CN112972331B - Skin care ointment containing litsea cubeba oil and preparation method thereof - Google Patents
Skin care ointment containing litsea cubeba oil and preparation method thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
- A61Q17/005—Antimicrobial preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/005—Preparations for sensitive skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/41—Particular ingredients further characterized by their size
- A61K2800/413—Nanosized, i.e. having sizes below 100 nm
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/59—Mixtures
- A61K2800/592—Mixtures of compounds complementing their respective functions
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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
Abstract
The invention relates to a skin-care ointment containing litsea cubeba oil and a preparation method thereof, and the skin-care ointment contains the following components: litsea cubeba essential oil-nano silver composite bacteriostatic agent, jerusalem artichoke, lithospermum, liquorice, scutellaria baicalensis, borneol and vaseline; the litsea cubeba essential oil-nano silver composite bacteriostatic agent is prepared by reducing silver nitrate with citral which is a main component of the litsea cubeba essential oil, is supplemented with jerusalem artichoke to create a beneficial bacteria growth environment, is prepared into skin care ointment by being matched with traditional Chinese medicine raw materials with mild properties, such as lithospermum, liquorice, scutellaria baicalensis, borneol and the like, for resisting bacteria and diminishing inflammation, can keep long acting, realize multiple effects, ensure the use safety and be suitable for skin-sensitive people such as pregnant women, infants and the like.
Description
Technical Field
The invention relates to a litsea cubeba oil-containing skin-care ointment and a preparation method thereof, belonging to the technical field of cosmetic processing.
Background
Fructus Litseae, Zanthoxylum piperitum, and Alpinia zerumbet belonging to Lauraceae. The litsea cubeba fruit has faint scent, purity and unique flavor, is rich in various trace elements such as selenium, zinc and the like, and is beneficial to human bodies. The fruit, named as Bicubeb, can be used for treating stomach cold pain and schistosomiasis, has the effects of invigorating stomach, dispelling cold and regulating qi, and can be used for treating cold and preventing cold. The litsea cubeba essential oil extracted from litsea cubeba is yellowish, has strong and pleasant lemon flavor, mainly contains active sterilization components such as citral, higher alcohol, organic acid and the like, has broad-spectrum antibacterial effect, has the inhibition effect on germs such as candida, aspergillus flavus and the like in the medical field, has the induction apoptosis and inhibition effect on tumor cells and leucocytes, is clinically used for treating gynecological diseases, and has the characteristics of quick acting and strong effect as a natural organic antibacterial agent.
The annual output of the litsea cubeba oil in China is 2000-2500 tons, the litsea cubeba oil is the largest world production and export country, but crude oil is mostly directly exported, the output value is low, the litsea cubeba oil is great economic loss, and the high-value utilization of the litsea cubeba oil is considered to be the inevitable direction for future development of the litsea cubeba industry.
At present, most litsea cubeba essential oil is mainly used in the daily chemical industry and is rarely used as a main component in the field of medicine as a daily necessity for producing a bactericide, mainly because the litsea cubeba essential oil serving as an organic antibacterial agent has the defects of easy volatilization and instability and is easy to generate drug resistance.
Disclosure of Invention
In order to solve the problems of easy volatilization, instability and easy generation of drug resistance of the litsea cubeba essential oil in the prior art, the invention provides the litsea cubeba oil-containing skin care ointment and the preparation method thereof.
The technical scheme of the invention is as follows:
the invention discloses a litsea cubeba oil-containing skin care ointment which comprises the following raw materials in parts by weight: 15-35 parts of litsea cubeba essential oil-nano silver composite bacteriostatic agent, 10-20 parts of jerusalem artichoke, 10-20 parts of lithospermum, 5-15 parts of liquorice, 5-15 parts of scutellaria baicalensis, 10-20 parts of borneol and 500-800 parts of vaseline.
Further, the litsea cubeba oil-containing skin care ointment comprises the following raw materials in parts by weight: 25 parts of litsea cubeba essential oil-nano silver composite bacteriostatic agent, 15 parts of jerusalem artichoke, 15 parts of lithospermum, 8 parts of liquorice, 8 parts of scutellaria baicalensis, 15 parts of borneol and 600 parts of vaseline.
