CN107970198B - Moistening and repairing hair conditioner containing periplaneta americana refined extract - Google Patents

Moistening and repairing hair conditioner containing periplaneta americana refined extract Download PDF

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CN107970198B
CN107970198B CN201810003454.2A CN201810003454A CN107970198B CN 107970198 B CN107970198 B CN 107970198B CN 201810003454 A CN201810003454 A CN 201810003454A CN 107970198 B CN107970198 B CN 107970198B
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periplaneta americana
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CN107970198A (en
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郝振平
徐溧
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KUNMING SINOWAY NATURAL PHARMACEUTICALS CO Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/98Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
    • A61K8/987Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin of species other than mammals or birds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/12Preparations containing hair conditioners

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Abstract

The invention relates to a moistening and repairing hair conditioner containing periplaneta americana extract. The invention uses the effective components in the liquid medicine and the water washing liquid discarded in the step E in the preparation method of the periplaneta americana extract for treating hepatitis B disclosed in the Chinese patent with the patent number of 201210446628.5 to finely extract the periplaneta americana extract. The components are as follows: 0.5-5% of periplaneta americana refined extract, 0.5-5% of prinsepia utilis royle oil, 10-20% of octadecyl trimethyl ammonium chloride, 3-10% of isopropyl lanolate, 1-5% of glycerol, 0.01-0.3% of essence and the balance of water. The hair conditioner can penetrate into damaged hair scales, and has good nourishing and repairing effects on hair damaged by chemical or external factors.

Description

Moistening and repairing hair conditioner containing periplaneta americana refined extract
Technical Field
The invention relates to the technical field of daily chemical products, in particular to a moistening and repairing hair conditioner containing periplaneta americana essence extract.
Background
The healthy hair surface layer is a protective film of hair formed by a group of complete hair flakes and naturally secreted grease, and the natural protective film can be damaged by excessive washing, scalding and dyeing and sunshine solarization, so that the water loss of the surface layer is caused, the hair is dried up, and the elasticity and the softness are lost. Only by using the hair conditioner frequently, the protective film of the hair can be formed permanently, and the hair can be prevented from being damaged.
The hair conditioner is mainly divided into the following types: (1) the product is a wash-free type. The leave-on hair conditioner can prevent the hair scales from being damaged and generating static electricity. Some components in the shampoo can only be absorbed by the surface of hair, so the leave-on hair conditioner can not play a role in radically curing damaged hair. (2) And (5) carrying out postdyeing. The special shampoo and hair conditioner for hair dyeing can stabilize pigment particles, so that the pigment particles are not easy to lose quickly. (3) And (5) hair waving. After the special shampoo after perming is used, the curl is maintained for a longer time and the hair is more glossy by matching with the hair conditioner with fixed curl, and the rinse-free curly hair conditioner is smeared after the hair is wiped and before air blowing and shaping, so that the hair is more moisturized and moist. (4) Specific type. The hair is kept natural and balanced moisture and the moisture is supplemented. Can be used for treating split hair, dry hair, or difficult combing hair. It can keep hair moisture, reduce static electricity and increase luster. It also produces a protective film during the heat styling of the hair, particularly for long, thin hairs.
Wherein, (1) dry hair is lack of water and oil, and is easy to become dry and dry when meeting the sunlight, and can be yellow, branched, fragile and easy to break, and hair conditioner with moisturizing effect is suitable for use; (2) oily hair is often greasy and sticky, and a hair conditioner for controlling oil and refreshing hair style is suitable to be used, so that the oily hair can keep dry, comfortable and comfortable for a long time; (3) the fragile hair quality is damaged due to the extreme lack of nutrition, so that the elasticity is lost, and the fragile hair quality is easy to break, and a hair conditioner containing nutrient components is preferably selected for nursing; (4) the dry yellow hair is preferably washed with shampoo and hair conditioner with hair blackening effect, and the hair conditioner with skin caring component is used 2 times per week.
