CN117643560A - Platycladus orientalis extract and preparation method and application thereof - Google Patents
Platycladus orientalis extract and preparation method and application thereof Download PDFInfo
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- CN117643560A CN117643560A CN202311104076.4A CN202311104076A CN117643560A CN 117643560 A CN117643560 A CN 117643560A CN 202311104076 A CN202311104076 A CN 202311104076A CN 117643560 A CN117643560 A CN 117643560A
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- biota
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- nanoemulsion
- arborvitae
- hair
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- 240000002924 Platycladus orientalis Species 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000000605 extraction Methods 0.000 title description 3
- 238000000855 fermentation Methods 0.000 claims abstract description 121
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- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 claims abstract description 70
- 210000004209 hair Anatomy 0.000 claims abstract description 45
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims abstract description 43
- 241000902900 cellular organisms Species 0.000 claims abstract description 37
- 235000012000 cholesterol Nutrition 0.000 claims abstract description 35
- LADGBHLMCUINGV-UHFFFAOYSA-N tricaprin Chemical compound CCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCC)COC(=O)CCCCCCCCC LADGBHLMCUINGV-UHFFFAOYSA-N 0.000 claims abstract description 35
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- 239000002994 raw material Substances 0.000 claims description 16
- 102100026663 All-trans-retinol dehydrogenase [NAD(+)] ADH7 Human genes 0.000 claims description 15
- 108010009384 L-Iditol 2-Dehydrogenase Proteins 0.000 claims description 15
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- Cosmetics (AREA)
Abstract
The invention provides a biota orientalis extract, a preparation method and application thereof. The fermentation broth of the biota extract is matched with cholesterol, caprylic/capric triglyceride, polyglycerol-10 diisostearate and the like to prepare the nanoemulsion. The biota extract fermentation liquor has antibacterial performance, can reduce scalp grease secretion, stabilize full and healthy hair follicles and inhibit alopecia when applied to hair care and shampoo cosmetics. The arborvitae extract fermentation liquor nanoemulsion has smaller nanometer particle size and uniformity, better stability and easier absorption by scalp, further improves the quantity of hair follicles and hair quality, reduces the secretion of scalp grease, reduces alopecia, improves the hair quality, improves the hair diameter, and avoids the whole hair from collapsing and sticking to the scalp.
Description
Technical Field
The invention relates to the field of cosmetics, in particular to a biota orientalis extract and a preparation method and application thereof.
Background
The hair care market of shampooing is long, and the product type speed-up is equal to the whole market of cosmetics. The scale reaches 500 hundred million yuan. The demand for hair loss prevention and hair growth has been expanding in recent years and is significantly higher than other demands. The anti-hair loss hair-growing products become diversified, and the demand for hair growth is changed along with the change of life habits, so that the demand for hair growth is increased by 30% compared with the annual cycle rate, and the demand for hair growth is far beyond the demands for other head care.
At present, a plurality of hair care products are added with plant extract components to improve the anti-hair loss effect of the hair care products, but the plant extract has poor antibacterial property, and the hair care products are required to be additionally added with preservatives and antibacterial agents to generate irritation. And some people have softer hair, and the hair is flat and skin-covered, so that the aesthetic feeling is affected.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a biota orientalis extract and a preparation method and application thereof.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: a method of preparing a biota orientalis extract, the method comprising the steps of:
(1) Crushing arborvitae and arborvitae twig as material;
(2) Extracting the raw material in the step (1) in water at 40-60 ℃ for 30-60 minutes;
(3) Cooling the mixed system obtained in the step (2) to 30-38 ℃, adding sorbitol dehydrogenase, retinol dehydrogenase and phosphite dehydrogenase, and stirring and reacting for 40-90 minutes; the amount of sorbitol dehydrogenase is 5U-10U/L according to the volume measurement of the mixed system; the dosage of retinol dehydrogenase is 3U-8U/L, and the dosage of phosphite dehydrogenase is 5U-10U/L;
(4) Removing solid substances after solid-liquid separation, and collecting liquid phase to obtain fermentation liquor of the biota orientalis extract.
The cacumen Platycladi has rich flavonoid compounds, and mainly contains quercetin, myricetin, rutin, amantadine, quercitrin neocedar, biflavone, hinokiflavone, bai Huangtong, etc. The cacumen Platycladi also contains volatile components such as alpha-pinene, caryophyllene, alpha-caryophyllene, isopuenol, cypress brain, alpha-biotone, and terpineol acetate. The preparation method of the biota orientalis extract takes biota orientalis and biota orientalis leaves as mixed raw materials, after water extraction, the raw materials and the mixed system are subjected to catalytic hydrolysis by sorbitol dehydrogenase, retinol dehydrogenase and phosphite dehydrogenase, the content of quercetin in the biota orientalis extract fermentation liquor is higher, and the biota orientalis extract fermentation liquor has antibacterial performance, and is applied to hair care and hair washing cosmetics without adding an antibacterial agent and a preservative, so that the irritation is reduced.
Preferably, the arborvitae is 50-150 years arborvitae trunk peeled wood.
The fermentation liquor of the biota orientalis extract obtained by the preparation method of the biota orientalis extract has better antibacterial performance.