Further, the preparation method of the litsea cubeba essential oil-nano silver composite bacteriostatic agent comprises the following steps:
a1, peeling and stoning fresh litsea cubeba, crushing and sieving by a 90-mesh sieve, dispersing litsea cubeba powder in distilled water according to the liquid-material ratio of 3:1, and fully stirring to obtain a litsea cubeba suspension;
a2, placing the litsea cubeba suspension in an ultrasonic cleaning machine for ultrasonic leaching, setting the ultrasonic power at 100-110W, the distillation temperature at 75-80 ℃, and the ultrasonic time at 35-50 min;
a3, filtering the litsea cubeba suspension after the ultrasonic leaching under reduced pressure, and evaporating the obtained filtrate by using a rotary evaporator to obtain a litsea cubeba extract;
a4, mixing litsea cubeba extract and propylene glycol according to the ratio of 1:14 to obtain the litsea cubeba essential oil solution.
A5, adding AgNO into the litsea cubeba essential oil solution 3 And (3) adjusting the pH value of the solution to 12-12.5 by using NaOH, adding EDTA (ethylene diamine tetraacetic acid) as a complexing agent, and performing magnetic stirring to react and mix uniformly to obtain the litsea cubeba essential oil-nano silver composite antibacterial agent.
Further, AgNO in the step A5 3 The mass concentration of the solution is 10-15%, and the concentration of NaOH is 0.1-0.2 mol/L.
The invention also discloses a preparation method of the litsea cubeba oil-containing skin care ointment, which comprises the following steps:
s1, crushing jerusalem artichoke, lithospermum, liquorice and scutellaria baicalensis by using a crusher, sieving by using a sieve of 90 meshes, adding distilled water according to the liquid-material ratio of 3:1, fully stirring to obtain a traditional Chinese medicine suspension, preliminarily preparing a traditional Chinese medicine mixed extracting solution by adopting an ultrasonic-assisted distillation method at 50-65 ℃, filtering under reduced pressure, and extracting and recovering by using ethanol to obtain a traditional Chinese medicine concentrated solution;
s2, adding vaseline into a clean pot, and heating to 50 ℃ until the vaseline is completely melted;
s3, adding the litsea cubeba essential oil-nano silver composite antibacterial agent prepared in the steps A1-A5 and the traditional Chinese medicine concentrated solution prepared in the step S1 into vaseline melted in the step S2, continuously heating to 80-90 ℃, and uniformly stirring by using a magnetic stirrer at the stirring speed of 500-550 r/min;
s4, naturally cooling the homogenized mixed solution obtained in the step S3 to 60-70 ℃, slowly scattering ground borneol, and stirring uniformly to obtain the litsea cubeba oil-containing skin care ointment.
Further, in the step S1, the ultrasonic time is 80-90 min, the ultrasonic power is 100-110W, and the distillation time is 2-2.5 h.
The invention has the beneficial effects that:
1. the invention provides a litsea cubeba oil-containing skin care ointment and a preparation method thereof, wherein nano-silver-litsea cubeba essential oil is prepared by the reduction reaction of litsea cubeba essential oil and silver nitrate and is used as a composite antibacterial agent, so that organic-inorganic composite antibacterial is realized; the antibacterial performance of the nano silver prepared by partial reduction of citral in the litsea cubeba essential oil is superior to that of a single silver nitrate aqueous solution or the litsea cubeba essential oil, wherein the effective concentration of the nano silver is nanomolar, silver ions in the silver nitrate solution are micromolar, the nano silver damages cell membranes through the action of peptidoglycan and plasma membranes of cell walls, and then enters the cells together with the citral in the litsea cubeba essential oil to act on cell key enzymes, induce the generation of active oxygen free radicals and damage DNA and the like, and the litsea cubeba essential oil and the nano silver have efficient synergistic effect, so that the antibacterial efficiency is greatly improved, and the skin care effect is realized.