Periplaneta americana is an insect of the genus Periplaneta of the family Periplaneta of the order Periplaneta of the class Insecta, commonly called Blatta seu periplaneta, the largest volume insect of the family Blattadae, native to south America. Periplaneta americana is a traditional Chinese medicinal material, and is recorded in Shen nong's herbal Jing, which is called salty and cold in taste. Mainly has the effects of blood stasis, hard mass, cold and heat, mass breaking, throat and throat contraction, internal cold and no seed, and is used for treating infantile malnutrition, furuncle, carbuncle, tonsillitis, innominate toxic swelling, syphilis, venomous snake bite, centipede bite and the like.
Modern researches find that the periplaneta americana dry worm extract contains active substances such as WHF (polyhydric alcohols, epidermal growth factor), muconic acid, mucoglycine and various amino acids, and has the effects of resisting inflammation, reducing swelling, promoting cell proliferation and growth of new granulation tissues, accelerating repair of damaged tissues, accelerating shedding of necrotic tissues, improving the immune function of organisms and the like. The research also finds that the ethanol extract of the periplaneta americana contains a large amount of free amino acids, and contains 18 kinds of amino acids essential to human bodies and also contains a plurality of other amino acids, and the total number of the amino acids is up to 26. It is the combination of these specific amino acids that makes the periplaneta americana extract have the remarkable effect of promoting the repair of damaged cells and the growth of new cells.
Prinsepia utilis Royle, also called Prinsepia utilis Royle, is called Prinsepia utilis Royle in Yunnan herbal medicine, and is produced on hillsides and wasteland with the altitude of 1400-3100 m in Yunnan, Guizhou and Sichuan. The average oil yield of the prinsepia utilis royle is 28%, the fruit oil is rich in various nutrient components required by a human body, is high-grade natural edible oil, and has important auxiliary effects on treating hyperlipidemia, reducing cholesterol, preventing and treating cardiovascular diseases and the like. The fatty acid composition of the prinsepia utilis royle oil mainly comprises unsaturated fatty acids, namely oleic acid and linoleic acid, wherein the content of the oleic acid is 33.38%, and the content of the linoleic acid is 40.82%; in addition, the olive oil also contains 17.2% of palmitic acid and 6% of stearic acid, contains various vitamins such as vitamin A, vitamin D, vitamin E, vitamin K and the like, contains 3.5mg of vitamin A, 2.1mg of vitamin D, 11.2mg of vitamin E and 0.30mg of vitamin K per 100g of prinsepia utilis royle oil, also contains very rich major and trace elements such as calcium, sulfur, manganese, magnesium, potassium, phosphorus, zinc, iron and the like, and compared with other edible oils, the element with the highest content is potassium, and the content is 9.8 mg/kg.
The Prinsepia utilis Royle oil retains pure natural bioactive components, contains multiple fat-soluble vitamins and microelements which are easy to be absorbed by human body, a large amount of amino acids which are necessary for human body, and a fatty acid structure (1: 1: 0.8) which is very close to the proportion (1: 1: 1) of human body lipid, so that the Prinsepia utilis Royle oil has good permeability and is easy to be absorbed by skin, can keep the nutrition, moisture and elasticity of the skin, improve the degeneration of the horny layer of the skin and repair rough skin. Scientific research finds that the prinsepia utilis royle oil has no toxic or side effect on human bodies no matter the prinsepia utilis royle oil is taken orally or used externally; has no irritation to human skin; the skin has good permeability, can improve cutin degradation, and has effects of keeping moisture, preventing chapping, and supplementing nutrition; has obvious functions of diminishing inflammation, inhibiting bacteria, resisting ultraviolet ray, resisting senility, improving the circulation of crinkles and promoting metabolism.