Preferably, in the step (1), the cacumen biotae is cleaned to remove surface ash and grease, and the cacumen biotae is crushed after removing surface adhesion water; peeling and crushing the biota orientalis wood into particles with the diameter of 0.1-0.5 mm.
Preferably, in the step (1), the weight ratio of the biota orientalis to the biota orientalis is (4-8): 1.
Preferably, in the step (2), the feed liquid ratio of the raw material to water is 100-300 g/L.
The preparation method of the biota orientalis extract has higher extraction rate of biota orientalis extract fermentation liquor.
The invention also provides a biota orientalis extract fermentation broth prepared by the preparation method of any biota orientalis extract.
The invention also provides application of the biota orientalis extract fermentation liquor in hair care products and hair washing products.
The biota extract fermentation liquor can be applied to hair care products and hair washing products, and can reduce scalp grease secretion, stabilize full and healthy hair follicles and inhibit alopecia.
The invention also provides a arborvitae extract fermentation broth nanoemulsion, comprising: the biota extract fermentation broth, deionized water, dipropylene glycol, squalane, cholesterol, caprylic/capric triglyceride, and polyglycerol-10 diisostearate;
the particle size distribution of the arborvitae extract fermentation liquor nanoemulsion is 20-150 nm, the average particle size of the arborvitae extract fermentation liquor nanoemulsion is 20-40 nm, and the PDI of the arborvitae extract fermentation liquor nanoemulsion is 0.15-0.30;
the biota extract fermentation liquor and deionized water are water phase components of the nanoemulsion, and dipropylene glycol, squalane, cholesterol, caprylic/capric triglyceride and polyglycerin-10 diisostearate are oil phase components of the nanoemulsion;
the weight ratio of the water phase component to the oil phase component is 1:1-2;
in the water phase component, the weight ratio of the biota extract fermentation liquor to deionized water is (5-15): 100;
the oil phase comprises 3-10 parts by weight of dipropylene glycol, 10 parts by weight of squalane, 0.5-5 parts by weight of cholesterol, 1-8 parts by weight of caprylic/capric triglyceride and 0.5-2 parts by weight of polyglycerol-10 diisostearate.
The arborvitae extract fermentation broth nanoemulsion has smaller nanometer particle size and uniformity, better stability and easier absorption by scalp, further improves the quantity of hair follicles and hair quality, reduces the secretion of scalp grease, reduces alopecia, improves the hair quality, improves the hair diameter, and avoids the integral collapse of hair to stick to scalp.
Preferably, the weight ratio of the water phase component to the oil phase component is 1:1.2-1.8.
Preferably, the oil phase component comprises 5-8 parts by weight of dipropylene glycol, 10 parts by weight of squalane, 1-3 parts by weight of cholesterol, 2-5 parts by weight of caprylic/capric triglyceride and 0.5-2 parts by weight of polyglycerol-10 diisostearate.
When the content of the components of the arborvitae extract fermentation liquor nanoemulsion accords with the proportion, the arborvitae extract fermentation liquor nanoemulsion has smaller nanometer particle size, and the particle size is more uniform and the stability is better.
Preferably, the preparation method of the arborvitae extract fermentation broth nanoemulsion comprises the following steps of:
(1) Mixing dipropylene glycol, squalane, cholesterol, caprylic acid/capric acid triglyceride, polyglycerol-10 diisostearate and the like according to weight proportion, heating and stirring at 55-65 ℃ for dissolving for 15-30 min to obtain an oil phase;
(2) Uniformly mixing the biota orientalis extract fermentation liquor with deionized water, and heating to 55-65 ℃; as an aqueous phase;
(3) Adding the water phase in the step (2) into the oil phase in the step (1), and carrying out heat preservation and stirring to obtain colostrum;
(4) And (3) carrying out ultrahigh-pressure nano homogenization on the colostrum ultrahigh-pressure nano emulsion, wherein the homogenization pressure is 900-1200 bar, and standing and cooling to obtain the biota orientalis extract fermentation broth nano emulsion.
The invention has the beneficial effects that: the invention provides a biota extract and a preparation method and application thereof. The biota orientalis extract is applied to hair care products and hair washing products, can reduce scalp grease secretion, stabilize full and healthy hair follicles and inhibit alopecia. The arborvitae extract fermentation liquor nanoemulsion has smaller nanometer particle size and uniformity, better stability and easier absorption by scalp, further improves the quantity of hair follicles and hair quality, reduces the secretion of scalp grease, reduces alopecia, improves the hair quality, improves the hair diameter, and avoids the whole hair from collapsing and sticking to the scalp.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the following specific examples.
Example 1
The preparation method of the biota orientalis extract provided by the embodiment of the invention comprises the following steps of:
(1) Crushing arborvitae and arborvitae twig as material;
(2) Extracting the raw materials in the step (1) in water at 50 ℃ for 45 minutes, wherein the feed liquid ratio of the raw materials to the water is 250g/L;
(3) Cooling the mixed system obtained in the step (2) to 37 ℃, adding sorbitol dehydrogenase, retinol dehydrogenase and phosphite dehydrogenase, and stirring and reacting for 50 minutes; the amount of sorbitol dehydrogenase is 8U/L according to the volume measurement of the mixed system; the dosage of retinol dehydrogenase is 5U/L, and the dosage of phosphite dehydrogenase is 8U/L;
(4) Removing solid substances after filtering and solid-liquid separation, collecting liquid phase, centrifuging and layering to remove water phase in the liquid phase, and collecting the fermentation liquor of the biota orientalis extract.
