CN112121100B - Itching-relieving and odor-removing chip, puerpera pad and preparation method of puerpera pad - Google Patents

Itching-relieving and odor-removing chip, puerpera pad and preparation method of puerpera pad Download PDF

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CN112121100B
CN112121100B CN202010962205.3A CN202010962205A CN112121100B CN 112121100 B CN112121100 B CN 112121100B CN 202010962205 A CN202010962205 A CN 202010962205A CN 112121100 B CN112121100 B CN 112121100B
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extract
plant
essential oil
itching
odor
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CN112121100A (en
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黄玉琴
裴新梅
邱永龙
何娟娟
龚云
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Qianjin Pharmaceutical Co ltd
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Qianjin Pharmaceutical Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/23Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
    • A61K36/234Cnidium (snowparsley)
    • AHUMAN NECESSITIES
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/045Hydroxy compounds, e.g. alcohols; Salts thereof, e.g. alcoholates
    • AHUMAN NECESSITIES
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K35/00Medicinal preparations containing materials or reaction products thereof with undetermined constitution
    • A61K35/56Materials from animals other than mammals
    • A61K35/63Arthropods
    • A61K35/64Insects, e.g. bees, wasps or fleas
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/48Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
    • A61K36/489Sophora, e.g. necklacepod or mamani
    • AHUMAN NECESSITIES
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    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/65Paeoniaceae (Peony family), e.g. Chinese peony
    • AHUMAN NECESSITIES
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
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    • A61K36/73Rosaceae (Rose family), e.g. strawberry, chokeberry, blackberry, pear or firethorn
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    • A61K9/5026Organic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyvinyl pyrrolidone, poly(meth)acrylates
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    • A61L15/00Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/40Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing ingredients of undetermined constitution or reaction products thereof, e.g. plant or animal extracts
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    • A61L15/16Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/42Use of materials characterised by their function or physical properties
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Abstract

The invention discloses an itching-relieving and odor-removing chip, a puerpera pad and a preparation method thereof. The itching-relieving and odor-removing chip is prepared by mixing the itching-relieving and odor-removing plant essential oil microcapsules, an adhesive and a dispersing agent and then loading the mixture on plant viscose fibers. Wherein the wall material of the plant essential oil microcapsule is octenyl succinate starch, polyvinylpyrrolidone and maltodextrin; the core material is plant essence liquid composed of cnidium oil, perilla leaf oil, gallnut extract, radix sophorae flavescentis extract, almond extract, peony root bark extract, cortex phellodendri extract, menthol and borneol. The plant essence in the chip for relieving itching and removing odor has excellent effects of relieving itching, removing odor and deodorizing, the plant essential oil microcapsules are uniformly distributed on the basis of the surface layer structure of the puerpera pad product, and the coated essential oil is slowly released in the using process to improve the effect durability, so that the product obtains better effect.

Description

Itching-relieving and odor-removing chip, puerpera pad and preparation method of puerpera pad
Technical Field
The invention belongs to the technical field of gynecological products. More particularly, relates to an itching-relieving and odor-removing chip, a puerpera pad and a preparation method thereof.
Background
The female private parts are important organs for metabolic secretion, are relatively complex due to physiological, fertility, sanitary and clean factors and other factors, are influenced by internal and external factors, are susceptible to various germs and cause diseases, not only influence the physical and mental health and the quality of life of the female, but also even cause infertility; meanwhile, private skin is sensitive, various inflammations or simple skin pruritus easily occur, and special nourishing and nursing are needed. With the increase of health consciousness, women have higher requirements for daily care of private parts and prevention and treatment of diseases of private parts.
The common private cleaning products with cleaning efficacy in the market at present can be used for simple cleaning, but cannot solve the problems of peculiar smell, pruritus and the like. For example, in 201610719166.8, the addition of chemical bacteriostatic component is liable to destroy the self-cleaning function of vagina, and may also cause allergy. Therefore, the development of a brand-new product with natural component sources and excellent antibacterial, itching relieving and odor removing effects has important application value.
Pure essential oil components are volatile, and can also volatilize at room temperature or below, so that the stability is poor, the fragrance retention time is short, the quality of the product is influenced, and the application of the essential oil is greatly limited.
Disclosure of Invention
The invention aims to provide the plant essence which has excellent effects of relieving itching and removing odor, has good stability, no layering and no precipitation, and is prepared into an essential oil microcapsule product by utilizing a microencapsulation technology, wherein the essential oil is prevented from volatilizing due to the sealing effect of a high-molecular polymer capsule wall, and the fragrance is completely reserved, so that the storage time of the essential oil is prolonged, and the use stability is improved. The essential oil microcapsule is further prepared into a puerpera pad with the chip with the functions of relieving itching, removing odor and deodorizing, and has very good application value in the aspects of relieving itching, removing odor and deodorizing for puerperas.
The invention aims to provide an itching-relieving and odor-removing chip and a preparation method thereof.
The invention also aims to provide the itching-relieving and odor-removing puerpera pad and the preparation method thereof.
The above purpose of the invention is realized by the following technical scheme:
an antipruritic and deodorant chip is prepared by mixing plant essential oil microcapsule with adhesive and dispersant, and loading onto plant viscose fiber;
wherein the plant essential oil microcapsule comprises the following components:
(1) Wall material: octenyl succinate starch, polyvinylpyrrolidone, maltodextrin;
(2) Core material: plant essence; the plant essence comprises the following components: cnidium fruit oil, perilla leaf oil, chinese gall extract, radix sophorae flavescentis extract, almond extract, peony root bark extract, golden cypress extract, menthol and borneol;
(3) Emulsifier: span-80, tween-80;
(4) Curing agent: glutaraldehyde.
Preferably, the weight ratio of the plant essential oil microcapsules for relieving itching and removing odor to the adhesive to the dispersing agent is 1:0.3 to 0.8:0.3 to 0.8.
More preferably, the weight ratio of the itching-relieving and odor-removing plant essential oil microcapsules, the adhesive and the dispersing agent is 1:0.5:0.5.
as an alternative embodiment, the preparation method of the chip for relieving itching and removing odor comprises the following steps: carrying out two-dipping two-rolling treatment on the mixture of the plant essential oil microcapsules, the binder and the dispersant, wherein the bath ratio is 1:15 to 25 percent, the first soaking is room temperature soaking for 20 to 40 minutes, the rolling residual rate is 80 percent, the second soaking time is 20 minutes, the rolling residual rate is 110 percent, the pre-drying temperature is set to be 60 to 80 ℃, the time is 3 to 5 minutes, and the finished product is ironed.
This step can also be done by means of smearing.
The plant essence in the scheme comprises the following components: cnidium fruit oil, perilla leaf oil, chinese gall extract, radix sophorae flavescentis extract, almond extract, peony root bark extract, golden cypress extract, menthol and borneol. The research shows that the different types of the essential oil and the extract and the different combinations of the antipruritic and deodorizing performances have larger difference, and the research shows that the combined effect of the cnidium fruit oil, the perilla leaf oil, the Chinese gall extract, the sophora flavescens extract, the almond extract, the peony root and bark extract, the phellodendron bark extract, the menthol crystal and the borneol is obviously improved.