2. The skin care ointment prepared according to the invention can achieve the purposes of long effect and multiple effects at the same time, the diameter of the nano-silver is between 1 and 100nm, and the nano-silver has special chemical, physical and biological functions due to small-size effect, surface effect, quantum effect and the like, so that the nano-silver has enhanced antibacterial ability, is easier to enter pathogens and kill the pathogens compared with common particles, has high stability, realizes long-acting bacteriostasis, and makes up the defect that litsea cubeba essential oil is easier to volatilize and has short action time through compounding; the litsea cubeba essential oil contains citral which has remarkable bacteriostatic activity on escherichia coli, staphylococcus aureus, enterococcus, bacillus cereus, salmonella typhimurium, listeria monocytogenes, proteus and gonococcus, and other components with antibacterial activity such as 6-methyl-5-heptene-2-ketone, linalool and the like, and the types of bacteria which can be killed by nano silver can reach as many as 650, including various microorganisms such as gram positive bacteria, gram negative bacteria, fungi, viruses and the like.
3. The skin-care ointment disclosed by the invention is added with traditional Chinese medicinal materials for compatibility, and the jerusalem artichoke mainly comprises inulin, crude fiber and rich mineral substances, so that the growth of beneficial bacteria is facilitated, and the immunity of a human body is improved; radix Arnebiae contains pigment components, mainly contains fatty acids such as palmitic acid, oleic acid and linoleic acid, and has effects of treating infantile dermatitis, vulval eczema, youth verruca plana and psoriasis; the licorice has anti-inflammatory and anti-allergic effects; the glycyrrhiza extract and glycyrrhizic acid have detoxification effect similar to that of glucuronic acid on certain poisons; the scutellaria baicalensis can be used for treating the infantile baldness, carbuncle, swelling and sore toxicity without generating drug resistance, ensures the skin health of a user and is the preferred choice for people with sensitive skin.
Detailed Description
The invention will be further described with reference to preferred embodiments.
Example 1
A skin care ointment containing litsea cubeba oil comprises the following raw materials in parts by weight: litsea cubeba essential oil-composite antibacterial agent 23 parts, jerusalem artichoke 15 parts, lithospermum 15 parts, liquorice 8 parts, scutellaria baicalensis 8 parts, borneol 15 parts and vaseline 600 parts.
Further, the preparation method of the litsea cubeba essential oil-nano silver composite antibacterial agent comprises the following steps:
a1, peeling and stoning fresh litsea cubeba, soaking in 0.1% NaCl concentrated solution for 0.5h, crushing, sieving with a 90-mesh sieve, dispersing litsea cubeba powder in distilled water according to the liquid-material ratio of 3:1, and fully stirring to obtain a litsea cubeba suspension;
a2, placing the litsea cubeba suspension in an ultrasonic cleaning machine for ultrasonic leaching, setting the ultrasonic power at 100W, the distillation temperature at 75 ℃, and the ultrasonic time at 35 min;
a3, filtering the litsea cubeba suspension after the ultrasonic leaching under reduced pressure, and evaporating the obtained filtrate by using a rotary evaporator to obtain a litsea cubeba extract;
a4, diluting the litsea cubeba extract with propylene glycol according to the proportion of 1:14 to obtain litsea cubeba essential oil solution.