According to the annual ring, the arborvitae wood of the embodiment has the tree age of 60-70 years, another similar cylinder shape is cut along the cross section vertical to the annual ring, the cylinder-shaped arborvitae wood is cut into small blocks, the small blocks are washed by deionized water to remove dust, the surface is dried to remove surface adhesion water, and the small blocks are crushed into particles with the diameter of 0.1-0.5 mm. Washing the picked cacumen Platycladi with water and ethanol at volume ratio of 1:1 to remove ash and grease on the surface, removing water on the surface, and crushing.
Example 2
The preparation method of the biota orientalis extract provided by the embodiment of the invention comprises the following steps of:
(1) Crushing arborvitae and arborvitae twig as material;
(2) Extracting the raw materials in the step (1) in water at 40 ℃ for 45 minutes, wherein the feed liquid ratio of the raw materials to the water is 250g/L;
(3) Cooling the mixed system obtained in the step (2) to 35 ℃, adding sorbitol dehydrogenase, retinol dehydrogenase and phosphite dehydrogenase, and stirring and reacting for 50 minutes; the amount of sorbitol dehydrogenase is 8U/L according to the volume measurement of the mixed system; the dosage of retinol dehydrogenase is 5U/L, and the dosage of phosphite dehydrogenase is 8U/L;
(4) Removing solid substances after filtering and solid-liquid separation, collecting liquid phase, centrifuging and layering to remove water phase in the liquid phase, and collecting the fermentation liquor of the biota orientalis extract.
Example 3
The preparation method of the biota orientalis extract provided by the embodiment of the invention comprises the following steps of:
(1) Crushing arborvitae and arborvitae twig as material;
(2) Extracting the raw materials in the step (1) in water at 50 ℃ for 45 minutes, wherein the feed liquid ratio of the raw materials to the water is 250g/L;
(3) Cooling the mixed system obtained in the step (2) to 35 ℃, adding sorbitol dehydrogenase, retinol dehydrogenase and phosphite dehydrogenase, and stirring and reacting for 50 minutes; the amount of sorbitol dehydrogenase is 10U/L according to the volume measurement of the mixed system; the dosage of retinol dehydrogenase is 3U/L, and the dosage of phosphite dehydrogenase is 5U/L;
(4) Removing solid substances after filtering and solid-liquid separation, collecting liquid phase, centrifuging and layering to remove water phase in the liquid phase, and collecting the fermentation liquor of the biota orientalis extract.
Example 4
The preparation method of the biota orientalis extract provided by the embodiment of the invention comprises the following steps of:
(1) Crushing arborvitae and arborvitae twig as material;
(2) Extracting the raw materials in the step (1) in water at 50 ℃ for 45 minutes, wherein the feed liquid ratio of the raw materials to the water is 250g/L;
(3) Cooling the mixed system obtained in the step (2) to 37 ℃, adding sorbitol dehydrogenase, retinol dehydrogenase and phosphite dehydrogenase, and stirring and reacting for 50 minutes; the amount of sorbitol dehydrogenase is 5U/L according to the volume measurement of the mixed system; the dosage of retinol dehydrogenase is 5U/L, and the dosage of phosphite dehydrogenase is 5U/L;
(4) Removing solid substances after filtering and solid-liquid separation, collecting liquid phase, centrifuging and layering to remove water phase in the liquid phase, and collecting the fermentation liquor of the biota orientalis extract.
Example 5
The preparation method of the biota orientalis extract provided by the embodiment of the invention comprises the following steps of:
(1) Crushing arborvitae and arborvitae twig as material;
(2) Extracting the raw materials in the step (1) in water at 50 ℃ for 45 minutes, wherein the feed liquid ratio of the raw materials to the water is 250g/L;
(3) Cooling the mixed system obtained in the step (2) to 30 ℃, adding sorbitol dehydrogenase, retinol dehydrogenase and phosphite dehydrogenase, and stirring and reacting for 50 minutes; the amount of sorbitol dehydrogenase is 10U/L according to the volume measurement of the mixed system; the dosage of retinol dehydrogenase is 8U/L, and the dosage of phosphite dehydrogenase is 10U/L;
(4) Removing solid substances after filtering and solid-liquid separation, collecting liquid phase, centrifuging and layering to remove water phase in the liquid phase, and collecting the fermentation liquor of the biota orientalis extract.