The Chinese patent with the patent number 201210446628.5, which was filed by the inventor 2012, discloses a preparation method of a periplaneta americana extract for treating hepatitis b, and the extraction process is as follows:
A. inactivation and crushing: killing the fresh American cockroach by hot water at 80-90 ℃, controlling the temperature within 60 +/-5 ℃ for drying, crushing, and sieving by a 24-mesh sieve to prepare coarse American cockroach powder;
B. extraction: c, performing 3-5 times of reflux extraction on the periplaneta americana coarse powder obtained in the step A at the temperature of 75-80 ℃, and adding 90-95% ethanol in an amount which is 5-8 times the weight of the coarse powder during the first extraction for 4-6 hours; adding 90-95% ethanol in an amount which is 3-6 times the weight of the coarse powder every time after the second time, wherein the extraction time is 3-5 hours; in the extraction process, the temperature of ethanol is kept at 75-80 ℃, after extraction is finished, the extracting solutions are combined and filtered to obtain an ethanol extracting solution;
C. primary concentration: concentrating the ethanol extract obtained in the step B under reduced pressure under the conditions of vacuum degree of-0.05 to-0.06 MPa and temperature of 50 to 60 ℃ until the specific gravity is 1.05 to 1.15 to obtain an ethanol concentrated solution;
D. degreasing and adsorbing: adding distilled water which is 7-10 times of the weight of the ethanol concentrated solution into the ethanol concentrated solution obtained in the step C, heating to 80-90 ℃ while stirring, stirring for 10-60 minutes at a stirring speed of 20-60 revolutions per minute, and then keeping the temperature and standing for 1-5 hours to separate oil from water; collecting the lower-layer water solution, filtering the lower-layer water solution by using filter paper, adding medicinal active carbon which is 0.5 to 1.0 time of the ethanol concentrated solution into the obtained filtrate, and stirring the mixture at the temperature of between 40 and 60 ℃ for 30 to 60 minutes to ensure that the mixture is fully adsorbed;
E. and (3) elution: d, filling the active carbon-containing liquid medicine obtained in the step D into a chromatographic column, discharging the liquid medicine, washing with distilled water which is 10-30 times of the amount of the active carbon, and discarding the water washing liquid; eluting with 30-60 times of eluant of medicinal active carbon, collecting eluent, and filtering with filter paper to obtain elution filtrate;
F. secondary concentration: concentrating the elution filtrate obtained in the step E under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa until the specific gravity is 1.20-1.30 to obtain the periplaneta americana extract for treating hepatitis B;
G. drying and crushing: and F, drying the American cockroach extract for treating the hepatitis B in vacuum at the temperature of 50-60 ℃ and under the vacuum degree of-0.04-0.07 MPa, and crushing into fine powder to obtain the finished product of the American cockroach extract for treating the hepatitis B.
The patent is a patent granted to the inventor. The step E procedure of this patent application is elution: and D, filling the active carbon-containing liquid medicine obtained in the step D into a chromatographic column, discharging the liquid medicine, washing with distilled water which is 10-30 times of the amount of the active carbon, and discarding the water washing liquid. Through years of research and experiments of the inventor, the discarded liquid medicine and water washing liquid still contain a lot of valuable effective components of the periplaneta americana, and the discarded white cockroach is very unfortunately, so that how to fully utilize the effective components in the discarded liquid medicine and the water washing liquid becomes another research and development target of the inventor.
Disclosure of Invention
The invention aims to provide a moistening and repairing hair conditioner containing periplaneta americana extract, which is developed by using effective components in liquid medicine and water washing liquid discarded in the step E in the preparation method of the periplaneta americana extract for treating hepatitis B disclosed by the Chinese patent with the patent number of 201210446628.5, can permeate into damaged hair scales and has good nourishing and repairing effects on chemically and externally damaged hair.
The present invention achieves the above object by the following method.
A moistening and repairing hair conditioner containing American cockroach refined extract comprises the following components in percentage by weight:
0.5-5% of periplaneta americana refined extract, 0.5-5% of prinsepia utilis royle oil, 10-20% of octadecyl trimethyl ammonium chloride, 3-10% of isopropyl lanolate, 1-5% of glycerol, 0.01-0.3% of essence and the balance of water.
Preferably, the moistening and repairing hair conditioner containing the periplaneta americana essence extract comprises the following components in percentage by weight:
1.5-3.2% of periplaneta americana refined extract, 1.5-3.2% of prinsepia utilis royle oil, 12-17% of octadecyl trimethyl ammonium chloride, 5-8% of isopropyl lanolate, 2.5-4% of glycerol, 0.08-0.2% of essence and the balance of water.
Preferably, the essence is one or a mixture of more of pomegranate essence, tea plant essence and grapefruit essence.