Preferably, the mass ratio of the cnidium fruit oil to the total amount of the plant essence is 0.5-2 g/kg, the perilla leaf oil is 0.1-2 g/kg, the Chinese gall extract is 1-5 g/kg, the sophora flavescens extract is 0.01-0.1 g/kg, the almond extract is 0.01-0.1 g/kg, the peony root bark extract is 0.01-0.1 g/kg, the phellodendron bark extract is 0.001-0.01 g/kg, the menthol is 3-6 g/kg, and the borneol is 0.1-0.5 g/kg.
More preferably, the mass ratio of the cnidium fruit oil to the total amount of the plant essence is 0.8-1 g/kg, the perilla leaf oil is 0.5-0.8 g/kg, the Chinese gall extract is 1.5-2 g/kg, the sophora flavescens extract is 0.03-0.06 g/kg, the almond extract is 0.03-0.06 g/kg, the peony root and bark extract is 0.03-0.06 g/kg, the phellodendron bark extract is 0.003-0.006 g/kg, the menthol is 4-5 g/kg, and the borneol is 0.1-0.3 g/kg.
Most preferably, the mass ratio of the cnidium fruit oil to the total amount of the plant essence is 0.9g/kg, the perilla leaf oil is 0.6g/kg, the Chinese gall extract is 1.8g/kg, the radix sophorae flavescentis extract is 0.05g/kg, the almond extract is 0.05g/kg, the peony root bark extract is 0.05g/kg, the phellodendron bark extract is 0.005g/kg, the menthol is 4.5g/kg, and the borneol is 0.2g/kg.
Bedsore is one of the common complications easily caused by long-term bedridden patients, and is caused by tissue ischemia and hypoxia caused by long-term compression of local tissues of a body and blood circulation disturbance, and ulceration and necrosis caused by general malnutrition. Therefore, the traditional Chinese medicine with the effects of clearing away heat and toxic materials, relaxing tendons and activating collaterals, and dispelling wind and removing stasis is selected for preventing pressure sores.
The female menstrual period is in a muggy and humid environment, is easy to breed microorganisms, is infected with gynecological inflammation, and produces pruritus and peculiar smell. The plant essence composition selects the traditional Chinese medicines with the effects of clearing heat and drying dampness to sterilize and relieve itching. Wherein, the cnidium fruit oil can eliminate dampness, dispel wind, kill parasites and relieve itching; perilla leaf oil has effects of promoting qi circulation and dispelling cold; the gallnut extract has the effects of reducing pathogenic fire and eliminating dampness; the sophora flavescens extract can clear heat, dry dampness and kill parasites; the almond extract has the effects of resisting inflammation, relieving pain and the like; the peony root bark has the functions of calming and relaxing muscles; the phellodendron extract has the functions of clearing heat, drying dampness, purging fire and removing toxicity. Modern pharmacological studies show that the phellodendron extract has an inhibiting effect on enterobacteria, staphylococcus aureus, gonococcus and the like, and the gallnut extract has an inhibiting effect on candida albicans.
Further preferably, the solvent is ethanol.
More preferably, the solvent is 60 to 80% ethanol.
Experiments show that the stability of the product can be maintained by diluting with 70% ethanol, borneol can be separated out when the concentration is too low, the components are not easy to dissolve, and the conditions of turbidity and poor stability can occur when the concentration is too high or at the bottom.
Most preferably, therefore, the solvent is 70% ethanol.
Preferably, the preparation method of the plant essence comprises the following steps:
(1) Dissolving Galla chinensis extract in 70% ethanol, and ultrasonic treating to dissolve completely;
(2) Dissolving radix Sophorae Flavescentis extract and cortex Phellodendri extract in 70% ethanol, and ultrasonic treating to dissolve completely;
(3) Dissolving cnidium fruit oil, perilla leaf oil, almond extract and peony root bark extract in 70% ethanol, and mixing;
(4) Dissolving Mentholum and Borneolum Syntheticum in 70% ethanol, and ultrasonic treating to dissolve completely;
(5) And (3) uniformly mixing the solutions obtained in the four steps, and adding 70% ethanol for diluting to a constant volume.
Wherein, preferably, the ultrasonic power is 330W, the frequency is 40Hz, and the time is 10min.
The plant essence liquid product does not generate the layering phenomenon, does not have sediment, and has stable product color. The plant essence liquid product is high in quality and excellent in itching relieving and odor removing effects. Can be applied to parturient cushion in the form of microcapsule. Therefore, the application of the plant essence in preparing the product for relieving itching and removing odor also belongs to the protection scope of the invention.
Specifically, research on an embedding process of plant essential oil microcapsules for relieving itching and removing odor is carried out, and a microcapsule product with a good embedding effect and high stability is obtained.
Namely, the plant essential oil microcapsule for relieving itching and removing odor is prepared from the following materials:
(1) The core material is the plant essence liquid;
(2) The emulsifier is span-80 and tween-80;
(3) The wall materials are octenyl succinate starch, polyvinylpyrrolidone and maltodextrin;
(4) The curing agent is glutaraldehyde.
Wherein the mass ratio of the plant essence, span-80 and tween-80 is 8-12: 1 to 3:1, preferably 8 to 12: 1.5-2: 1, the optimal ratio is 10:2:1. the plant essence is added into span-80, and the tween-80 is mixed according to the mass ratio of 3: distilled water (tween-80: distilled water =3: 10) was added to 10, and then both were mixed uniformly.
The mass ratio of the octenyl succinate starch to the polyvinylpyrrolidone to the maltodextrin is 2-4: 2 to 4:1, and the optimal ratio is 3:3:1.
the addition amount of the glutaraldehyde is 0.1-2% by mass, and the optimal mass ratio of the glutaraldehyde is 1.0%.
As an alternative embodiment, the preparation method of the plant essential oil microcapsule comprises the following steps:
(1) Preparation of plant essential oil emulsion
Adding span-80 (lipophilic emulsifier) into the plant essence, adding Tween-80 (hydrophilic emulsifier) into distilled water, stirring for dissolving, mixing, and shearing and emulsifying with ultrasonic cell pulverizer to obtain plant essential oil emulsion;
(2) Preparation of wall material mixed solution
Weighing octenyl succinate starch, polyvinylpyrrolidone and maltodextrin, adding into deionized water, and stirring at 400rpm for 2-5 min to prepare a wall material mixed solution;
(3) Preparation of core-wall mixed emulsion
Slowly dripping the prepared wall material mixed solution into the prepared plant essential oil emulsion, stirring at 8000rpm for 5-10 min, carrying out complex coacervation reaction, and finally dripping glutaraldehyde to cure for about 60min to prepare the deodorant microcapsule core wall mixed emulsion; the addition amount of glutaraldehyde is 1.0% by mass.
(4) Preparation of microcapsule emulsions
Carrying out colloid milling on the core-wall mixed emulsion prepared in the step (3), and homogenizing for 2-3 times under the pressure of 25-35 mPa to obtain microcapsule emulsion; homogenizing for 3 times at optimal temperature of 30 MPA;
(5) Preparation of microcapsule solid powder
Spray drying the prepared microcapsule emulsion to obtain plant essential oil microcapsule solid powder; the air inlet temperature is 160-200 ℃, and the air outlet temperature is 80-110 ℃. The optimal air inlet temperature is 170-190 ℃, and the air outlet temperature is 90-100 ℃.
