CN107669613B - A nanometer Margarita extract, its extraction method, and cosmetic containing the same - Google Patents
A nanometer Margarita extract, its extraction method, and cosmetic containing the same Download PDFInfo
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
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Abstract
The invention discloses a nano pearl extract, an extraction method thereof and cosmetics containing the pearl extract, wherein the method comprises the following steps: a. grinding pearl particles to below 100 nanometers to obtain pearl powder; b. b, mixing the pearl powder and the ethanol aqueous solution in the step a in a kettle type reactor, and introducing carbon dioxide gas for reaming; c. b, filtering the solid-liquid mixture obtained after hole expansion treatment in the step b to obtain filtrate and filter residues; d. c, washing and drying the filter residue obtained in the step c to obtain the reaming pearl powder; e. mixing the hole-enlarged pearl powder with an acetic acid-sodium acetate buffer solution, extracting in a kettle type reactor, and centrifuging to obtain a supernatant; f. and d, mixing the supernatant obtained in the step d and the filtrate obtained in the step c, concentrating and drying to obtain the pearl extract. The pearl extract provided by the method contains more effective components, and can improve the performance of the pearl extract and cosmetics.
Description
Technical Field
The invention relates to the technical field of cosmetics, in particular to a pearl extract, an extraction method thereof and a cosmetic containing the pearl extract.
Background
The pearl is an ancient organic gem, which is mainly produced in the bodies of pearl shellfish and nacre shellfish mollusks; the mineral (aragonite) bead containing calcium carbonate generated by endocrine action is formed by gathering a large number of tiny aragonite crystals, and modern science proves that pearls and extracts thereof can be used as raw materials of cosmetics and have various effects.
Chinese patent publication No. CN105168257A discloses a method for producing pearl liquid, pearl ginseng liquid and pearl powder easily absorbed by human body by using Chinese medicinal material pearl powder, belonging to the technical field of pearl liquid production. The method comprises the following steps: preparing pearl powder or pearl layer powder. The pH value is 6.4-6.6 after the materials are dissolved by hydrochloric acid. Diluting, and filtering by using filter paper to obtain the pearl keratin. Fourthly, a plurality of parts of the pearl conchiolin in the step 3 are merged, and citric acid is adopted for hydrolysis. And fifthly, neutralizing to a PH value of 4.4-4.6 to obtain liquor A. Sixthly, continuously neutralizing the solution A to the PH of 8, and precipitating for 3-4 hours. Filtration through filter paper yielded liquid B and residue C. And adding the liquid B into the ingredient formula according to the percentage weight of the predicted volume yield of the product for preparation. Filtering with self-skin filter paper, and removing residue. Filling the liquid and sterilizing. Making into Margarita liquid or Margarita and Ginseng radix liquid product. And drying, crushing and packaging the filter residue C to obtain the calcium citrate supplement. Drying water, pulverizing, and packaging.
Chinese patent publication No. CN1083362A discloses a method for extracting pearl liquid from mother-of-pearl shell of pinctada martensii. Soaking cleaned Concha Margaritifera in acetic acid, softening, mechanically autogenously grinding to obtain pure Margarita laminate, oven drying, pulverizing, grinding, hydrolyzing with sulfuric acid under heating, neutralizing with calcium carbonate or lime milk, vacuum concentrating, decolorizing with active carbon, and removing impurities to obtain Margarita stock solution. According to the patent method, the shells are completely and cleanly stripped, and the recovery rate is up to more than 80%. The prepared pearl oral liquid has no bitter, salty and astringent peculiar smell, has good taste, and is a good medical health product.
The existing pearl extraction method generally adopts a buffer solution containing weak acid to treat calcium carbonate in pearls so as to utilize organic components in the pearls, but the method can lose part of effective components reacted with the weak acid so as to reduce the performance of the pearl extract.
Disclosure of Invention
The invention aims to provide a nano pearl extract, an extraction method thereof and cosmetics containing the pearl extract.