The moistening and repairing hair conditioner containing the periplaneta americana refined extract is prepared by the following process:
s1, weighing the components of the skin cream according to the parts by weight;
s2, adding water into a pot, heating to 60-70 ℃, adding octadecyl trimethyl ammonium chloride, isopropyl lanolate and glycerol, and uniformly stirring;
s3, cooling the liquid in the pot to 30-40 ℃, adding the periplaneta americana extract, the prinsepia utilis royle oil and the essence, homogenizing at a high speed and stirring for 5-20 minutes, and cooling to obtain the feed.
Preferably, the moistening and repairing hair conditioner containing the periplaneta americana extract is prepared by refining the liquid medicine and the water washing liquid discarded in the step E in the preparation process of the periplaneta americana extract disclosed in the Chinese patent 201210446628.5 according to the following process, and the specific process comprises the following steps:
a. inactivation and crushing: killing the fresh American cockroach by hot water at 80-90 ℃, controlling the temperature within 60 +/-5 ℃ for drying, crushing, and sieving by a 24-mesh sieve to prepare coarse American cockroach powder;
b. extraction: c, performing 3-5 times of reflux extraction on the periplaneta americana coarse powder obtained in the step a at the temperature of 75-80 ℃, and adding 90-95% ethanol in an amount which is 5-8 times the weight of the coarse powder during the first extraction for 4-6 hours; adding 90-95% ethanol in an amount which is 3-6 times the weight of the coarse powder every time after the second time, wherein the extraction time is 3-5 hours; in the extraction process, the temperature of ethanol is kept at 75-80 ℃, after extraction is finished, the extracting solutions are combined and filtered to obtain an ethanol extracting solution;
c. primary concentration: c, concentrating the ethanol extract obtained in the step b under reduced pressure under the conditions of vacuum degree of-0.05 to-0.06 MPa and temperature of 50 to 60 ℃ until the specific gravity is 1.05 to 1.15 to obtain an ethanol concentrated solution;
d. degreasing and adsorbing: adding distilled water which is 7-10 times of the weight of the ethanol concentrated solution into the ethanol concentrated solution obtained in the step c, heating to 80-90 ℃ while stirring, stirring for 10-60 minutes at a stirring speed of 20-60 revolutions per minute, and then keeping the temperature and standing for 1-5 hours to separate oil from water; collecting the lower-layer water solution, filtering the lower-layer water solution by using filter paper, adding medicinal active carbon which is 0.5 to 1.0 time of the ethanol concentrated solution into the obtained filtrate, and stirring the mixture at the temperature of between 40 and 60 ℃ for 30 to 60 minutes to ensure that the mixture is fully adsorbed;
e. and (3) elution: d, filling the activated carbon-containing liquid medicine obtained in the step d into a chromatographic column, discharging the liquid medicine, washing with distilled water 10-30 times of the amount of the medicinal activated carbon, and collecting and uniformly mixing the liquid medicine and the washing liquid;
f. membrane separation: under the pressure of 50-200kPa, collecting the liquid medicine and the water washing liquid which are uniformly mixed in the step e, passing through an ultrafiltration ceramic membrane with the molecular cut-off value of 50kD, discarding the cut-off liquid, and collecting penetrating fluid;
g. secondary concentration: c, concentrating the penetrating fluid obtained in the step a under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa to 1/10-1/30 of the original volume;
h. ion exchange: taking the secondary concentrated solution obtained in the step g, using hydrochloric acid with the concentration of 1mol/L and sodium hydroxide with the concentration of 1mol/L to adjust the pH value of the concentrated penetrating fluid obtained in the step g to be 5-7, then passing through a regenerated sodium type HD-8 strong-acid styrene type cation exchange resin column, using sodium type HD-8 strong-acid styrene type cation exchange resin which is 3-7 times of the concentrated penetrating fluid obtained in the step g according to the volume, after the adsorption of the sodium type HD-8 strong-acid styrene type cation exchange resin column is finished, firstly using deionized water with the volume of 2-4 times of the amount of the sodium type HD-8 strong-acid styrene type cation exchange resin, then using ammonia water solution with the concentration of 1-3mol/L to elute, wherein the using amount of the ammonia water solution with the concentration of 1-3mol/L is 5-8 times of the amount of the sodium type HD-8 strong-acid styrene type cation exchange resin, controlling the flow rate of the eluent to ensure that the time of the whole elution process is 8-12 hours, and collecting the eluent;
i. and (3) third-stage concentration: and (5) concentrating the eluent obtained in the step h under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa to obtain an extract with the specific gravity of 1.20-1.30, thus obtaining the periplaneta americana refined extract.