In the scheme for preparing the plant essential oil microcapsule product, the wall material is a mixture of octenyl succinate starch, polyvinylpyrrolidone and maltodextrin, so that the plant essential oil microcapsule product has good film forming property and emulsifying property, and the embedding rate is high and reaches 98.0%. The octenyl succinic acid esterified starch HI-CAP100 is prepared by connecting a small amount of hydroxyl in starch with octenyl succinic acid ester group, and after hydrophilic starch is added with lipophilic long-chain alkenyl, the starch has hydrophilic and lipophilic amphoteric properties, and the product has good emulsibility. In the structure of polyvinylpyrrolidone, methylene groups forming a chain and a pyrrolidone ring are nonpolar groups and have lipophilicity, and lactam in a molecule is a strong polar group and has a hydrophilic effect. Polyvinylpyrrolidone is non-toxic and non-irritating to the skin. The octenyl succinate starch and the polyvinylpyrrolidone form a stable amphoteric macromolecular framework, and a certain proportion of micromolecular maltodextrin is added to fill macromolecular crosslinking gaps, so that the emulsion is more stable, and the combination of a water phase, an oil phase and a wall material is firmer, thereby improving the embedding rate of the plant mixed essential oil. The plant mixed essential oil emulsion prepared by compounding the nonionic oleophilic emulsifier span-80 and the hydrophilic emulsifier Tween-80 has good stability.
The plant essential oil microcapsule obtained by the invention has the water content of only 0.7 percent and is convenient to store.
Finally, based on the research result, the invention also provides an itching-relieving and odor-removing puerpera pad which is prepared by placing the itching-relieving and odor-removing chip into the puerpera pad. Can also be applied to sanitary products such as sanitary towels, sanitary pads and the like.
Specifically, as an alternative embodiment, the chip for relieving itching and removing odor is arranged between the wet-strength paper layer and the non-woven fabric layer of the puerpera pad for relieving itching and removing odor.
The invention has the following beneficial effects:
according to the invention, a group of plant essence combinations with excellent itching relieving and odor removing effects are obtained through research, namely the cnidium fruit oil, the perilla leaf oil, the Chinese gall extract, the radix sophorae flavescentis extract, the almond extract, the peony root bark extract, the phellodendron bark extract, the menthol crystal and the borneol, and the product is good in stability, free of layering and turbid precipitation, highly natural in components and high in safety; is suitable for preparing related products and has good application prospect.
Furthermore, the essential oil microcapsule product prepared by the microcapsule technology has the advantages that volatilization of the essential oil is inhibited due to the sealing effect of the capsule wall of the high-molecular polymer, and fragrance is completely reserved, so that the storage time of the essential oil is prolonged, the use stability is improved, and the essential oil microcapsule product has good application value in the aspect of being used as a product capable of relieving itching, removing odor and deodorizing.
Furthermore, the active component extract of the plant mixed essential oil is coated to prepare microcapsules, so that the processing performance of the essential oil is improved, the application range is expanded, and the microcapsules are treated on the surface layer structure of the sanitary towel product by using an after-treatment technology. In the using process, the coated deodorization essential oil is slowly released to improve the deodorization durability, so that the product obtains better effect, the clinical practice is effective, the use is safe, the sensitization and the toxic and side effects do not exist, the preparation method is simple, feasible, scientific and reasonable, and the coated deodorization essential oil is conveniently used for preventing and treating gynecological diseases.
Detailed Description
The present invention is further illustrated by the following specific examples, which are not intended to limit the invention in any way.
Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Unless otherwise indicated, reagents and materials used in the present invention are commercially available.
The following examples are examples in which the main instruments used for the experiments included: MR-96A enzyme-labeling instrument (Shenzhen Meyer biomedical electronics, inc.); RM2235 paraffin slicer, TP1020 full-automatic dehydrator, HI1220 baking machine, HI1210 sheet spreading machine, EG1150H + C tissue embedding machine, DM2000 biological microscope, and DFC420C pathological imaging system (Leica, germany); a ZG-1 gas collection pump, a hydrogen sulfide detection tube and an ammonia gas detection tube (all Shanghai Kuncui instrument Co., ltd.); BSCIIB model 2-1101 Biosafety cabinets (Shanghai Riyan decontamination Equipment, inc.); YXQ-50A type vertical pressure steam sterilizer (Shanghai Bo Xun medical biological instruments, inc.); SPX-250B Biochemical incubator (Tester instruments, inc. of Tianjin).
The statistical method of the experimental data in the examples is as follows: the data are measured as mean + -standard deviation
Figure BDA0002680978430000061
Statistical analysis shows data using SPSS statistical software. The homogeneity of variance was checked by the Leven's test method. If homogeneity of variance (P) is satisfied>0.05 Statistical analysis was performed using One-Way analysis of variance (One-Way ANOVA). ANOVA has statistical significance (P is less than or equal to 0.05), and LSD test (parameter method) is used for comparative analysis. Variance (P is less than or equal to 0.05), then Kruskal-Wallis test is used. The Kruskal-Wallis Test is statistically significant (P.ltoreq.0.05), and a comparative analysis is performed using Dunnett's Test (nonparametric method). P<0.05 was considered statistically significant.
Example 1 plant essence
A plant essence: 9g of cnidium fruit oil, 6g of perilla leaf oil, 18g of Chinese gall extract, 0.5g of radix sophorae flavescentis extract, 0.5g of almond extract, 0.5g of peony root-bark extract, 0.05g of golden cypress extract, 45g of menthol and 2g of borneol.
The preparation method of the plant essence comprises the following steps:
(1) Dissolving Galla chinensis extract in 70% ethanol, and ultrasonic treating to dissolve completely;
(2) Dissolving radix Sophorae Flavescentis extract and cortex Phellodendri extract in 70% ethanol, and ultrasonic treating to dissolve completely;
(3) Dissolving oleum Cnidii, perilla leaf oil, semen Armeniacae amarum extract, and cortex moutan extract in 70% ethanol, and mixing;
(4) Dissolving Mentholum and Borneolum Syntheticum in 70% ethanol, and ultrasonic treating to dissolve completely;
(5) And (3) uniformly mixing the solutions obtained in the four steps, and adding 70% ethanol for dilution until the total weight is 10kg.
Wherein the ultrasonic power is 330W, the frequency is 40Hz, and the time is 10min.
Example 2 plant essence
A plant essence: 10g of cnidium fruit oil, 8g of perilla leaf oil, 20g of Chinese gall extract, 0.6g of radix sophorae flavescentis extract, 0.6g of almond extract, 0.6g of peony root-bark extract, 0.06g of golden cypress extract, 50g of menthol and 3g of borneol.
The preparation method of the plant essence comprises the following steps:
(1) Dissolving Galla chinensis extract in 70% ethanol, and ultrasonic treating to dissolve completely;
(2) Dissolving radix Sophorae Flavescentis extract and cortex Phellodendri extract in 70% ethanol, and ultrasonic treating to dissolve completely;
(3) Dissolving oleum Cnidii, perilla leaf oil, semen Armeniacae amarum extract, and cortex moutan extract in 70% ethanol, and mixing;
(4) Dissolving Mentholum and Borneolum Syntheticum in 70% ethanol, and ultrasonic treating to dissolve completely;
(5) And (3) uniformly mixing the solutions obtained in the four steps, and adding 70% ethanol for dilution until the total weight is 10kg.
Wherein the ultrasonic power is 330W, the frequency is 40Hz, and the time is 10min.
Example 3 plant essence
A plant essence: 8g of cnidium fruit oil, 5g of perilla leaf oil, 15g of Chinese gall extract, 0.3g of radix sophorae flavescentis extract, 0.3g of almond extract, 0.3g of peony root-bark extract, 0.03g of golden cypress extract, 40g of menthol and 1g of borneol.