In order to realize the purpose, the invention provides an extraction method of nano pearls, which comprises the following extraction steps:
a. grinding pearl particles to below 100 nanometers to obtain pearl powder;
b. b, mixing the pearl powder obtained in the step a with an ethanol water solution containing 30-50 wt% of ethanol in a kettle type reactor, introducing carbon dioxide gas, keeping the partial pressure (gauge pressure) of the carbon dioxide at 0.3-1.5 MPa, and then carrying out hole expansion treatment at-5-10 ℃ for 1-10 hours;
c. b, filtering the solid-liquid mixture obtained after hole expansion treatment in the step b to obtain filtrate and filter residues;
d. c, washing and drying the filter residue obtained in the step c to obtain the reaming pearl powder;
e. mixing the pearl powder with acetic acid-sodium acetate buffer solution with pH of 2-5, extracting in a kettle-type reactor, and centrifuging to obtain supernatant;
f. and e, mixing the supernatant obtained in the step e and the filtrate obtained in the step c, concentrating and drying to obtain the pearl extract.
Optionally, in the step b, the solid-liquid weight ratio of the pearl powder to the ethanol aqueous solution is 1: (0.3-5), wherein the weight of ethanol in the ethanol water solution is 35-40 wt%, the partial pressure (gauge pressure) of carbon dioxide is 0.5-0.7 MPa, and the temperature of hole expanding treatment is-1-4 ℃.
Optionally, in step d and step f, the drying temperature is 35-60 ℃ and the drying time is 1-12 hours.
Optionally, in step e, the pH of the acetic acid-sodium acetate buffer solution is 3 to 4.
Optionally, in step e, the conditions of the extraction process are as follows: the temperature is 35-60 ℃, the time is 2-48 hours, and the liquid-solid weight ratio of the acetic acid-sodium acetate buffer solution to the pearl powder with enlarged pores is (1-5): 1, the pressure is the autogenous pressure of the kettle reactor.
Optionally, in the step e, the acetic acid-sodium acetate buffer solution contains a dark plum extract, and the dark plum extract accounts for 0.1-1% of the acetic acid-sodium acetate buffer solution by weight.
The invention also provides a nano pearl extract extracted by the method for extracting nano pearls.
The invention also provides a cosmetic containing the nano pearl extract provided by the invention.
Optionally, the cosmetic is at least one selected from the group consisting of face wash, bath lotion, shampoo, lotion, perfume, skin cleanser, makeup remover, essence, stock solution, honey, milk, hair cream, essence cream, face cream, foundation cream, shampoo, concealer, hair treatment cream, essence cream, pre-makeup cream, face powder, toilet powder, loose powder, skin powder, honey powder, foundation, makeup kit, lipstick, hair wax, makeup remover, skin oil, hair oil, and essence oil.
The invention has the following advantages:
the inventor of the invention unexpectedly finds that the treatment of the pearl by using the carbon dioxide under the specific condition can extract partial pearl organic matters in advance, thereby preventing the pearl organic matters from being decomposed in the subsequent extraction of weak acid buffer solution, improving the extraction yield and improving the performance of the pearl extract.
Drawings
FIG. 1 is a schematic flow chart of an embodiment of the extraction method of the present invention.
Detailed Description
The following specific embodiments are provided to illustrate the present invention, but are not intended to limit the scope of the present invention.
As shown in figure 1, the invention provides an extraction method of nano pearls, which comprises the following extraction steps:
a. grinding pearl particles to below 100 nanometers to obtain pearl powder;
b. b, mixing the pearl powder obtained in the step a with an ethanol water solution containing 30-50 wt% of ethanol in a kettle type reactor, introducing carbon dioxide gas, keeping the partial pressure (gauge pressure) of the carbon dioxide at 0.3-1.5 MPa, and then carrying out hole expansion treatment at-5-10 ℃ for 1-10 hours;
c. b, filtering the solid-liquid mixture obtained after hole expansion treatment in the step b to obtain filtrate and filter residues;
d. c, washing and drying the filter residue obtained in the step c to obtain the reaming pearl powder;
e. mixing the pearl powder with acetic acid-sodium acetate buffer solution with pH of 2-5, extracting in a kettle-type reactor, and centrifuging to obtain supernatant;
f. and e, mixing the supernatant obtained in the step e and the filtrate obtained in the step c, concentrating and drying to obtain the pearl extract.