A5, adding 8 parts of AgNO with the mass concentration of 10% into 15 parts of litsea cubeba essential oil 3 Adjusting the pH value of the solution to 12 by using NaOH with the concentration of 0.1mol/L, adding EDTA as a complexing agent, and stirring the solution by magnetic force to react and mix the solution uniformly at the stirring speed of 500r/min to obtain the litsea cubeba essential oil-nano silver composite antibacterial agent;
the preparation method of the skin care ointment containing litsea cubeba oil specifically comprises the following steps:
s1, pulverizing Jerusalem artichoke, radix Arnebiae, Glycyrrhrizae radix, and Scutellariae radix with pulverizer, sieving with 90 mesh sieve, adding distilled water at liquid-to-material ratio of 3:1, stirring to obtain suspension, primarily preparing mixed extractive solution of Chinese medicinal materials by ultrasonic-assisted distillation at 50 deg.C, filtering under reduced pressure, extracting with ethanol, and recovering to obtain concentrated solution of Chinese medicinal materials;
s2, adding vaseline into a clean pot, and heating to 50 ℃ until the vaseline is completely melted;
s3, adding the litsea cubeba essential oil-nano silver composite antibacterial agent prepared in the steps A1-A5 and the traditional Chinese medicine concentrated solution prepared in the step S1 into the vaseline melted in the step S2, continuously heating to 80 ℃, and uniformly stirring by using a magnetic stirrer at the stirring speed of 500 r/min;
s4, cooling the homogeneous mixture obtained in step S3 to 60 deg.C, slowly adding ground Borneolum Syntheticum, and stirring to obtain skin care ointment containing Litsea cubeba oil.
Example 2
A skin care ointment containing litsea cubeba oil comprises the following raw materials in parts by weight: 25 parts of litsea cubeba essential oil-compound antibacterial agent, 20 parts of jerusalem artichoke, 20 parts of lithospermum, 5 parts of liquorice, 5 parts of scutellaria baicalensis, 20 parts of borneol and 500 parts of vaseline.
Further, the preparation method of the litsea cubeba essential oil-nano silver composite antibacterial agent comprises the following steps:
a1, peeling and stoning fresh litsea cubeba, soaking in 0.1% NaCl concentrated solution for 0.5h, crushing, sieving with a 90-mesh sieve, dispersing litsea cubeba powder in distilled water according to the liquid-material ratio of 3:1, and fully stirring to obtain a litsea cubeba suspension;
a2, placing the litsea cubeba suspension in an ultrasonic cleaning machine for ultrasonic leaching, setting the ultrasonic power at 100W, the distillation temperature at 75 ℃ and the ultrasonic time at 35 min;
a3, filtering the litsea cubeba suspension after the ultrasonic leaching under reduced pressure, and evaporating the obtained filtrate by using a rotary evaporator to obtain a litsea cubeba extract;
a4, diluting the litsea cubeba extract with propylene glycol according to the proportion of 1:14 to obtain litsea cubeba essential oil solution.
A5, adding 10 parts of AgNO with the mass concentration of 10% into 15 parts of litsea cubeba essential oil 3 Adjusting the pH value of the solution to 12 by using NaOH with the concentration of 0.1mol/L, adding EDTA as a complexing agent, and stirring the solution by magnetic force to react and mix the solution uniformly at the stirring speed of 500r/min to obtain the litsea cubeba essential oil-nano silver composite antibacterial agent;
the preparation method of the litsea cubeba oil-containing skin care ointment specifically comprises the following steps:
s1, pulverizing Jerusalem artichoke, radix Arnebiae, Glycyrrhrizae radix, and Scutellariae radix with pulverizer, sieving with 90 mesh sieve, adding distilled water at liquid-to-material ratio of 3:1, stirring to obtain suspension, primarily preparing mixed extractive solution of Chinese medicinal materials by ultrasonic-assisted distillation at 50 deg.C, filtering under reduced pressure, extracting with ethanol, and recovering to obtain concentrated solution of Chinese medicinal materials;
s2, adding vaseline into a clean pot, and heating to 50 ℃ until the vaseline is completely melted;
s3, adding the litsea cubeba essential oil-nano silver composite antibacterial agent prepared in the steps A1-A5 and the traditional Chinese medicine concentrated solution prepared in the step S1 into the vaseline melted in the step S2, continuously heating to 80 ℃, and uniformly stirring by using a magnetic stirrer at the stirring speed of 500 r/min;
s4, cooling the homogeneous mixture obtained in step S3 to 60 deg.C, slowly adding ground Borneolum Syntheticum, and stirring to obtain skin care ointment containing Litsea cubeba oil.