The preparation method of the plant essence comprises the following steps:
(1) Dissolving Galla chinensis extract in 70% ethanol, and ultrasonic treating to dissolve completely;
(2) Dissolving radix Sophorae Flavescentis extract and cortex Phellodendri extract in 70% ethanol, and ultrasonic treating to dissolve completely;
(3) Dissolving oleum Cnidii, perilla leaf oil, semen Armeniacae amarum extract, and cortex moutan extract in 70% ethanol, and mixing;
(4) Dissolving Mentholum and Borneolum Syntheticum in 70% ethanol, and ultrasonic dissolving;
(5) And (3) uniformly mixing the solutions obtained in the four steps, and adding 70% ethanol for dilution until the total weight is 10kg.
Wherein the ultrasonic power is 330W, the frequency is 40Hz, and the time is 10min.
Example 4 plant essence
A plant essence: 20g of cnidium fruit oil, 20g of perilla leaf oil, 10g of Chinese gall extract, 1g of radix sophorae flavescentis extract, 0.1g of almond extract, 1g of peony root-bark extract, 0.01g of golden cypress extract, 60g of menthol and 1g of borneol.
The preparation method of the plant essence comprises the following steps:
(1) Dissolving Galla chinensis extract in 60% ethanol, and ultrasonic treating to dissolve completely;
(2) Dissolving radix Sophorae Flavescentis extract and cortex Phellodendri extract in 60% ethanol, and ultrasonic treating to dissolve completely;
(3) Dissolving cnidium fruit oil, perilla leaf oil, almond extract and peony root bark extract in 60% ethanol, and mixing;
(4) Dissolving Mentholum and Borneolum Syntheticum in 60% ethanol, and ultrasonic treating to dissolve completely;
(5) And (3) uniformly mixing the solutions obtained in the four steps, and adding 60% ethanol for dilution until the total weight is 10kg.
Wherein the ultrasonic power is 330W, the frequency is 40Hz, and the time is 10min.
Example 5 plant essence
A plant essence: 5g of cnidium fruit oil, 1g of perilla leaf oil, 50g of Chinese gall extract, 0.1g of radix sophorae flavescentis extract, 1g of almond extract, 0.1g of peony root-bark extract, 0.1g of cortex phellodendri extract, 30g of menthol and 5g of borneol.
The preparation method of the plant essence comprises the following steps:
(1) Dissolving Galla chinensis extract in 80% ethanol, and performing ultrasonic treatment to dissolve completely;
(2) Dissolving radix Sophorae Flavescentis extract and cortex Phellodendri extract in 80% ethanol, and ultrasonic treating to dissolve completely;
(3) Dissolving cnidium fruit oil, perilla leaf oil, almond extract and peony root bark extract in 80% ethanol, and mixing;
(4) Dissolving Mentholum and Borneolum Syntheticum in 80% ethanol, and ultrasonic treating to dissolve completely;
(5) And (3) uniformly mixing the solutions obtained in the four steps, and adding 80% ethanol for dilution until the total weight is 10kg.
Wherein the ultrasonic power is 330W, the frequency is 40Hz, and the time is 10min.
Example 6 taste-removing test of plant essence
The experiment shows that the plant essence liquid has the function of removing the odor through the absorption test of the hydrogen sulfide and the ammonia gas. Tea oil is used as a reference substance, and a positive reference medicine is inflammation diminishing and granulation promoting ointment (production unit: fujian Yanshan pharmacy Co., ltd.).
1. Test method
The odor removing effect evaluation test is carried out in a self-made gas preparation test bottle, and hydrogen sulfide and ammonia gas are used as odor removing objects. The hydrogen sulfide is generated by the reaction of iron sulfide powder and hydrochloric acid in a closed conical flask and stored in a wide-mouth flask; ammonia gas is directly added into ammonia water and then evaporated into a wide-mouth bottle for storage. A certain volume of a control (tea oil), a positive control (antiphlogistic granulation promoting ointment) and the essence of example 1-5 are dripped into filter paper, the filter paper is placed in a wide-mouth glass bottle filled with hydrogen sulfide or ammonia gas with determined concentration, the concentration of the hydrogen sulfide or ammonia gas in the wide-mouth glass bottle is detected at different time before and after odor removal, and the odor removal rate is calculated.
2. Detecting the index
Detecting the concentration of hydrogen sulfide and ammonia gas: 100mL of gas in the wide-mouth bottle is collected by a ZG-1 gas collection pump in a sampling manner, and the concentrations of hydrogen sulfide and ammonia gas in the wide-mouth glass bottle before and after smell removal are respectively detected by utilizing hydrogen sulfide and ammonia gas detection tubes so as to calculate the removal rate of the hydrogen sulfide and the ammonia gas. Clearance = (pre-treatment measurement-post-treatment measurement)/pre-treatment measurement x 100%.
3. The test results are shown in Table 1
TABLE 1
Group of Hydrogen sulfide clearance (%) Ammonia gas removal rate (%)
Reference (tea oil) 0 0
Positive control drug (antiphlogistic granulation promoting ointment) 5.9 7.2
Example 1 37.9 21.2
Example 2 36.9 20.8
Example 3 37.1 19.9
Example 4 36.7 20.2
Example 5 36.5 20.7
Example 7 antibacterial test of plant essence
The experiment detects the Minimum Inhibitory Concentration (MIC) of the plant essence on staphylococcus epidermidis, staphylococcus aureus, candida albicans, diphtheroid bacillus and corynebacterium propionicum, and evaluates the antibacterial effect of the plant essence. Tea oil is used as a reference substance, and a positive reference medicine is antiphlogistic granulation promoting ointment (production unit: fujian Yanshan pharmacy Co., ltd.) and penicillin G.
The strain information is as follows:
staphylococcus epidermidis (code CMCC (B) 26069, shanghai lu microtechnique ltd);
staphylococcus aureus (code CMCC (B) 26003, shanghai, ru micro-science ltd);
candida albicans (code CMCC (F) 98001, shanghai Lu Microscience, inc.);
diphtheroid bacilli (accession No. BNCC 138427, north nai bio-technology limited);
corynebacterium propionicum (accession No. BNCC 336443, north Na Biotechnology Ltd.).
1. Test method
MIC values of Staphylococcus epidermidis, staphylococcus aureus, candida albicans, diphtheroid bacillus and Corynebacterium propionicum were determined by continuous 2-fold dilution method.
(1) Pharmaceutical formulation
The preparation and dilution of the drug stock was performed according to the guidelines set forth by the clinical and laboratory standards institute "standards for the performance of antimicrobial drug susceptibility testing (CLSI M100-ED 30). Prepared with dimethyl sulfoxide (DMSO).
(2) Preparation of bacterial suspension
And streaking and inoculating the purified staphylococcus epidermidis and staphylococcus aureus copper on a nutrient agar plate, and culturing for 18-24 h in a constant-temperature incubator at 35 +/-2 ℃. The concentration was made into 0.5M cell suspension using 0.9% sodium chloride injection.
The purified candida albicans is streaked and inoculated on a glucose agar plate of Shashi, and cultured in a constant temperature incubator with the temperature of 35 +/-2 ℃ for 40-48 h. The concentration was made into 0.5M cell suspension using 0.9% sodium chloride injection.
The purified diphtheroid and corynebacterium propionicum are streaked and inoculated on a blood agar plate and cultured in a constant temperature incubator at 35 +/-2 ℃ for 18-24 h. The concentration was made into 0.5M cell suspension using 0.9% sodium chloride injection.