Example 6
As an embodiment of the present invention, a arborvitae extract fermentation broth nanoemulsion, the nanoemulsion comprising: a biota extract broth, deionized water, dipropylene glycol, squalane, cholesterol, caprylic/capric triglyceride, polyglycerol-10 diisostearate as described in example 1;
the particle size distribution of the arborvitae extract fermentation liquor nanoemulsion is 20-150 nm, the average particle size of the arborvitae extract fermentation liquor nanoemulsion is 20-40 nm, and the PDI of the arborvitae extract fermentation liquor nanoemulsion is 0.15-0.30;
the biota extract fermentation liquor and deionized water are water phase components of the nanoemulsion, and dipropylene glycol, squalane, cholesterol, caprylic/capric triglyceride and polyglycerin-10 diisostearate are oil phase components of the nanoemulsion;
the weight ratio of the water phase component to the oil phase component is 1:1.5;
in the water phase component, the weight ratio of the biota extract fermentation liquor to deionized water is 10:100;
the oil phase comprises, by weight, 5 parts of dipropylene glycol, 10 parts of squalane, 2.5 parts of cholesterol, 3 parts of caprylic/capric triglyceride and 1 part of polyglycerol-10 diisostearate.
The preparation method of the arborvitae extract fermentation broth nanoemulsion comprises the following steps:
(1) Mixing dipropylene glycol, squalane, cholesterol, caprylic acid/capric acid triglyceride, polyglycerol-10 diisostearate, etc. according to weight ratio, heating at 60deg.C, stirring, and dissolving for 20min to obtain oil phase;
(2) Dissolving and dispersing the biota orientalis extract fermentation liquor in deionized water, and heating to 60 ℃; as an aqueous phase;
(3) Adding the water phase in the step (2) into the oil phase in the step (1), and carrying out heat preservation and stirring to obtain colostrum;
(4) And (3) carrying out ultrahigh-pressure nanometer homogenization on the colostrum ultrahigh-pressure nanometer emulsion, wherein the homogenization pressure is 1000bar, homogenizing for 3 times under ultrahigh pressure, and standing and cooling to obtain the biota orientalis extract fermentation broth nanometer emulsion.
Example 7
As an embodiment of the present invention, a arborvitae extract fermentation broth nanoemulsion, the nanoemulsion comprising: a biota extract broth, deionized water, dipropylene glycol, squalane, cholesterol, caprylic/capric triglyceride, polyglycerol-10 diisostearate as described in example 1;
the particle size distribution of the arborvitae extract fermentation liquor nanoemulsion is 20-150 nm, the average particle size of the arborvitae extract fermentation liquor nanoemulsion is 20-40 nm, and the PDI of the arborvitae extract fermentation liquor nanoemulsion is 0.15-0.30;
the biota extract fermentation liquor and deionized water are water phase components of the nanoemulsion, and dipropylene glycol, squalane, cholesterol, caprylic/capric triglyceride and polyglycerin-10 diisostearate are oil phase components of the nanoemulsion;
the weight ratio of the water phase component to the oil phase component is 1:1;
in the water phase component, the weight ratio of the biota extract fermentation liquor to deionized water is 10:100;
the oil phase comprises, by weight, 5 parts of dipropylene glycol, 10 parts of squalane, 2.5 parts of cholesterol, 3 parts of caprylic/capric triglyceride and 1 part of polyglycerol-10 diisostearate.
The preparation method of the arborvitae extract fermentation broth nanoemulsion comprises the following steps:
(1) Mixing dipropylene glycol, squalane, cholesterol, caprylic acid/capric acid triglyceride, polyglycerol-10 diisostearate, etc. according to weight ratio, heating at 60deg.C, stirring, and dissolving for 20min to obtain oil phase;
(2) Dissolving and dispersing the biota orientalis extract fermentation liquor in deionized water, and heating to 60 ℃; as an aqueous phase;
(3) Adding the water phase in the step (2) into the oil phase in the step (1), and carrying out heat preservation and stirring to obtain colostrum;
(4) And (3) carrying out ultrahigh-pressure nanometer homogenization on the colostrum ultrahigh-pressure nanometer emulsion, wherein the homogenization pressure is 1000bar, homogenizing for 3 times under ultrahigh pressure, and standing and cooling to obtain the biota orientalis extract fermentation broth nanometer emulsion.
Example 8
As an embodiment of the present invention, a arborvitae extract fermentation broth nanoemulsion, the nanoemulsion comprising: a biota extract broth, deionized water, dipropylene glycol, squalane, cholesterol, caprylic/capric triglyceride, polyglycerol-10 diisostearate as described in example 1;
the particle size distribution of the arborvitae extract fermentation liquor nanoemulsion is 20-150 nm, the average particle size of the arborvitae extract fermentation liquor nanoemulsion is 20-40 nm, and the PDI of the arborvitae extract fermentation liquor nanoemulsion is 0.15-0.30;
the biota extract fermentation liquor and deionized water are water phase components of the nanoemulsion, and dipropylene glycol, squalane, cholesterol, caprylic/capric triglyceride and polyglycerin-10 diisostearate are oil phase components of the nanoemulsion;
the weight ratio of the water phase component to the oil phase component is 1:1.2;
in the water phase component, the weight ratio of the biota extract fermentation liquor to deionized water is 10:100;
the oil phase comprises, by weight, 5 parts of dipropylene glycol, 10 parts of squalane, 2.5 parts of cholesterol, 3 parts of caprylic/capric triglyceride and 1 part of polyglycerol-10 diisostearate.