Example 3
A skin care ointment containing litsea cubeba oil comprises the following raw materials in parts by weight: 35 parts of litsea cubeba essential oil-composite antibacterial agent, 10 parts of jerusalem artichoke, 10 parts of lithospermum, 15 parts of liquorice, 15 parts of scutellaria baicalensis, 10 parts of borneol and 800 parts of vaseline.
Further, the preparation method of the litsea cubeba essential oil-nano silver composite antibacterial agent comprises the following steps:
a1, peeling and stoning fresh litsea cubeba, soaking in 0.1% NaCl concentrated solution for 0.5h, crushing, sieving with a 90-mesh sieve, dispersing litsea cubeba powder in distilled water according to the liquid-material ratio of 3:1, and fully stirring to obtain a litsea cubeba suspension;
a2, placing the litsea cubeba suspension in an ultrasonic cleaning machine for ultrasonic leaching, setting the ultrasonic power at 100W, the distillation temperature at 75 ℃, and the ultrasonic time at 35 min;
a3, filtering the litsea cubeba suspension after the ultrasonic leaching under reduced pressure, and evaporating the obtained filtrate by using a rotary evaporator to obtain a litsea cubeba extract;
a4, diluting the litsea cubeba extract with propylene glycol according to the proportion of 1:14 to obtain litsea cubeba essential oil solution.
A5, adding 15 parts of AgNO with the mass concentration of 10% into 20 parts of litsea cubeba essential oil 3 Adjusting the pH value of the solution to 12 by using NaOH with the concentration of 0.1mol/L, adding EDTA as a complexing agent, and stirring the solution by magnetic force to react and mix the solution uniformly at the stirring speed of 500r/min to obtain the litsea cubeba essential oil-nano silver composite antibacterial agent;
the preparation method of the skin care ointment containing litsea cubeba oil specifically comprises the following steps:
s1, pulverizing Jerusalem artichoke, radix Arnebiae, Glycyrrhrizae radix, and Scutellariae radix with pulverizer, sieving with 90 mesh sieve, adding distilled water at liquid-to-material ratio of 3:1, stirring to obtain suspension, primarily preparing mixed extractive solution of Chinese medicinal materials by ultrasonic-assisted distillation at 50 deg.C, filtering under reduced pressure, extracting with ethanol, and recovering to obtain concentrated solution of Chinese medicinal materials;
s2, adding vaseline into a clean pot, and heating to 50 ℃ until the vaseline is completely melted;
s3, adding the litsea cubeba essential oil-nano silver composite antibacterial agent prepared in the steps A1-A5 and the traditional Chinese medicine concentrated solution prepared in the step S1 into the vaseline melted in the step S2, continuously heating to 80 ℃, and uniformly stirring by using a magnetic stirrer at the stirring speed of 500 r/min;
s4, cooling the homogeneous mixture obtained in step S3 to 60 deg.C, slowly adding ground Borneolum Syntheticum, and stirring to obtain skin care ointment containing Litsea cubeba oil.
Example 4
A skin care ointment containing litsea cubeba oil comprises the following raw materials in parts by weight: 22 parts of litsea cubeba essential oil-compound antibacterial agent, 15 parts of jerusalem artichoke, 18 parts of lithospermum, 10 parts of liquorice, 10 parts of scutellaria baicalensis, 18 parts of borneol and 700 parts of vaseline.
Further, the preparation method of the litsea cubeba essential oil-nano silver composite antibacterial agent comprises the following steps:
a1, peeling and stoning fresh litsea cubeba, soaking in 0.1% NaCl concentrated solution for 0.5h, crushing, sieving with a 90-mesh sieve, dispersing litsea cubeba powder in distilled water according to the liquid-material ratio of 3:1, and fully stirring to obtain a litsea cubeba suspension;
a2, placing the litsea cubeba suspension in an ultrasonic cleaning machine for ultrasonic leaching, setting the ultrasonic power at 100W, the distillation temperature at 75 ℃, and the ultrasonic time at 35 min;
a3, filtering the litsea cubeba suspension after the ultrasonic leaching under reduced pressure, and evaporating the obtained filtrate by using a rotary evaporator to obtain a litsea cubeba extract;
a4, diluting the litsea cubeba extract with propylene glycol according to the proportion of 1:14 to obtain litsea cubeba essential oil solution.