In the present invention, the oxidation of carbon dioxide is usedThe carbon pretreats the pearl powder at a lower temperature and a higher pressure, so that organic matters in partial pearls can be extracted, and the difficulty of subsequent extraction treatment is reduced, and the possible mechanism is as follows: under higher pressure, the carbon dioxide and water react with calcium carbonate in the pearl, and the specific reaction formula is as follows: CaCO3+CO2+H2O＝Ca(HCO3)2And calcium bicarbonate with lower temperature and higher carbon dioxide partial pressure is in a stable dissolved state, so that calcium carbonate in the pearl powder is precipitated in the form of calcium bicarbonate, thus not only realizing the extraction of partial easily-decomposed and easily-extracted substances in the pearl powder, but also forming an organic framework filled with holes in the pearl powder and facilitating the subsequent extraction. Preferably, in the step b, the solid-liquid weight ratio of the pearl powder to the ethanol aqueous solution is 1: (0.3-5), wherein the weight of ethanol in the ethanol water solution is 35-40 wt%, the partial pressure (gauge pressure) of carbon dioxide is 0.5-0.7 MPa, and the temperature of hole expanding treatment is-1-4 ℃.
In the present invention, the drying is preferably carried out at a relatively low temperature for a relatively long time, for example, at a temperature of 35 to 60 ℃ for 1 to 12 hours in the step d and in the step f.
In the invention, the buffer solution of acetic acid and sodium acetate can be further carried out on the pearl organic skeleton, and in the step e, the pH value of the acetic acid-sodium acetate buffer solution is preferably 3-4.
In the invention, the extraction treatment can be performed under conventional conditions, but because the pore-expanding treatment is performed in advance, the extraction treatment conditions are milder, the time is shorter, the extraction efficiency is higher, and in the step e, the conditions of the extraction treatment are preferably as follows: the temperature is 35-60 ℃, the time is 2-48 hours, and the liquid-solid weight ratio of the acetic acid-sodium acetate buffer solution to the pearl powder with enlarged pores is (1-5): 1, the pressure is the autogenous pressure of the kettle reactor.
The inventor of the present invention finds that if the extraction treatment of the dark plum extract and the acetic acid-sodium acetate buffer solution is performed together, the oxidation resistance of the subsequent pearl is favorably improved, and therefore, in step e, the acetic acid-sodium acetate buffer solution preferably contains the dark plum extract, and the dark plum extract may account for 0.1-1% of the weight of the acetic acid-sodium acetate buffer solution.
The invention also provides a nano pearl extract extracted by the method for extracting nano pearls.
The invention also provides a cosmetic containing the nano pearl extract provided by the invention.
The pearl extract of the present invention may be applied to various cosmetics, for example, the cosmetics may be at least one selected from the group consisting of a face wash, a body lotion, a hair lotion, a face lotion, a perfume, a skin cleanser, a makeup remover, a essence, a body lotion, a honey, a milk, a hair cream, a essence cream, a foundation cream, a shampoo, a concealer, a hair treatment cream, an essence cream, a makeup cream, a face powder, a toilet powder, a loose powder, a skin cleanser, a honey powder, a pressed powder, a cosmetic box, a lipstick, a hair wax, a makeup remover oil, a skin oil, a hair cream, and an essence oil. In addition to pearl extracts, other plant extracts may be added to the cosmetic, such as: plants with anti-inflammatory effects such as sword bean, pink bamboo, pseudo-ginseng, platycodon root and the like, plants with allergy prevention such as folium artemisiae argyi, fructus kochiae, scutellaria baicalensis and chrysanthemum, plants with acne treatment such as mango, folium mori and dandelion, antibacterial plants such as garlic, nardostachys and peony, plants with skin firming effects such as peony, shiitake mushroom and perilla, blood activating plants such as angelica and safflower, whitening plants such as pawpaw, asparagus and crispus, moisturizing plants such as fig, radix ophiopogonis and bighead atractylodes rhizome, oral treatment plants such as rose, cortex acanthopanacis and radix zanthoxyli and the like, and other additives with stabilizing, thickening, preservative, antioxidant and the like can be added by a person skilled in the art, and the invention is not repeated.