The preparation method of the arborvitae extract fermentation broth nanoemulsion comprises the following steps:
(1) Mixing dipropylene glycol, squalane, cholesterol, caprylic acid/capric acid triglyceride, polyglycerol-10 diisostearate, etc. according to weight ratio, heating at 60deg.C, stirring, and dissolving for 20min to obtain oil phase;
(2) Dissolving and dispersing the biota orientalis extract fermentation liquor in deionized water, and heating to 60 ℃; as an aqueous phase;
(3) Adding the water phase in the step (2) into the oil phase in the step (1), and carrying out heat preservation and stirring to obtain colostrum;
(4) And (3) carrying out ultrahigh-pressure nanometer homogenization on the colostrum ultrahigh-pressure nanometer emulsion, wherein the homogenization pressure is 1000bar, homogenizing for 3 times under ultrahigh pressure, and standing and cooling to obtain the biota orientalis extract fermentation broth nanometer emulsion.
Example 9
As an embodiment of the present invention, a arborvitae extract fermentation broth nanoemulsion, the nanoemulsion comprising: a biota extract broth, deionized water, dipropylene glycol, squalane, cholesterol, caprylic/capric triglyceride, polyglycerol-10 diisostearate as described in example 1;
the particle size distribution of the arborvitae extract fermentation liquor nanoemulsion is 20-150 nm, the average particle size of the arborvitae extract fermentation liquor nanoemulsion is 20-40 nm, and the PDI of the arborvitae extract fermentation liquor nanoemulsion is 0.15-0.30;
the biota extract fermentation liquor and deionized water are water phase components of the nanoemulsion, and dipropylene glycol, squalane, cholesterol, caprylic/capric triglyceride and polyglycerin-10 diisostearate are oil phase components of the nanoemulsion;
the weight ratio of the water phase component to the oil phase component is 1:1.8;
in the water phase component, the weight ratio of the biota extract fermentation liquor to deionized water is 10:100;
the oil phase comprises, by weight, 5 parts of dipropylene glycol, 10 parts of squalane, 2.5 parts of cholesterol, 3 parts of caprylic/capric triglyceride and 1 part of polyglycerol-10 diisostearate.
The preparation method of the arborvitae extract fermentation broth nanoemulsion comprises the following steps:
(1) Mixing dipropylene glycol, squalane, cholesterol, caprylic acid/capric acid triglyceride, polyglycerol-10 diisostearate, etc. according to weight ratio, heating at 60deg.C, stirring, and dissolving for 20min to obtain oil phase;
(2) Dissolving and dispersing the biota orientalis extract fermentation liquor in deionized water, and heating to 60 ℃; as an aqueous phase;
(3) Adding the water phase in the step (2) into the oil phase in the step (1), and carrying out heat preservation and stirring to obtain colostrum;
(4) And (3) carrying out ultrahigh-pressure nanometer homogenization on the colostrum ultrahigh-pressure nanometer emulsion, wherein the homogenization pressure is 1000bar, homogenizing for 3 times under ultrahigh pressure, and standing and cooling to obtain the biota orientalis extract fermentation broth nanometer emulsion.
Example 10
As an embodiment of the present invention, a arborvitae extract fermentation broth nanoemulsion, the nanoemulsion comprising: a biota extract broth, deionized water, dipropylene glycol, squalane, cholesterol, caprylic/capric triglyceride, polyglycerol-10 diisostearate as described in example 1;
the particle size distribution of the arborvitae extract fermentation liquor nanoemulsion is 20-150 nm, the average particle size of the arborvitae extract fermentation liquor nanoemulsion is 20-40 nm, and the PDI of the arborvitae extract fermentation liquor nanoemulsion is 0.15-0.30;
the biota extract fermentation liquor and deionized water are water phase components of the nanoemulsion, and dipropylene glycol, squalane, cholesterol, caprylic/capric triglyceride and polyglycerin-10 diisostearate are oil phase components of the nanoemulsion;
the weight ratio of the water phase component to the oil phase component is 1:2;
in the water phase component, the weight ratio of the biota extract fermentation liquor to deionized water is 10:100;
the oil phase comprises, by weight, 5 parts of dipropylene glycol, 10 parts of squalane, 2.5 parts of cholesterol, 3 parts of caprylic/capric triglyceride and 1 part of polyglycerol-10 diisostearate.
The preparation method of the arborvitae extract fermentation broth nanoemulsion comprises the following steps:
(1) Mixing dipropylene glycol, squalane, cholesterol, caprylic acid/capric acid triglyceride, polyglycerol-10 diisostearate, etc. according to weight ratio, heating at 60deg.C, stirring, and dissolving for 20min to obtain oil phase;
(2) Dissolving and dispersing the biota orientalis extract fermentation liquor in deionized water, and heating to 60 ℃; as an aqueous phase;
(3) Adding the water phase in the step (2) into the oil phase in the step (1), and carrying out heat preservation and stirring to obtain colostrum;
(4) And (3) carrying out ultrahigh-pressure nanometer homogenization on the colostrum ultrahigh-pressure nanometer emulsion, wherein the homogenization pressure is 1000bar, homogenizing for 3 times under ultrahigh pressure, and standing and cooling to obtain the biota orientalis extract fermentation broth nanometer emulsion.