Preferably, the process of the step f is membrane separation: and e, under the pressure of 80kPa, collecting the uniformly mixed liquid medicine and water washing liquid, passing through an ultrafiltration ceramic membrane with the molecular cut-off value of 50kD, discarding the cut-off liquid, and collecting penetrating fluid.
Preferably, the process of the step g comprises two-stage concentration: and f, concentrating the penetrating fluid obtained in the step f under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa to 1/20 of the original volume.
Preferably, the process of the step h is that ion exchange: taking the secondary concentrated solution obtained in the step g, regulating the pH value of the concentrated penetrating fluid obtained in the step g to be 6.0 by using hydrochloric acid with the concentration of 1mol/L and sodium hydroxide with the concentration of 1mol/L, then passing through a regenerated sodium type HD-8 strong-acid styrene type cation exchange resin column, washing the sodium type HD-8 strong-acid styrene type cation exchange resin with deionized water with the volume of 3 times of the amount of the sodium type HD-8 strong-acid styrene type cation exchange resin after the adsorption of the sodium type HD-8 strong-acid styrene type cation exchange resin column is finished, then eluting by using ammonia water with the concentration of 1-3mol/L, wherein the using amount of the ammonia water with the concentration of 1.5mol/L is 6 times of the amount of the sodium type HD-8 strong-acid styrene type cation exchange resin, controlling the flow rate of the eluent to ensure that the time of the whole elution process is 10 hours, and collecting the eluent.
The invention has the beneficial effects that:
1. the American cockroach refined extract contains up to 26 pure natural amino acids and 18 amino acids necessary for human body, and by the process, the ineffective components are removed, so that the total amino acid content in the refined extract is up to 60-80%. The high-quality periplaneta americana refined extract enables the hair conditioner of the invention to have obvious effects of promoting damaged cell repair and new cell growth.
2. The periplaneta americana refined extract added in the invention is prepared by extracting the periplaneta americana extract for treating hepatitis B from the periplaneta americana and then refining the periplaneta americana extract by using waste liquid medicine and washing liquid, belongs to waste recycling, and can furthest utilize active substances in the periplaneta americana medicinal material, thereby achieving the purposes of recycling waste, reducing cost, increasing resource utilization rate, increasing profits, saving energy and reducing emission, and effectively improving the product competitiveness of enterprises.
3. The moistening and repairing hair conditioner containing the periplaneta americana essence extract produced by the invention can permeate into damaged hair scales, and has good nourishing and repairing effects on chemically and externally damaged hair.
4. The American cockroach fine extract extracted by the process can effectively remove peculiar smell and color of the American cockroach, the produced American cockroach fine extract is almost colorless and tasteless, and is added as a raw material for producing the hair conditioner, the color of the produced hair conditioner is not influenced by the color of the American cockroach, the foreign smell of the American cockroach is avoided, and the hair conditioner is easy to accept by consumers.
Detailed Description
The present invention is further illustrated by the following specific examples, which are provided for illustrative purposes only and do not limit the scope of the present invention. The moistening and repairing hair conditioner containing the periplaneta americana essence extract prepared in the following example has the following preparation method:
s1, weighing the components of the skin cream according to the parts by weight.
S2, adding water into the pot, heating to 60 ℃, adding octadecyl trimethyl ammonium chloride, isopropyl lanolate and glycerol, and stirring uniformly.
S3, cooling the liquid in the pot to 35 ℃, adding the periplaneta americana extract, the prinsepia utilis royle oil and the essence, homogenizing at a high speed, stirring for 15 minutes, and cooling to obtain the compound feed.