The following examples further illustrate the invention but are not to be construed as limiting thereof.
The pearls used in the embodiment of the invention are purchased from Yuecui industries, Inc. of Zhu Chi city, Zhejiang province, the dark plum extract is purchased from Xiansaiao biotechnology, Inc., and the other reagents are analytically pure.
The kettle type reactor used in the embodiment of the invention is a 250mL closed reaction kettle, and comprises a kettle body, a polytetrafluoroethylene lining and an upper cover, wherein the upper cover is spirally connected with the kettle body, and the upper cover is provided with a gas injection hole. The heating device is a temperature-controlled oven, and the cooling mode adopts an ice-water mixture for cooling.
The model of the centrifuge is Thermo ScientificTMSorvall ofTMLYNX high speed centrifuge.
The rotary evaporator is a german IKAika rv10 rotary evaporator.
The average particle diameter of the pearl powder is measured by a Malvern laser particle size analyzer.
Example 1
Grinding 15g Margarita particles (diameter of 3-5 mm) in a mortar to below 100 nm (average particle diameter of 76 nm), and adding dropwise anhydrous ethanol for lubrication to obtain Margarita powder.
Putting 10g of pearl powder into a polytetrafluoroethylene lining of a closed reaction kettle body, adding 40g of ethanol aqueous solution containing 42 wt% of ethanol, screwing an upper cover, placing a kettle-type reactor into ice-water mixed liquid, connecting a gas injection hole of the upper cover with a compressed carbon dioxide steel cylinder, controlling the pressure of carbon dioxide to be 0.6MPa, carrying out reaming treatment for 5 hours, releasing pressure, opening the upper cover, taking out a treated solid-liquid mixture for filtering to obtain filtrate and filter residue, cleaning the filter residue with deionized water for three times, and drying in an oven at 50 ℃ for 2 hours to obtain reamed pearl powder for later use.
Putting 6g of pore-enlarged pearl powder into a polytetrafluoroethylene lining of a closed reaction kettle, adding an acetic acid-sodium acetate buffer solution with the temperature of 26gpH being 3.5, screwing a top cover and sealing a gas injection hole, putting the closed reaction kettle into an oven, heating to 50 ℃ at the heating rate of 3 ℃/min, keeping the temperature for 12 hours for extraction treatment, releasing pressure, opening the top cover, taking out an extracted product, putting the extracted product into a centrifuge, centrifuging for 3min at the rotating speed of 1000rpm/min, and pouring out a supernatant.
Mixing the above filtrate and supernatant, placing into rotary evaporator, performing rotary evaporation concentration at 40 deg.C to obtain rotary evaporation product, taking out rotary evaporation product, placing into drying dish, and drying in oven at 40 deg.C for 6 hr to obtain Margarita extract, and recording as product S1.
Example 2
Grinding 15g Margarita particles (diameter of 3-5 mm) in a mortar to below 100 nm (average particle diameter of 78 nm), and adding dropwise anhydrous ethanol for lubrication to obtain Margarita powder.