(3) Inoculation of the Strain
10 clean sterile test tubes were each filled with 2.0mL of CAMHB broth (i.e., candida albicans-containing Saccharum sinensis liquid medium, corynebacterium diphtheriae and Corynebacterium acnes propionate-containing CAMHB broth 2.5-5.0% v/v defibrinated sheep blood) as a positive control (no drug added with bacteria) and a negative control (no drug added with bacteria), and the final total volume of each tube was 2.0mL, and a positive control group (antiphlogistic myogenic ointment and penicillin G) and a negative control group (tea oil) were prepared. (Note that the final inoculation bacterial quantity of each tube is 1-5X 10 within 15 minutes after the preparation of the bacterial suspension 5 CFU/ml)。
(4) Incubation culture
After inoculation, culturing the staphylococcus epidermidis and the staphylococcus aureus at the constant temperature of 35 +/-2 ℃ for 16-20 hours; culturing the candida albicans at the constant temperature of 35 +/-2 ℃ for 40-44 h; culturing diphtheroid bacillus at 28 +/-2 deg.c for 20-24 hr; the corynebacterium acnes propionate is cultured for 20-24 h at the constant temperature of 35 +/-2 ℃.
(5) Interpretation of results
The growth of the control group was checked and the data needed for reading were observed with the naked eye or turbidimetric agent. The highest dilution of the drug without bacterial growth is taken as the Minimum Inhibitory Concentration (MIC) of the drug.
2. The test results are shown in Table 2
TABLE 2 Minimum Inhibitory Concentrations (MIC) of the botanical essences at different concentrations against Staphylococcus epidermidis, staphylococcus aureus, candida albicans, diphtheroid diphtheroids, corynebacterium acnes propionate
Figure BDA0002680978430000111
Example 8 anti-itching test of plant essence
1. Incubation period of pruritus
70 mice weighing about 20g were randomly divided into 7 groups of 10 mice each. 12g/kg of Jingfang antipruritic granule (Jingfang antipruritic granule: lizhu group Sichuan Dai pharmaceutical Co., ltd.) was administered to the positive control group, and the same volume (10 ml/kg) of 0.9% sodium chloride solution was administered to the model control group.
1h after administration, the mice were injected with dextran 1.25mg/kg in the tail vein. The head of the mouse was scratched by the front paw, the trunk of the mouse was scratched by the right paw, and the itching indications were obtained by biting the whole body with the mouth. The incubation time of scratching and the number of scratching of the mice within 30min were observed and recorded. Compared with the model blank control group, the mice of the examples 1 to 5 have obviously prolonged pruritus latency time and obviously reduced pruritus times (p is less than 0.01). See table 3.
Table 3 effect of skin itch model in mice of each group (n = 10)
Figure BDA0002680978430000112
Figure BDA0002680978430000121
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Remarking: p was less than 0.01 compared to the blank group.
2. Experiment of histamine phosphate induced skin itch model of guinea pig
70 male guinea pigs weighing about 180g were randomly divided into 7 groups of 10 animals each. The positive control group was administered 6.04g/kg of Jingfang antipruritic granule, and the model control group was administered the same volume (10 ml/kg) of 0.9% sodium chloride solution, examples 1 to 5.
After 24 hours of administration, the skin of the shaved part of the right instep is scratched by abrasive paper (taking the degree of bleeding), histamine phosphate solution (0.01%, 0.02%, 0.03%. 0.2%) is sequentially and incrementally dropped on the wound surface from low concentration to high concentration 10 minutes after application, and the itching concentration value is counted until the guinea pig licks the right foot back, and compared with a model control group and a positive control group, the itching concentration value of the guinea pig caused by histamine phosphate can be improved in examples 1 to 5, which shows that the plant essence liquid has a better antagonistic effect on the itching of the guinea pig caused by histamine phosphate. The results are shown in Table 4.
Table 4 effect of plant essences on values of itch-causing concentration in guinea pigs (n = 10)
Group of Concentration values causing itching
Blank control group 0.081±0.017**
Jingfang antipruritic granule group 0.152±0.042**
Example 1 0.143±0.033**
Example 2 0.163±0.029**
Example 3 0.178±0.015**
Example 4 0.186±0.052**
Example 5 0.193±0.087**
Remarking: p is less than 0.01 compared to blank group.
Example 9 stability testing of plant extracts
1. The physicochemical indexes and the microbial indexes of the essence are shown in table 5, and the detection of all sanitary and sensory physicochemical indexes of the essence prepared by the invention meets the standard requirements.
TABLE 5
Figure BDA0002680978430000131
2. The products of examples 1 to 5 were subjected to stability tests at constant temperature of 50 ℃,4 ℃ and-10 ℃ respectively, and the stability of the products after 1 month, 3 months, 6 months and 12 months was recorded, and the acceptable products were those which did not cause precipitation, odor and discoloration and were free from significant changes in viscosity and pH, and the test results are shown in table 6.
Table 6 stability test results
Figure BDA0002680978430000132
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Figure BDA0002680978430000141
Remarking: wherein √ represents a normal; x represents the change in one or more of odor, color, uniformity, viscosity, pH.
Example 10 Experimental testing of skin irritation of plant essences
1. Skin irritation test
(1) Experimental animals: rabbits, offered by changsha, tianjiu biotechnology limited. The temperature of the animal room is 24-28 ℃, and the relative humidity is 54-60%.
(2) The detection basis is as follows: disinfection Specification 2002 edition 2.3.3.1.
(3) The detection method comprises the following steps:
3 white rabbits, 2 males and 1 female rabbit, the weight of the rabbits is 2.0-2.5 kg, the hair on the two sides of the backs of the rabbits is cut 24 hours before the experiment, the hair removing areas on the left side and the right side are about 3cm multiplied by 3cm, the left side is a medicine coating area, and the right side is a control area. Respectively weighing 0.5ml of the test substance, smearing the test substance on the skin of the medicine application area, covering the test substance with a layer of non-irritating plastic film, fixing the test substance with a non-irritating adhesive tape, and applying the test substance for 24 hours. The control group was coated with an equal amount of distilled water.
After application 24, the application area is rinsed with warm water to remove residue. The local skin reactions were observed at 1h, 24h, and 48h after removal of the test substance, respectively. The experiment was repeated three times and the mean value was taken. The highest skin irritation index is taken, and the level of the skin irritation intensity of the tested substances to the animals is evaluated according to the disinfection technical specification 2002 edition table 2-12.
(4) The results are shown in Table 7: after the administration for 2h, no erythema and edema of the skin can be seen in the drug-coated area of the animal, and no other abnormal phenomena can occur in the animal within the observation period of 48h. The highest skin irritation index is 0, and the skin in the control area has no abnormal phenomenon.
TABLE 7 results of irritation test
Figure BDA0002680978430000151
According to the skin irritation intensity grading standard in the 2002 edition of the disinfection technical Specification, the test result of the acute once complete skin irritation of the washing liquid of the invention to rabbits is as follows: has no irritation, and meets the requirements of disinfection technical Specification 2002 edition 2.3.13.1.
2. Vaginal mucosa irritation test
(1) Experimental animals: rabbits, offered by changsha, tianqin biotechnology limited. The temperature of the animal room is 24-28 ℃, and the relative humidity is 54-60%.
