing into a 3% histamine test solution.
(2) Test procedure: the left (right) hand forearm was divided into 3 circular areas of 1.5cm diameter, marked separately, 30 μl of sensitizer was applied to the patch, immediately applied to the marked circular areas, counted for 30min, the patch was torn off, and the transition of skin reaction before and after sensitization was recorded with the grading scale shown in table 1, thereby judging whether or not there was an antiallergic effect.
(3) Anti-sensitization agent: a test substance.
(4) Test procedure: and (3) taking 20 mu L of the anti-allergic agent on a new patch, immediately attaching the patch to the sensitized different areas, starting timing, recording the disappearing time of allergic symptoms (such as itching feeling and tingling feeling), recording the transition of skin reaction before and after sensitization and anti-sensitization by using the grading grade shown in the table 16, and judging whether the patch has the anti-allergic effect.
Table 16 rating scale
As shown in figure 9, the skin has obvious red swelling and itching after the anti-allergic agent is added, but has obvious red swelling eliminating effect after the paper mulberry fruit oil moisturizing cream is smeared.
Although the foregoing embodiments have been described in some, but not all embodiments of the invention, other embodiments may be obtained according to the present embodiments without departing from the scope of the invention.
Claims (9)
1. The application of papermulberry fruit oil in cosmetics is characterized in that the cosmetics comprise one or more of skin photoaging resisting cosmetics, moisturizing cosmetics, whitening cosmetics and anti-inflammatory and anti-allergic cosmetics; the preparation method of the papermulberry fruit oil comprises the following steps:
parching fructus Broussonetiae, and squeezing to obtain fructus Broussonetiae crude oil; the stir-frying temperature is less than or equal to 60 ℃;
heating and mixing the papermulberry fruit crude oil and acid clay, and standing to obtain a mixture; the standing temperature is more than or equal to 60 ℃;
filtering the mixture through a membrane to obtain the papermulberry fruit oil.
2. The use according to claim 1, wherein the membrane filtration comprises performing a first membrane filtration and a second membrane filtration in sequence;
the diameters of the filter membranes used for the first membrane filtration and the second membrane filtration are independently 1-5 mu m, and the pressures of the first membrane filtration and the second membrane filtration are independently 0.02-0.06 MPa.
3. The use according to claim 1, wherein the temperature of the stir-frying is 40-60 ℃.
4. The use according to claim 1, wherein the temperature of rest is 60-80 ℃; the standing time is 20-30 min.
5. The use according to claim 1 or 4, characterized in that the acid clay accounts for 1-4% of the papermulberry fruit crude oil by mass.
6. The use according to claim 1, characterized in that the water content of the papermulberry fruit is 6-8%.
7. The use according to claim 1, characterized in that in the anti-inflammatory and anti-allergic cosmetic, the effective mass percentage of the papermulberry fruit oil is 0.025-10%;
in the whitening cosmetic, the effective mass percentage of the papermulberry fruit oil is 0.0006-5%;
in the skin photoaging resistant cosmetic, the effective mass percentage of the papermulberry fruit oil is 0.003-5%.
8. An anti-inflammatory and anti-sensitization cosmetic comprising papermulberry fruit oil and a cosmetic base; the preparation method of the papermulberry fruit oil comprises the following steps:
parching fructus Broussonetiae, and squeezing to obtain fructus Broussonetiae crude oil; the stir-frying temperature is less than or equal to 60 ℃;
heating and mixing the papermulberry fruit crude oil and acid clay, and standing to obtain a mixture; the standing temperature is more than or equal to 60 ℃;
filtering the mixture through a membrane to obtain the papermulberry fruit oil.
9. The anti-inflammatory and anti-sensitization cosmetic according to claim 8, wherein the cosmetic base comprises cetostearyl alcohol, a non-ionic sugar based emulsifier, vitamin E, caprylic/capric triglyceride, 1, 3-butylene glycol, glycerol, ammonium acryloyldimethyl taurate, water, p-hydroxyacetophenone, and 1,2 hexanediol.
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Non-Patent Citations (1)
| Title |
|---|
| HONGFANG ZHAO等: "Antioxidative and anti-inflammatory properties of Chushizi oil from Fructus Broussonetiae", 《JOURNAL OF MEDICINAL PLANTS RESEARCH》, vol. 5, no. 28, pages 6407 - 6412 * |
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