Putting 10g of pearl powder into a polytetrafluoroethylene lining of a closed reaction kettle body, adding 40g of ethanol aqueous solution containing 42 wt% of ethanol, screwing an upper cover, placing a kettle-type reactor into ice-water mixed liquid, connecting a gas injection hole of the upper cover with a compressed carbon dioxide steel cylinder, controlling the pressure of carbon dioxide to be 0.6MPa, carrying out reaming treatment for 5 hours, releasing pressure, opening the upper cover, taking out a treated solid-liquid mixture for filtering to obtain filtrate and filter residue, cleaning the filter residue with deionized water for three times, and drying in an oven at 50 ℃ for 2 hours to obtain reamed pearl powder for later use.
Putting 6g of pore-enlarged pearl powder into a polytetrafluoroethylene lining of a closed reaction kettle, adding 26gpH acetic acid-sodium acetate buffer solution with the concentration of 3.5 and 0.2g of dark plum extract, screwing an upper cover and sealing a gas injection hole, putting the closed reaction kettle into an oven, heating to 50 ℃ at the heating rate of 3 ℃/min, keeping the temperature for 12 hours for extraction treatment, releasing pressure, opening the upper cover, taking out an extracted product, putting the extracted product into a centrifuge, centrifuging at the rotating speed of 1000rpm/min for 3min, and pouring out supernatant.
Mixing the above filtrate and supernatant, placing into rotary evaporator, performing rotary evaporation concentration at 40 deg.C to obtain rotary evaporation product, taking out rotary evaporation product, placing into drying dish, and drying in oven at 40 deg.C for 6 hr to obtain Margarita extract, and recording as product S2.
Comparative example 1
Grinding 15g Margarita particles (diameter of 3-5 mm) in a mortar to below 100 nm (average particle diameter of 71 nm), and adding dropwise anhydrous ethanol for lubrication to obtain Margarita powder.
Putting 6g of pearl powder into a polytetrafluoroethylene lining of a closed reaction kettle, adding 26g of acetic acid-sodium acetate buffer solution with the pH value of 3.5, screwing an upper cover and sealing a gas injection hole, putting the closed reaction kettle into an oven, heating to 50 ℃ at the heating rate of 3 ℃/min, keeping the temperature for 12 hours for extraction treatment, releasing pressure, opening the upper cover, taking out an extracted product, putting the extracted product into a centrifuge, centrifuging for 3min at the rotating speed of 1000rpm/min, and pouring out a supernatant.
Placing the supernatant into a rotary evaporator, performing rotary evaporation concentration at 40 ℃ to obtain a rotary evaporation product, taking out the rotary evaporation product, placing the rotary evaporation product into a drying dish, and drying in an oven at 40 ℃ for 6 hours to obtain the pearl extract which is recorded as a product D1.
Test example
The moisture absorption rate, moisture retention rate and free radical scavenging rate of the pearl extract products prepared in the above examples and comparative examples are measured by a conventional method in the industry, the specific results are shown in table 1, and the specific test method is as follows:
moisture absorption rate: putting 0.5g of product into a watch glass, putting the watch glass into a dryer which uses saturated ammonium sulfate aqueous solution and saturated potassium carbonate aqueous solution to maintain the relative humidity at 50% for moisture absorption, taking out the watch glass after 24 hours, and weighing the weight of each product, wherein the moisture absorption rate is the ratio of the weight difference of the product before and after moisture absorption to the weight of the product before moisture absorption.
Moisture retention rate: putting 0.5g of product into a watch glass, then sucking 0.04g of deionized water by using a liquid transfer gun, dripping the deionized water into the product, uniformly oscillating, moisturizing in a drier which uses saturated ammonium sulfate aqueous solution and saturated potassium carbonate aqueous solution to maintain the relative humidity to be 15%, taking out after 12 hours, weighing the weight of each product, wherein the moisturizing rate is the weight ratio of the difference between the weight of the product before and after moisturizing to the weight of the product before and after moisturizing, and taking the absolute value.