(2) The detection basis is as follows: disinfection Specification 2002 edition 2.3.5.
(3) The detection method comprises the following steps:
experimental animals were randomly divided into a contaminated group (group 1) and a control group (group 2), 3 animals per group, blunt-ended flexible tubes 8cm in length were connected to 2ml syringes, and test solutions were filled for use, one set for each animal.
Fixing the animal on the back, exposing perineum and vaginal orifice, soaking the catheter with the test solution, inserting the catheter into the vagina gently for 4-5 cm, slowly injecting 2ml of the test solution with an injector, and drawing out the catheter to finish the contamination. Control animals were treated with saline as well.
24h after infection, the animals are killed by an air embolism method, the whole vagina is taken out after laparotomy, the longitudinal incision is carried out, and whether congestion, edema and other manifestations exist is observed. Then, the vagina is put into 10% formalin solution for fixation for more than 24h, tissues at two ends and 3 parts in the center of the vagina are selected for flaking, histopathology examination is carried out after HE staining, and the stimulation reaction is scored according to the vaginal mucosa stimulation reaction scoring standard in the 2002 edition 2.3.5 of the disinfection technical Specification.
(4) And (3) detection results:
the animals in the control group and the infected group have no abnormal conditions such as food intake, drinking, defecation and urination, behavioral activities and the like in the later treatment period. After 24 toxicant exposure, the vaginal mucosa is basically intact, and no obvious congestion, edema and other manifestations are seen. The pathological examination result shows that the stimulation index of the vaginal mucosa of the infected group is 0.75. According to the skin irritation intensity grading standard in the 2002 edition of the technical Specification for disinfection, the test result of the irritation test of the lotion on the vaginal mucosa of the rabbit is as follows: has no irritation, and meets the requirements of disinfection technical Specification 2002 edition 2.3.13.1.
Comparative example
1. Taking the plant essence of example 1 as an example, the experimental group was compounded with different combinations of essential oil, as shown in table 8
TABLE 8
Figure BDA0002680978430000161
2. The odor removing effect and stability data of comparative groups 1 to 9 were tested by the methods of examples 1 to 5.
(1) The results of the odor removing effect are shown in table 9 below, and the odor removing effect of the plant essence of the comparative group is significantly inferior to that of the essence of the present invention.
TABLE 9 taste-removing Effect results
Figure BDA0002680978430000162
Figure BDA0002680978430000171
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(2) The results of the bacteriostatic effect are shown in the following table 10, and the bacteriostatic effect of the plant essence of the comparative group is obviously inferior to that of the essence of the invention.
TABLE 10
Figure BDA0002680978430000172
(3) The results of the mouse skin itch model experiments are shown in table 11. Compared with example 1, the mice in the control group have obviously reduced pruritus latency time and obviously increased pruritus frequency.
Table 11 effects of skin itch model in groups of mice (n = 12)
Group of Number of itching (times) Incubation time for pruritus (min)
Blank control group 22.87±5.14** 6.92±4.52**
Jingfang antipruritic granule group 14.91±6.12** 7.58±3.15**
Comparative group 1 15.12±1.12** 12.32±5.02**
Comparative group 2 16.25±3.21** 12.01±4.21**
Comparative group 3 14.28±1.16** 13.26±3.12**
Comparative group 4 16.20±3.25** 12.45±2.03**
Comparative group 5 13.17±1.06** 14.67±2.18**
Comparative group 6 15.28±3.14** 13.26±2.17**
Comparative group 7 12.57±1.26** 15.01±2.22**
Comparative group 8 13.51±2.48** 15.06±1.18**
Comparative group 9 10.28±3.52** 17.22±3.15**
Example 1 5.89±1.17** 10.18±9.16**
Remarking: p was less than 0.01 compared to the blank group.
(4) The stability data are given in table 12 below:
TABLE 12
Figure BDA0002680978430000181
Figure BDA0002680978430000191
Remarking: wherein √ represents a normal; x represents the change in one or more of odor, color, uniformity, viscosity, pH.
Example 11 preparation of plant essence microcapsules
1. Material
(1) Core material: taking the plant essence of example 1 as an example, experiments are carried out;
(2) The wall materials are octenyl succinate starch, polyvinylpyrrolidone and maltodextrin, the emulsifying agents are span-80 and tween-80, and the curing agent is glutaraldehyde.
2. Preparation method
(1) Preparation of plant essence
1) Dissolving Galla chinensis extract in 70% ethanol, and ultrasonic treating to dissolve completely;
2) Dissolving radix Sophorae Flavescentis extract and cortex Phellodendri extract in 70% ethanol, and ultrasonic treating to dissolve completely;
3) Dissolving oleum Cnidii, perilla leaf oil, semen Armeniacae amarum extract, and cortex moutan extract in 70% ethanol, and mixing;
4) Dissolving Mentholum and Borneolum Syntheticum in 70% ethanol, and ultrasonic treating to dissolve completely;
5) And (3) uniformly mixing the solutions obtained in the four steps, and adding 70% ethanol for diluting to a constant volume.
(2) Preparation of plant essential oil emulsion
Adding 60g span-80 (lipophilic emulsifier) into 300g plant essence, adding 30g tween-80 (hydrophilic emulsifier) into 100g distilled water, stirring for dissolving, mixing, and shearing and emulsifying with ultrasonic cell pulverizer to obtain plant essential oil emulsion.
Wherein, the working conditions of the ultrasonic cell crusher are as follows: working time 2s, interval time 3s, working frequency 300W and emulsification 200 times.
(3) Preparation of wall material mixed solution
Weighing 64.5g of octenyl succinic acid esterified starch, 64.5g of polyvinylpyrrolidone and 21.5g of maltodextrin, adding into 150g of deionized water, and stirring at the rotating speed of 400rpm for 2-5 min to prepare a wall material mixed solution;
(4) Preparation of core-wall mixed emulsion
Slowly dripping the prepared wall material mixed solution into the prepared plant essential oil emulsion, stirring at 8000rpm for 5-10 min, carrying out complex coacervation reaction, and finally dripping glutaraldehyde to cure for about 60min to obtain the deodorant microcapsule core wall mixed emulsion. The addition amount of glutaraldehyde was 1.0% by mass.
(5) Preparation of microcapsule emulsions
And (5) carrying out colloid milling on the core-wall mixed emulsion prepared in the step (4), and homogenizing for 3 times under the pressure of 30MPA to obtain the microcapsule emulsion.
(6) Preparation of microcapsule solid powder
And (4) carrying out spray drying on the prepared microcapsule emulsion to obtain the plant essence microcapsule solid powder.
Spray drying conditions: the air inlet temperature is 180 ℃, and the air outlet temperature is 100 ℃.
Example 12 examination of embedding effect and particle size of plant essence microcapsules
1. Investigating the influence of emulsifiers on the stability of plant essential oil emulsions
Respectively using span-80 and tween-80 in different mass ratios to prepare the plant essential oil emulsion, calculating the hydrophilic-lipophilic balance value HLB of the plant essential oil compound emulsifier in different mass ratios according to a formula, and then observing the stability of the emulsion to determine the optimal HLB value.
Wherein the stability is divided into standing stability and centrifugal stability, namely, whether the emulsion is layered or not is observed under the conditions of standing for a day and a night and centrifugation for 5min at the rotation speed of a centrifugal machine of 4000 r/min.