Example 1
The moistening and repairing hair conditioner containing the American cockroach refined extract comprises the following components in percentage by weight: 2% of periplaneta americana extract, 2% of prinsepia utilis royle oil, 15% of octadecyl trimethyl ammonium chloride, 7% of isopropyl lanolate, 3% of glycerol, 0.1% of pomegranate essence and the balance of water. The moistening and repairing hair conditioner containing the American cockroach refined extract is prepared.
The periplaneta americana extract is prepared by refining the liquid medicine and the water washing liquid discarded in the step E in the preparation process of the periplaneta americana extract disclosed in the Chinese patent 201210446628.5 according to the following process:
a. inactivation and crushing: killing fresh Periplaneta americana with 80 deg.C hot water, oven drying at 60 + -5 deg.C, pulverizing, and sieving with 24 mesh sieve to obtain Periplaneta americana coarse powder;
b. extraction: c, performing reflux extraction on the periplaneta americana coarse powder obtained in the step a for 3 times at the temperature of 75 ℃, and adding 90% ethanol in an amount which is 5 times the weight of the coarse powder during the first extraction for 4 hours; adding 90% ethanol with 3 times of the weight of the coarse powder for 3 hr each time; in the extraction process, the temperature of the ethanol is kept at 75 ℃, after the extraction is finished, the extracting solutions are combined and filtered to obtain an ethanol extract;
c. primary concentration: c, concentrating the ethanol extract obtained in the step b under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa until the specific gravity is 1.05 to obtain an ethanol concentrated solution;
d. degreasing and adsorbing: adding distilled water which is 7 times of the weight of the ethanol concentrated solution into the ethanol concentrated solution obtained in the step c, heating to 80 ℃ while stirring, stirring for 10 minutes at the stirring speed of 20 r/min, and then keeping the temperature and standing for 4 hours to separate oil from water; collecting lower layer water solution, filtering with filter paper, adding 0.5 times of medicinal active carbon into the filtrate, stirring at 40 deg.C for 50 min for full adsorption;
e. and (3) elution: d, filling the activated carbon-containing liquid medicine obtained in the step d into a chromatographic column, discharging the liquid medicine, washing with distilled water 10-30 times of the amount of the medicinal activated carbon, and collecting and uniformly mixing the liquid medicine and the washing liquid;
f. membrane separation: under the pressure of 200kPa, collecting the liquid medicine and the water washing liquid which are uniformly mixed in the step e, passing through an ultrafiltration ceramic membrane with the molecular cut-off value of 50kD, discarding the cut-off liquid, and collecting penetrating fluid;
g. secondary concentration: concentrating the penetrating fluid obtained in the step f under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa to 1/20 of the original volume;
h. ion exchange: taking the secondary concentrated solution obtained in the step g, using hydrochloric acid with the concentration of 1mol/L and sodium hydroxide with the concentration of 1mol/L to adjust the pH value of the concentrated penetrating fluid obtained in the step g to be 5, then passing through a regenerated sodium type HD-8 strong-acid styrene type cation exchange resin column, using sodium type HD-8 strong-acid styrene type cation exchange resin which is 4 times of the concentrated penetrating fluid obtained in the step g according to the volume, after the adsorption of the sodium type HD-8 strong-acid styrene type cation exchange resin column is finished, firstly using deionized water with the volume of 2 times of the amount of the sodium type HD-8 strong-acid styrene type cation exchange resin, then using ammonia water with the concentration of 1mol/L to elute, wherein the using amount of the ammonia water with the concentration of 1.5mol/L is 6 times of the amount of the sodium type HD-8 strong-acid styrene type cation exchange resin, controlling the flow rate of the eluent to ensure that the time of the whole elution process is 10 hours, and collecting the eluent;
i. and (3) third-stage concentration: and (5) concentrating the eluent obtained in the step h under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa to obtain an extract with the specific gravity of 1.24, thus obtaining the periplaneta americana refined extract.
The hair conditioner prepared in this example has the comprehensive effects shown in Table 1. The periplaneta americana refined extract prepared by the embodiment contains up to 26 pure natural small molecular amino acids, and the total amino acid content in the refined extract is up to 62.6%.