Example 11
As an embodiment of the present invention, a arborvitae extract fermentation broth nanoemulsion, the nanoemulsion comprising: a biota extract broth, deionized water, dipropylene glycol, squalane, cholesterol, caprylic/capric triglyceride, polyglycerol-10 diisostearate as described in example 1;
the particle size distribution of the arborvitae extract fermentation liquor nanoemulsion is 20-150 nm, the average particle size of the arborvitae extract fermentation liquor nanoemulsion is 20-40 nm, and the PDI of the arborvitae extract fermentation liquor nanoemulsion is 0.15-0.30;
the biota extract fermentation liquor and deionized water are water phase components of the nanoemulsion, and dipropylene glycol, squalane, cholesterol, caprylic/capric triglyceride and polyglycerin-10 diisostearate are oil phase components of the nanoemulsion;
the weight ratio of the water phase component to the oil phase component is 1:1.5;
in the water phase component, the weight ratio of the biota extract fermentation liquor to deionized water is 10:100;
the oil phase comprises 8 parts by weight of dipropylene glycol, 10 parts by weight of squalane, 1 part by weight of cholesterol, 5 parts by weight of caprylic/capric triglyceride and 1.5 parts by weight of polyglycerol-10 diisostearate.
The preparation method of the arborvitae extract fermentation broth nanoemulsion comprises the following steps:
(1) Mixing dipropylene glycol, squalane, cholesterol, caprylic acid/capric acid triglyceride, polyglycerol-10 diisostearate, etc. according to weight ratio, heating at 60deg.C, stirring, and dissolving for 20min to obtain oil phase;
(2) Dissolving and dispersing the biota orientalis extract fermentation liquor in deionized water, and heating to 60 ℃; as an aqueous phase;
(3) Adding the water phase in the step (2) into the oil phase in the step (1), and carrying out heat preservation and stirring to obtain colostrum;
(4) And (3) carrying out ultrahigh-pressure nanometer homogenization on the colostrum ultrahigh-pressure nanometer emulsion, wherein the homogenization pressure is 1000bar, homogenizing for 3 times under ultrahigh pressure, and standing and cooling to obtain the biota orientalis extract fermentation broth nanometer emulsion.
Comparative example 1
As an emulsion of a biota extract fermentation broth of comparative example 1 of the present invention, the only difference between this comparative example and example 6 is that dipropylene glycol was not added.
Comparative example 2
As an emulsion of a fermentation broth of a Platycladus orientalis extract of comparative example 1 of the present invention, the only difference between this comparative example and example 6 is that squalane was not added.
Experimental method
1. Inhibition of 5-alpha reductase activity
The sample set was added with 300. Mu.L of 1mol/L Tris-HCl buffer solution with pH=7.5, 500. Mu.L of 2 g/L5. Alpha. -reductase solution, 50. Mu.L of 1mmol/L testosterone solution, respectively, the biota extract fermentation broths of examples 1-5, and finally 1mmol/L NADPH 100. Mu.L, and after thoroughly mixing, the reaction was started, the mixed solution was incubated at 37℃for 60min, 1mL of pre-cooled methanol was added to terminate the reaction, and the absorbance A of NADPH of each set was measured at 340 nm. The positive control group replaces the sample extracting solution with 1mg/mL finasteride; the blank group replaces the sample extracting solution with 75% ethanol; the rest of the process is the same.
5 alpha-reductase inhibition ratio (%) = (1- (a positive-a sample)/(a positive-a blank)) ×100% two, antibacterial properties
Dissolving the fermentation liquor of the biota orientalis extract obtained in the test in ethanol, and then injecting the fermentation liquor into a beef extract peptone culture medium to prepare solid culture media with the concentration of the final biota orientalis extract fermentation liquor of 0.01mg/mL to 0.30mg/mL respectively. The bacterial content is about 2×10 9 CFU/ml bacterial suspension, diluted 10 with sterile physiological saline 5 After doubling, 0.10ml of diluted bacteria solution was sucked up and spread on solid medium plates of various concentrated biota extract fermentation broths, respectively, to prepare bacteria-containing solid medium plates, and the bacteria-containing solid medium plates were incubated at 37℃for 24 hours with a normal medium plate containing no biota extract fermentation broth as a blank, and then colony formation was observed, and the minimum biota extract fermentation broth concentration formed by aseptic colony was the minimum inhibitory concentration (MIC/mg/ml) of each biota extract fermentation broth. Staphylococcus aureus and escherichia coli are used as test bacteria.
The experimental results are shown in Table 1
As can be seen from Table 1, the fermentation broth of the biota extract obtained by the preparation method of the biota extract has antibacterial performance, and is applied to hair care and shampoo cosmetics without adding any additional antibacterial agent or preservative, thereby reducing irritation.
3. Particle size and particle size distribution of arborvitae extract fermentation broth nanoemulsion
Particle diameters and particle diameter distributions of the arborvitae extract fermentation broth nanoemulsions of examples 6 to 11 were measured by using a Zetasizer Nano ZS laser particle sizer, 1mL of the arborvitae extract fermentation broth nanoemulsions of examples 6 to 11 and comparative examples 1 to 2 were diluted to 50mL with ultrapure water, 2mL of the nanoemulsion was collected in a sample cell, and the measurement was performed at 25 ℃ by using a laser particle sizer, and the measurement result was a mean value of 3 times of parallel measurement. The experimental results are shown in table 2.