The formula for calculating the mixed HLB value of the compound emulsifier is as follows:
HLBa,b=HLBa×A%+HLBb×B%
in the above formula: HLBa, b — HLB value of mixed emulsifier; HLBa-the HLB value of emulsifier a; HLBb — HLB value of emulsifier b; a% -the mass fraction thereof in the mixture; b% -the mass fraction thereof in the mixture.
TABLE 13 influence of the mass ratio of emulsifiers on the emulsion stability
Span-80: tween-80 1:2 1:1.5 1:1 1.5:1 2:1 2.5:1
Mixed HLB value 11.5 10.7 9.6 8.6 7.9 7.4
Stability of standing Not layering Without delamination Not layering Not layering Without delamination Not layering
Centrifugal stability Layering Layering Not layering Without delamination Not layering Slightly delaminated
As a result, as shown in Table 13, when the HLB value of the mixture was less than 7.9, the emulsion was free from the phenomenon of separation after standing for one day and night, and had good stability and oil droplets on the surface after centrifugation; when the HLB value is more than 9.6, the emulsion has no layering phenomenon after standing for a day and a night, the emulsion has layering of different degrees after centrifugation, and the centrifugal stability is increasingly poor along with the increase of the HLB value: when the HLB value is 7.9-9.6, no layering phenomenon occurs in the emulsion after standing and centrifugation, so the HLB value of the plant mixed essential oil is determined to be 7.9-9.6, and the stability of the essential oil emulsion is optimal, namely span-80: the mass ratio of the tween-80 is 1-2: 1, the stability is the best.
2. Investigating the embedding effect of the microcapsule and the particle diameter of the microcapsule
(1) Determination of encapsulation efficiency of microcapsules
And (3) measuring microcapsule surface oil: accurately weighing 2g of sample (accurately to 0.001 g) m to a triangular flask m1 with constant weight, adding 15mL of petroleum ether (boiling range of 30-60 ℃), oscillating at intervals, extracting for 10min, filtering the sample with filter paper, leaching for 3 times, washing the triangular flask and the filter paper with 10mL of petroleum ether, combining filtrates in a dried and weighed heart-shaped flask, carrying out vacuum spin-drying at 30 ℃, cooling and weighing m2.
Surface oil content% = (m 2-m 1)/m × 100
And (3) total oil determination: accurately weighing 2g of plant mixed essential oil microcapsule, dissolving in 10mL of 60 ℃ hot water, adding alpha-amylase, carrying out water bath at 60 ℃ for 10min, hydrolyzing starch in microcapsule wall materials, and releasing essential oil. After cooling, adding chloroform/methanol (15/30 mL) mixture, shaking for 10min, adding 15mL chloroform, shaking for 2min, adding 15mL distilled water, shaking for 5min, pouring into a centrifuge cup, centrifuging at 4200r/min for 5min, taking the lower layer liquid, placing in a dry weighed round bottom flask, and vacuum drying at 30 ℃.
Encapsulation ratio% = ([% total oil content-surface oil content)/total oil content ] × 100%
Scanning the prepared plant mixed essential oil emulsion by adopting an electronic scanning microscope, and observing the micro appearance of the deodorant plant mixed essential oil.
(2) Investigating the embedding rate of the microcapsule emulsion prepared by the wall material mixed solution with different mass ratios
Octenyl succinated starch, polyvinylpyrrolidone, maltodextrin were selected for testing in various proportions, and the total mass was about 150g.
TABLE 14
Ratio of Embedding rate
4:4:1 975
3:3:1 98.7
2:2:1 96.2
1:1:2 93.2
1:1:4 73.4
1:1:8 65.6
The results are shown in Table 14, with an octenyl succinated starch, polyvinylpyrrolidone, maltodextrin ratio of 4:4:1,3:3:1,2:2:1,1:1:2, the embedding rate is more than 90%, and the embedding rates are respectively 97.5%,98.7%,96.2% and 93.2%, wherein the proportion is 3:3: the embedding rate is higher when 1 hour is used, and is obviously larger than the rate of 1:1:2,1:1:4 (73.4%), 1:1: embedding rate at 8 (65.6%). Thereby determining the mass ratio of the octenyl succinate starch, the polyvinylpyrrolidone and the maltodextrin wall material to be 2-4: 2 to 4:1, most preferably 3:3:1.
the reason may be that octenyl succinate starch and polyvinylpyrrolidone are amphiphilic macromolecules, and a certain proportion of micromolecular maltodextrin is added to fill macromolecular cross-linking gaps so as to improve the embedding rate, but when the micromolecules are excessive, the embedding rate is reduced because the micromolecules do not have amphipathy and cannot form a macromolecular framework wall capsule structure.
(3) Investigating the embedding rate of microcapsule emulsion prepared by curing agents with different mass ratios and the particle size distribution of microcapsules
And the addition amounts of glutaraldehyde curing agents (mass ratio of glutaraldehyde to the total amount of the wall material mixed solution and the plant essential oil emulsion) are respectively 0.1%, 0.2%, 0.3%, 0.4%, 1%, 2%, 3% and 4%, so as to prepare the deodorant microcapsule core-wall mixed emulsion.
Watch 15
Glutaraldehyde addition amount% The embedding rate% Average particle diameter of nm
0.1 97.5 300
0.2 97.3 280
0.3 97.1 270
0.4 96.9 260
1 98.2 220
2 96.6 300
3 78.4 400
4 70.3 800
As shown in table 15, the microcapsule embedding rate gradually decreased with the increase of the addition amount of glutaraldehyde, the embedding rate was 96.6% or more for all of the addition amounts of 0.1% to 2%, and the embedding rate was significantly decreased (85.3% and 80.4%) for both of the addition amounts of 3% and 4%. The average particle size of the emulsion is firstly reduced and then increased along with the increase of the addition amount of the glutaraldehyde, and when the addition amount is 1%, the average particle size of the emulsion is the smallest, the dispersion is the most uniform, and the stability of the emulsion is the highest. It can be concluded from the table that the smaller the average particle size of the emulsion, the more stable the emulsion and the higher the embedding rate of the obtained microcapsules, because too little glutaraldehyde has poor curability and cannot form a stable emulsion; excessive glutaraldehyde causes excessive aggregation of macromolecular wall materials, flocculation is formed, and the stability of the emulsion is reduced. Therefore, the addition amount of glutaraldehyde is 0.1 to 2%, and the optimum addition amount is 1%.
(4) Investigating the embedding rate of the microcapsule emulsion and the particle size distribution of the microcapsule under the action of colloid rods with different homogenization pressures and different homogenization times
In the preparation of the microcapsule emulsion, when the homogenization pressure is 20, 25, 30, 35 and 40 times and the homogenization times are 2, 3 and 4 times, the embedding rate and the particle size distribution of the prepared microcapsule emulsion are realized.
TABLE 16
Figure BDA0002680978430000231
As a result, as shown in Table 16, the homogeneous pressure was 20 to 40mPa, the embedding rate increased with the increase in the pressure, and the embedding rate decreased with the increase in the pressure above 35 mPa. The highest embedding rate (98.4%) was obtained at 30mPa, and only 94.5% was obtained at 20 mPa. This phenomenon occurs in relation to the degree of shear break of the emulsion.
The embedding rate is obviously increased along with the increase of the homogenization times. The embedding rate of 3 and 4 homogenizations is 98.4% and 97.4%, respectively, which is significantly higher than that of 1 and 2 homogenizations (88.8% and 94.3%). The homogenizing times are increased, the shearing and crushing degree of the emulsion is higher, the combination of the wall material and the core material is firmer, the embedding rate is higher, and the homogenizing is selected for 3 times.