A5, adding 10 parts of AgNO with the mass concentration of 10% into 12 parts of litsea cubeba essential oil 3 Adjusting the pH value of the solution to 12 by using NaOH with the concentration of 0.1mol/L, adding EDTA as a complexing agent, and stirring the solution by magnetic force to react and mix the solution uniformly at the stirring speed of 500r/min to obtain the litsea cubeba essential oil-nano silver composite antibacterial agent;
the preparation method of the litsea cubeba oil-containing skin care ointment specifically comprises the following steps:
s1, pulverizing Jerusalem artichoke, radix Arnebiae, Glycyrrhrizae radix, and Scutellariae radix with pulverizer, sieving with 90 mesh sieve, adding distilled water at liquid-to-material ratio of 3:1, stirring to obtain suspension, primarily preparing mixed extractive solution of Chinese medicinal materials by ultrasonic-assisted distillation at 50 deg.C, filtering under reduced pressure, extracting with ethanol, and recovering to obtain concentrated solution of Chinese medicinal materials;
s2, adding vaseline into a clean pot, and heating to 50 ℃ until the vaseline is completely melted;
s3, adding the litsea cubeba essential oil-nano silver composite antibacterial agent prepared in the steps A1-A5 and the traditional Chinese medicine concentrated solution prepared in the step S1 into the vaseline melted in the step S2, continuously heating to 80 ℃, and uniformly stirring by using a magnetic stirrer at the stirring speed of 500 r/min;
s4, cooling the homogeneous mixture obtained in step S3 to 60 deg.C, slowly adding ground Borneolum Syntheticum, and stirring to obtain skin care ointment containing Litsea cubeba oil.
The evaluation of the antibacterial efficacy of the skin care ointment containing litsea cubeba oil prepared according to the above embodiments 1 to 4 adopts a perforation method in an antibacterial circle method, and the litsea cubeba oil-nano silver composite antibacterial agent prepared according to the embodiments 1 to 4 is used as an experimental group, and the specific evaluation method is as follows:
(1) the LB solid culture medium is adopted in the experiment, and the preparation method of the culture medium comprises the following steps: accurately weighing 5g of yeast powder, 10g of NaCl, 10g of tryptone and 20g of agar, dissolving in 1000mL of distilled water, adjusting the pH to 7.5 by using a PBS buffer solution, subpackaging in conical flasks, and sterilizing at the high temperature of 121 ℃ for 20 min;
(2) transferring the test bacteria into a corresponding solid culture medium for activation, and culturing in a culture medium at 37 ℃ for 16-24 h; after activation, a small amount of thalli is picked by using an inoculating loop, put into a test tube filled with sterile water, and shaken uniformly to prepare bacterial suspension; counting by adopting the method of SN/T2098-2008 standard, and adjusting the concentration of the bacterial suspension to make the concentration of the bacterial body about 105 CFU/mL;
(3) pouring the bacterial suspension in the step (2) into the agar in the step (1), and shaking to uniformly mix the bacterial suspension and the agar, wherein the volume ratio of the bacterial suspension to the agar is 1: 100;
(4) pouring 20ml of agar mixed with the bacterial liquid obtained in the step (3) into a sterile culture medium with the diameter of 90mm, solidifying to obtain a bacterial-containing flat plate, and punching the flat plate by using a sterile puncher with the diameter of 6 mm;
(5) using a sterile pipette to pipette 200 mu l of the litsea cubeba essential oil-nano silver composite antibacterial agent prepared in the examples 1 to 4, injecting the litsea cubeba essential oil-nano silver composite antibacterial agent into the hole of the flat plate to be punched obtained in the step (4), placing the flat plate into an incubator at 37 ℃ for culturing for 24 hours, measuring the diameter of a surrounding antibacterial ring in the hole (subtracting the aperture of 6mm from the diameter of the obtained ring), observing the antibacterial effect, repeating the experiment for three times for each bacterium, and finally taking an average value; under the above experimental conditions, the same concentration of sodium benzoate was used for comparative experiments, and the experimental results are shown in table 1;
wherein, the diameter of the inhibition zone is more than 20mm, and the inhibition zone is highly sensitive; 10-20 mm, moderate sensitivity; 5-10 mm, low sensitivity.