TABLE 2 particle size and particle size distribution of arborvitae extract fermentation broth nanoemulsion
The arborvitae extract fermentation liquor nanoemulsion has smaller nanometer particle size and uniformity, better stability and easier absorption by scalp, and is beneficial to further improving the quantity of hair follicles and hair quality.
4. Alopecia preventing and hair quality improving effects of arborvitae extract fermentation broth nanoemulsion
(one) anti-drop test
1. Volunteer
The proportion of men and women with healthy bodies aged 20-40 years is 1:1, the hair length is about 5-40 cm and does not exceed that of a scapular person; the hair loss is excessive and the hair is slightly sparse, and the hair loss count is more than 10 according to a 60-comb method, and the hair loss count is still more than 10 after 2 weeks of elution; no special hair-dressing treatment such as hair dyeing, hair waving and shaping is performed within 1 month; the test process can be read and understood, and the informed consent can be signed in a written manner; can promise to complete the specified content according to the requirements of the test scheme. Patients with diseases unsuitable for experiments, pregnancy or lactation, etc. cannot be volunteers.
2. Test rule
(1) During the screening and testing period of the subjects, the hair cannot be washed within 48 hours before each visit evaluation, the time of not washing the hair before each visit is basically consistent, and the hair cannot be combed by oneself on the day of the visit; (2) no haircut in 2 before each return visit during the trial evaluation; (3) No hair product was used during the test except for the test and/or control products provided by the test facility; (4) During the test, any hair care and hairdressing treatment measures cannot be performed, and any treatments for preventing alopecia and generating hair cannot be accepted; (5) The original work and rest law is kept during the test, the original good living habit is not changed, and the large emotion fluctuation is avoided.
3. Sample method
(1) 80 volunteers were selected with a ratio of 1:1. Written informed consent was signed, the number of hair loss was counted using a 60 comb method, and recorded. Qualified subjects perform a 2-week washout period, men use the same model of the cleaning shampoo, and women use the same model of the Sha Xuan shampoo; after the 2 weeks of the washing-out period, the hair-combing method is carried out again for 60 times, the hair loss count is still greater than 10, 54 volunteers which meet the conditions are selected, 27 men and women are randomly divided into 9 groups, three men and women in each group are subjected to formal tests.
(2) Subjects enrolled in the formal trial underwent evaluation of hair foundations, including hair loss count, hair diameter, tensile deformation of individual hair fibers, photographs, before use of the product.
(3) The test samples were continuously used for at least 12 weeks in 9 groups of subjects, and the test was performed 4 weeks and 12 weeks after use. The samples to be tested are respectively the arborvitae extract fermentation liquor nanoemulsion of examples 6-11, the arborvitae extract fermentation liquor nanoemulsion of comparative examples 1 and 2, and the blank reference is a mixed solution of the arborvitae extract fermentation liquor and deionized water, wherein the mass ratio of the arborvitae extract fermentation liquor to the deionized water is 2.5:100.
The medicine is used once every two days, the dosage of men is 2mL, and the dosage of women is 5mL.
(4) The subjects were combed with their hair by a trained staff member using a 60-time combing method at each return visit, the number of hair shed was counted, and recorded. The same specification comb must be used throughout the test. Comb: the comb teeth have moderate density (6-7 teeth/cm), the comb can not be replaced in the test process, and high-pressure sterilization is needed after each use.
(II) detection of hairiness
1. Hair diameter detection
The method comprises the steps of taking hair of a subject before using a sample to be tested and after using the sample to be tested for 12 weeks, randomly selecting 10 hairs, measuring the diameter of single hairs by using a laser calliper, and taking the average value of the 10 hairs. The rate of change of hair diameter was calculated for each tester for 12 weeks using the sample to be tested, and the average value of the rate of change of diameter was taken for the same group.
2. 10 hairs are randomly selected from hairs of a subject after 12 weeks of the test sample before the test sample is used, the hairs are fixed in length, the hair fibers with known lengths are stretched at a stretching speed of 1mm/min by a miniature tension tester, and the elongation at break (%) is tested under the conditions of 25 ℃ and relative humidity of 1.5%.
TABLE 3 Experimental results (root) of the amount of alopecia
Sample of | 0 week | 4 weeks of | For 12 weeks |
Example 6 | 16.33 | 9.33 | 4.67 |
Example 7 | 18.67 | 10.5 | 5.33 |
Example 8 | 14.83 | 8.83 | 4.67 |
Example 9 | 21.17 | 12.67 | 5.83 |
Example 10 | 17.5 | 9.17 | 5.17 |
Example 11 | 15.83 | 10.17 | 5.5 |
Comparative example 1 | 19.33 | 15.83 | 10.33 |
Comparative example 2 | 16.83 | 14.67 | 9.83 |
Reference substance | 17.16 | 15.5 | 11.16 |
As shown in Table 3, the arborvitae extract fermentation broth nanoemulsion has smaller nanometer particle size and uniformity, better stability and easier absorption by scalp, further improves the number of hair follicles and hair quality, reduces the secretion of scalp grease, and reduces alopecia.