(5) Investigating the embedding rate and the water distribution of the microcapsule solid powder under the action of different air inlet temperatures and different air outlet temperatures
TABLE 17
The temperature of the inlet air is lower The embedding rate% Water content%
160 97.2 1.4
170 98.3 1.2
180 98.5 0.9
190 98.7 0.9
200 98.6 0.8
Watch 18
Air outlet temperature DEG C The embedding rate% Water content%
60 93.5 5.5
70 97.5 2.0
80 97.6 1.3
90 98.3 0.9
100 98.6 0.7
As shown in tables 17 and 18, the embedding rates are not significantly different and are 97.2-98.7% when the inlet air temperature is 160-200 ℃, and the water content of the microcapsule is significantly higher than other inlet air temperatures when the inlet air temperature is 160 ℃; when the air outlet temperature is 60 ℃, the embedding rate (93.5%) is obviously lower than that (97.5% -98.6%) of the air outlet temperature, but the moisture content is obviously reduced along with the rise of the air outlet temperature, and when the air outlet temperature is 100 ℃, the moisture content is only 0.7%. The result shows that the air inlet temperature has no obvious influence on the embedding rate and the moisture of the microcapsule, and the air outlet temperature has obvious influence on the embedding rate and the moisture of the microcapsule. Namely the optimal air inlet temperature is 170-190 ℃, and the air outlet temperature is 90-100 ℃.
Example 13 antipruritic and deodorant chip and pad for puerperal use
An antipruritic and deodorant chip is prepared by the following steps: the plant essential oil microcapsules prepared in example 11 were mixed with a binder and a dispersant, and the mixture was subjected to a two-dip two-roll treatment in which the bath ratio was 1:20, the first soaking is carried out for 30 minutes at room temperature, the rolling residual rate is 80 percent, the second soaking is carried out for 20 minutes, the rolling residual rate is 110 percent, the pre-drying temperature is set to be 70 ℃, the time is 5 minutes, and the finished product is ironed.
A puerpera pad with itching relieving and odor removing effects is prepared by placing the chip with itching relieving and odor removing effects into the middle of the inner layer of puerpera pad according to required size to form a functional chip layer.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (6)

1. A special chip for relieving itching and removing odor for women is characterized in that the chip is prepared by mixing plant essential oil microcapsules for relieving itching and removing odor with an adhesive and a dispersing agent and then loading the mixture on plant viscose fibers;
wherein the plant essential oil microcapsule comprises the following components:
(1) Wall material: octenyl succinate starch, polyvinylpyrrolidone, maltodextrin; the mass ratio of the octenyl succinate starch to the polyvinylpyrrolidone to the maltodextrin is 2-4: 2 to 4:1;
(2) Core material: plant essence; the plant essence comprises the following components: cnidium fruit oil, perilla leaf oil, chinese gall extract, radix sophorae flavescentis extract, almond extract, peony root bark extract, golden cypress extract, menthol and borneol; calculated by mass ratio of the total amount of the plant essence, 0.5-2 g/kg of cnidium fruit oil, 0.1-2 g/kg of perilla leaf oil, 1-5 g/kg of Chinese gall extract, 0.01-0.1 g/kg of radix sophorae flavescentis extract, 0.01-0.1 g/kg of almond extract, 0.01-0.1 g/kg of peony root bark extract, 0.001-0.01 g/kg of phellodendron extract, 3-6 g/kg of menthol and 0.1-0.5 g/kg of borneol;
(3) Emulsifier: span-80, tween-80;
(4) Curing agent: glutaraldehyde;
the mass ratio of the plant essence, span-80 and tween-80 is 8-12: 1 to 3:1;
the weight ratio of the itching relieving and odor removing plant essential oil microcapsule, the adhesive and the dispersing agent is 1:0.3 to 0.8:0.3 to 0.8.
2. The chip for relieving itching and removing odor according to claim 1, wherein the weight ratio of the plant essential oil microcapsules for relieving itching and removing odor, the adhesive and the dispersant is 1:0.5:0.5.
3. the chip for relieving itching and removing odor according to any one of claims 1 or 2, wherein the preparation method of the plant essence is as follows:
(1) Dissolving Galla chinensis extract in 70% ethanol, and ultrasonic treating to dissolve completely;
(2) Dissolving radix Sophorae Flavescentis extract and cortex Phellodendri extract in 70% ethanol, and ultrasonic treating to dissolve completely;
(3) Dissolving oleum Cnidii, perilla leaf oil, semen Armeniacae amarum extract, and cortex moutan extract in 70% ethanol, and mixing;
(4) Dissolving Mentholum and Borneolum Syntheticum in 70% ethanol, and ultrasonic dissolving;
(5) And (3) uniformly mixing the solutions obtained in the four steps, and adding 70% ethanol for diluting to a constant volume.
4. The chip for relieving itching and removing odor according to claim 1, wherein the preparation method of the plant essential oil microcapsule for relieving itching and removing odor comprises the following steps:
(1) Preparation of plant essential oil emulsion
Adding span-80 into the plant essence, adding tween-80 into distilled water, stirring for dissolving, mixing the two, and shearing and emulsifying with ultrasonic cell pulverizer to obtain plant essential oil emulsion;
(2) Preparation of wall material mixed liquid
Weighing octenyl succinate starch, polyvinylpyrrolidone and maltodextrin, adding into deionized water, and stirring to prepare a wall material mixed solution;
(3) Preparation of core-wall mixed emulsion
Slowly dripping the prepared wall material mixed solution into the prepared plant essential oil emulsion, stirring for complex coacervation reaction, and finally dripping glutaraldehyde for curing to prepare the deodorant microcapsule core wall mixed emulsion;
(4) Preparation of microcapsule emulsions
Carrying out colloid milling on the prepared core wall mixed emulsion, and homogenizing to obtain microcapsule emulsion;
(5) Preparation of microcapsule solid powder
Spray drying the prepared microcapsule emulsion to obtain plant essential oil microcapsule solid powder;
wherein, in the step (1), the working conditions of the ultrasonic cell crushing instrument are as follows: working time is 2s, interval time is 3s, working frequency is 300W, and emulsification is carried out for 200 times;
in the step (3), stirring is carried out for 5-10 min at the rotating speed of 8000 rpm; the addition amount of the glutaraldehyde is 0.1-2% by mass;
in the step (4), the homogenizing conditions are as follows: homogenizing for 2-3 times under the pressure of 25-35 mPa;
in the step (5), spray drying conditions are as follows: the air inlet temperature is 160-200 ℃, and the air outlet temperature is 80-110 ℃.
5. The chip for relieving itching and removing odor of claim 1, wherein the preparation method of the chip for relieving itching and removing odor comprises: carrying out two-dipping two-rolling treatment on the mixture of the plant essential oil microcapsules, the binder and the dispersant, wherein the bath ratio is 1:15 to 25 percent, the first soaking is room temperature soaking for 20 to 40 minutes, the rolling residual rate is 80 percent, the second soaking time is 20 minutes, the rolling residual rate is 110 percent, the pre-drying temperature is set to be 60 to 80 ℃, the time is 3 to 5 minutes, and the finished product is ironed.
6. A puerpera pad for relieving itching and removing odor is characterized in that the puerpera pad is prepared by placing the chip for relieving itching and removing odor of any one of claims 1 to 5 into the puerpera pad.
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