TABLE 1 results of different antibacterial agents
TABLE 2 antibacterial experiment of antibacterial agent prepared from Litsea cubeba essential oil with different concentrations
TABLE 3 antibacterial experiments with antibacterial agents prepared with silver nitrate in different concentrations
The method provided by the embodiment 1 in the application is utilized to prepare the litsea cubeba oil-containing skin care ointment, wherein the concentration of the litsea cubeba essential oil and the concentration of silver nitrate are continuously adjusted, the antibacterial effect of the prepared litsea cubeba essential oil-nano silver composite antibacterial agent is shown in tables 2 and 3, as can be seen from tables 2 and 3, when the concentration of the litsea cubeba essential oil in the litsea cubeba essential oil-nano silver composite antibacterial agent is 0.2%, the prepared litsea cubeba essential oil-nano silver composite antibacterial agent has the most remarkable antibacterial effect on staphylococcus aureus, escherichia coli, pseudomonas aeruginosa, propionibacterium acnes and candida albicans, and when the concentration of the silver nitrate is 0.25%, the prepared litsea cubeba essential oil-nano silver composite antibacterial agent has the most remarkable antibacterial effect on staphylococcus aureus, escherichia coli, candida coli, pseudomonas aeruginosa, propionibacterium acnes and candida albicans, and meanwhile, as can be seen from the tables, the litsea cubeba essential oil-nano silver composite antibacterial agent prepared by the application has good antibacterial effect on staphylococcus aureus, escherichia coli, pseudomonas aeruginosa, propionibacterium acnes and candida albicans.
Evaluation of skin irritation of skin ointment containing Litsea cubeba oil prepared according to the above example 1 skin irritation/corrosivity test method using the second part toxicology test method in the "cosmetic sanitation Specification" was carried out by the following specific evaluation methods:
skin irritation refers to reversible inflammatory changes that occur locally after the skin is coated with a subject. 4 adult, healthy and skin-intact white female rabbits are selected and bred in a single cage, and are adapted to the environment of an experimental animal room for 3d before the experiment. Before the test, the two sides of the spine of the white female rabbit are cut off, the hair removing range is respectively 2cm multiplied by 3cm, and the smearing area is 2.5cm multiplied by 2.5 cm. 0.5g of the litsea cubeba oil-containing skin care ointment prepared in the embodiment 1-4 is taken and smeared on one side of the skin, vaseline is smeared on the other side of the skin as a control, and the ointment is smeared for 1 time every day and is smeared for 14 days continuously. Shearing hair before each application from the next day, and removing residual test substance with warm water. The results were observed after one hour and scored according to table 4, with the control and test zones treated identically.
And (4) evaluating the results: the average integral per animal per day was calculated according to the following formula, and the skin irritation intensity was determined as shown in Table 5.