TABLE 4 improving effect of arborvitae extract fermentation broth nanoemulsion on hair quality
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According to visual observation of the photographed picture, after 12 weeks using the sample of example, the hair of the subject was observed to be more fluffy overall and the phenomenon of sticking to the scalp was remarkably improved. Through detection, as shown in table 4, the arborvitae extract fermentation broth nanoemulsion has smaller nano particle size and uniformity, better stability, easier absorption by scalp, improved hair quality, improved hair diameter and avoided the whole collapse of hair to stick to scalp.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (10)
1. A method for preparing a biota orientalis extract, comprising the steps of:
(1) Crushing arborvitae and arborvitae twig as material;
(2) Extracting the raw material in the step (1) in water at 40-60 ℃ for 30-60 minutes;
(3) Cooling the mixed system obtained in the step (2) to 30-38 ℃, adding sorbitol dehydrogenase, retinol dehydrogenase and phosphite dehydrogenase, and stirring and reacting for 40-90 minutes; the amount of sorbitol dehydrogenase is 5U-10U/L according to the volume measurement of the mixed system; the dosage of retinol dehydrogenase is 3U-8U/L, and the dosage of phosphite dehydrogenase is 5U-10U/L;
(4) Removing solid substances after solid-liquid separation, and collecting liquid phase to obtain fermentation liquor of the biota orientalis extract.
2. The method for producing a biota orientalis extract according to claim 1, wherein the biota orientalis is trunk peeled wood of 50 to 150 years.
3. The method for producing a biota orientalis extract according to claim 1, wherein in the step (1), biota orientalis leaves are washed to remove surface ash and grease, and broken after removing surface-adhering water; peeling and crushing the biota orientalis wood into particles with the diameter of 0.1-0.5 mm.
4. The method of producing a biota orientalis extract according to claim 1, wherein in the step (1), the weight ratio of biota orientalis to biota orientalis is (4-8): 1.
5. The method for producing a biota orientalis extract according to claim 1, wherein in the step (2), the ratio of the raw material to water is 100 to 300g/L.
6. A biota orientalis extract fermentation broth prepared by the method for preparing biota orientalis extract according to any one of claims 1 to 5.
7. The use of the biota orientalis extract fermentation broth according to claim 6 in hair care products and hair wash products.
8. A arborvitae extract fermentation broth nanoemulsion, said nanoemulsion comprising: the biota extract fermentation broth of claim 6, deionized water, dipropylene glycol, squalane, cholesterol, caprylic/capric triglyceride, polyglycerol-10 diisostearate;
the particle size distribution of the arborvitae extract fermentation liquor nanoemulsion is 20-150 nm, the average particle size of the arborvitae extract fermentation liquor nanoemulsion is 20-40 nm, and the PDI of the arborvitae extract fermentation liquor nanoemulsion is 0.15-0.30;
the biota extract fermentation liquor and deionized water are water phase components of the nanoemulsion, and dipropylene glycol, squalane, cholesterol, caprylic/capric triglyceride and polyglycerin-10 diisostearate are oil phase components of the nanoemulsion;
the weight ratio of the water phase component to the oil phase component is 1:1-2;
in the water phase component, the weight ratio of the biota extract fermentation liquor to deionized water is (5-15): 20, a step of;
the oil phase comprises 3-10 parts by weight of dipropylene glycol, 10 parts by weight of squalane, 0.5-5 parts by weight of cholesterol, 1-8 parts by weight of caprylic/capric triglyceride and 0.5-2 parts by weight of polyglycerol-10 diisostearate.
9. The biota extract fermentation broth nanoemulsion of claim 8, wherein the weight ratio of the aqueous phase component to the oil phase component is 1:1.2-1.8;
the oil phase comprises, by weight, 5-8 parts of dipropylene glycol, 10 parts of squalane, 1-3 parts of cholesterol, 2-5 parts of caprylic/capric triglyceride and 0.5-2 parts of polyglycerol-10 diisostearate.
10. The biota orientalis extract fermented liquid nanoemulsion according to claim 8 or 9, wherein the preparation method of the biota orientalis extract fermented liquid nanoemulsion comprises the following steps:
(1) Mixing dipropylene glycol, squalane, cholesterol, caprylic acid/capric acid triglyceride, polyglycerol-10 diisostearate and the like according to weight proportion, heating and stirring at 55-65 ℃ for dissolving for 15-30 min to obtain an oil phase;
(2) Mixing the biota orientalis extract fermentation liquor with deionized water, and heating to 55-65 ℃; as an aqueous phase;
(3) Adding the water phase in the step (2) into the oil phase in the step (1), and carrying out heat preservation and stirring to obtain colostrum;
(4) And (3) carrying out ultrahigh-pressure nano homogenization on the colostrum ultrahigh-pressure nano emulsion, wherein the homogenization pressure is 900-1200 bar, and standing and cooling to obtain the biota orientalis extract fermentation broth nano emulsion.
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