Radical clearance rate: 10mL of 4mmol/L FeSO4Mixing the solution, 10mL of salicylic acid-ethanol solution with concentration of 6mmol/L and 0.5g of product, dripping 5 drops of hydrogen peroxide, reacting at 25 ℃ for 10 minutes, and measuring the absorption value at 510nm by using deionized water as reference liquid. Free radical scavenging rate (absorbance of no product added-absorbance of no hydrogen peroxide added)/absorbance of no product added.
TABLE 1
| Product numbering | Moisture absorption rate% | Moisture retention rate% | Clearance of free radicals,% |
| S1 | 32 | 79 | 83 |
| S2 | 27 | 73 | 96 |
| D1 | 22 | 52 | 75 |
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. The extraction method of the nano pearls is characterized by comprising the following extraction steps:
a. grinding pearl particles to below 100 nanometers to obtain pearl powder;
b. b, mixing the pearl powder obtained in the step a with an ethanol water solution containing 30-50 wt% of ethanol in a kettle type reactor, introducing carbon dioxide gas, keeping the partial pressure of the carbon dioxide at 0.3-1.5 MPa, and then carrying out hole expansion treatment at-5-10 ℃ for 1-10 hours;
c. b, filtering the solid-liquid mixture obtained after hole expansion treatment in the step b to obtain filtrate and filter residues;
d. c, washing and drying the filter residue obtained in the step c to obtain the reaming pearl powder;
e. mixing the pearl powder with acetic acid-sodium acetate buffer solution with pH of 2-5, extracting in a kettle-type reactor, and centrifuging to obtain supernatant;
f. and e, mixing the supernatant obtained in the step e and the filtrate obtained in the step c, concentrating and drying to obtain the pearl extract.
2. The extraction method according to claim 1, wherein in the step b, the solid-liquid weight ratio of the pearl powder to the ethanol aqueous solution is 1: (0.3-5), wherein the weight of ethanol in the ethanol water solution is 35-40 wt%, the partial pressure of carbon dioxide is 0.5-0.7 MPa, and the temperature of hole expanding treatment is-1-4 ℃.
3. The extraction process according to claim 1, wherein the drying temperature in step d and in step f is 35-60 ℃ for 1-12 hours.
4. The extraction process according to claim 1, wherein in step e, the pH of the acetic acid-sodium acetate buffer solution is 3-4.
5. The extraction method according to claim 1 or 4, wherein in step e, the extraction process conditions are: the temperature is 35-60 ℃, the time is 2-48 hours, and the liquid-solid weight ratio of the acetic acid-sodium acetate buffer solution to the pearl powder with enlarged pores is (1-5): 1, the pressure is the autogenous pressure of the kettle reactor.
6. The extraction method as claimed in claim 1, wherein in step e, the acetate-sodium acetate buffer solution contains mume fructus extract, and the mume fructus extract accounts for 0.1-1% of the acetate-sodium acetate buffer solution.
7. A nano pearl extract extracted by the method for extracting nano pearls according to any one of claims 1 to 6.
8. A cosmetic comprising the pearl extract as set forth in claim 7.
9. The cosmetic according to claim 8, wherein the cosmetic is at least one selected from the group consisting of face washes, body washes, shampoos, lotions, perfumes, makeup removers, essences, liquids, honeys, milks, hair tonics, essence milks, face creams, foundation creams, shampoos, concealers, hair tonics, essences, pre-makeup creams, powders, loose powders, skin cleansers, powders, pressed powders, compacts, lipsticks, pomades, makeup removers, emollient oils, and essential oils.
10. The cosmetic according to claim 9, wherein the lotion is a skin cleansing lotion.
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| CN101288679A (en) * | 2008-05-23 | 2008-10-22 | 海南京润珍珠生物技术股份有限公司 | Dissolving and reducing generation method of nano pearl powder |
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| 淡水珍珠功能成分的水提取工艺;钱俊青等;《氨基酸和生物资源》;20091231;第8页第2.1部分，第9页第3.1部分 * |
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