TABLE 4 skin irritation response score
Table 5 skin irritation intensity grading
TABLE 6 EXAMPLE 1 repeated skin irritation test results of rabbits with litsea cubeba oil-containing skin care ointment
TABLE 7 EXAMPLES 1-4 repeated skin irritation test results of skin care ointments containing pungent litse fruit oil on rabbits
Skin irritation tests were performed on white female rabbits for a plurality of times by using the skin care ointment containing litsea cubeba oil prepared by the methods provided in examples 1 to 4, and 14d of the test results were recorded as represented by example 1 to obtain table 6, and other examples are the same as those in the above. The results in table 7 show that the integral mean value of each animal in each day in examples 1-4 is less than 0.5, and comparison with table 5 shows that the litsea cubeba oil-containing skin care ointment has no irritation to skin and is suitable for people with sensitive skin, such as pregnant women, infants and the like.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (6)
1. The skin care ointment containing litsea cubeba oil is characterized by comprising the following raw materials in parts by weight: 15-35 parts of litsea cubeba essential oil-nano silver composite bacteriostatic agent, 10-20 parts of jerusalem artichoke, 10-20 parts of lithospermum, 5-15 parts of liquorice, 5-15 parts of scutellaria baicalensis, 10-20 parts of borneol and 500-800 parts of vaseline; the preparation method of the litsea cubeba essential oil-nano silver composite bacteriostatic agent comprises the following steps:
a1, peeling and stoning the fresh litsea cubeba, crushing and sieving by a 90-mesh sieve, dispersing litsea cubeba powder into distilled water according to the liquid-material ratio of 3:1, and fully stirring to obtain a litsea cubeba suspension;
a2, placing the litsea cubeba suspension in an ultrasonic cleaning machine for ultrasonic leaching, setting the ultrasonic power at 100-110W, the distillation temperature at 75-80 ℃, and the ultrasonic time at 35-50 min;
a3, filtering the litsea cubeba suspension after the ultrasonic leaching under reduced pressure, and evaporating the obtained filtrate by using a rotary evaporator to obtain a litsea cubeba extract;
a4, diluting the litsea cubeba extract with propylene glycol according to the proportion of 1:14 to obtain litsea cubeba essential oil solution;
a5, adding AgNO into the litsea cubeba essential oil solution 3 And (3) adjusting the pH value of the solution to 12-12.5 by using NaOH, adding EDTA (ethylene diamine tetraacetic acid) as a complexing agent, and performing magnetic stirring to react and mix uniformly to obtain the litsea cubeba essential oil-nano silver composite antibacterial agent.
2. The skin care ointment containing litsea cubeba oil as claimed in claim 1, which is characterized by comprising the following raw materials in parts by weight: 25 parts of litsea cubeba essential oil-nano silver composite bacteriostatic agent, 15 parts of jerusalem artichoke, 15 parts of lithospermum, 8 parts of liquorice, 8 parts of scutellaria baicalensis, 15 parts of borneol and 600 parts of vaseline.
3. The skin care ointment of claim 1, wherein the fresh litsea cubeba fruit is peeled and denucleated in step A1, and then soaked in 0.1% NaCl solution.
4. The skin care ointment of claim 1 wherein AgNO in step A5 is Litsea cubeba oil 3 The mass concentration of the solution is 10-15%, and the concentration of NaOH is 0.1-0.2 mol/L.
5. The method for preparing the skin care ointment containing litsea cubeba oil according to claim 1, which comprises the following steps:
s1, crushing jerusalem artichoke, lithospermum, liquorice and scutellaria baicalensis by using a crusher, sieving by using a sieve of 90 meshes, adding distilled water according to the liquid-material ratio of 3:1, fully stirring to obtain a traditional Chinese medicine suspension, preliminarily preparing a traditional Chinese medicine mixed extracting solution by adopting an ultrasonic-assisted distillation method at 50-65 ℃, filtering under reduced pressure, and extracting and recovering by using ethanol to obtain a traditional Chinese medicine concentrated solution;
s2, adding vaseline into a clean pot, and heating to 50 ℃ until the vaseline is completely melted;
s3, adding the litsea cubeba essential oil-nano silver composite antibacterial agent prepared in the steps A1-A5 and the traditional Chinese medicine concentrated solution prepared in the step S1 into vaseline melted in the step S2, continuously heating to 80-90 ℃, and uniformly stirring by using a magnetic stirrer at the stirring speed of 500-550 r/min;
s4, naturally cooling the homogenized mixed solution obtained in the step S3 to 60-70 ℃, slowly scattering ground borneol, and stirring uniformly to obtain the litsea cubeba oil-containing skin care ointment.
6. The method for preparing skin care ointment containing litsea cubeba oil as claimed in claim 5, which is characterized in that: in the step S1, the ultrasonic time is 80-90 min, the ultrasonic power is 100-110W, and the distillation time is 2-2.5 h.
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