Example 2
The moistening and repairing hair conditioner containing the American cockroach refined extract comprises the following components in percentage by weight: 1% of periplaneta americana extract, 3% of prinsepia utilis royle oil, 10% of octadecyl trimethyl ammonium chloride, 8% of isopropyl lanolate, 1% of glycerol, 0.2% of tea plant essence and the balance of water. The moistening and repairing hair conditioner containing the American cockroach refined extract is prepared.
The periplaneta americana extract is prepared by refining the liquid medicine and the water washing liquid discarded in the step E in the preparation process of the periplaneta americana extract disclosed in the Chinese patent 201210446628.5 according to the following process:
a. inactivation and crushing: killing fresh Periplaneta americana with hot water of 90 deg.C, oven drying at 60 + -5 deg.C, pulverizing, and sieving with 24 mesh sieve to obtain Periplaneta americana coarse powder;
b. extraction: c, performing reflux extraction on the periplaneta americana coarse powder obtained in the step a for 5 times at the temperature of 80 ℃, and adding 95% ethanol with the concentration being 8 times of the weight of the coarse powder during the first extraction, wherein the extraction time is 6 hours; adding 95% ethanol 6 times the weight of the coarse powder for 5 hr each time; in the extraction process, the temperature of ethanol is kept at 80 ℃, after the extraction is finished, the extracting solutions are combined and filtered to obtain an ethanol extract;
c. primary concentration: c, concentrating the ethanol extract obtained in the step b under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa until the specific gravity is 1.15 to obtain an ethanol concentrated solution;
d. degreasing and adsorbing: adding distilled water which is 10 times of the weight of the ethanol concentrated solution into the ethanol concentrated solution obtained in the step c, heating to 90 ℃ while stirring, stirring for 60 minutes at the stirring speed of 60 revolutions per minute, and then keeping the temperature and standing for 5 hours to separate oil from water; collecting lower layer water solution, filtering with filter paper, adding 1.0 times of medicinal active carbon into the filtrate, stirring at 60 deg.C for 60 min for full adsorption;
e. and (3) elution: d, filling the liquid medicine containing the activated carbon obtained in the step d into a chromatographic column, discharging the liquid medicine, washing the liquid medicine with distilled water 30 times of the amount of the medicinal activated carbon, and collecting and uniformly mixing the liquid medicine and the washing liquid;
f. membrane separation: under the pressure of 50kPa, collecting the liquid medicine and the water washing liquid which are uniformly mixed in the step e, passing through an ultrafiltration ceramic membrane with the molecular cut-off value of 50kD, discarding the cut-off liquid, and collecting penetrating fluid;
g. secondary concentration: concentrating the penetrating fluid obtained in the step f under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa to 1/10 of the original volume;
h. ion exchange: taking the secondary concentrated solution obtained in the step g, using hydrochloric acid with the concentration of 1mol/L and sodium hydroxide with the concentration of 1mol/L to adjust the pH value of the concentrated penetrating fluid obtained in the step g to be 7, then passing through a regenerated sodium type HD-8 strong-acid styrene type cation exchange resin column, using sodium type HD-8 strong-acid styrene type cation exchange resin which is 7 times of the concentrated penetrating fluid obtained in the step g according to the volume, after the adsorption of the sodium type HD-8 strong-acid styrene type cation exchange resin column is finished, firstly using deionized water with the volume of 4 times of the amount of the sodium type HD-8 strong-acid styrene type cation exchange resin, then using ammonia water with the concentration of 3mol/L to elute, wherein the usage amount of the ammonia water with the concentration of 3mol/L is 8 times of the amount of the sodium type HD-8 strong-acid styrene type cation exchange resin, controlling the flow rate of the eluent to ensure that the time of the whole elution process is 12 hours, and collecting the eluent;
i. and (3) third-stage concentration: and (5) concentrating the eluent obtained in the step h under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa to obtain an extract with the specific gravity of 1.30, thus obtaining the periplaneta americana refined extract.
The hair conditioner prepared in this example has the comprehensive effects shown in Table 1. The periplaneta americana refined extract prepared by the embodiment contains up to 26 pure natural small molecular amino acids, and the total amino acid content in the refined extract is up to 68.2%.
Example 3
The moistening and repairing hair conditioner containing the American cockroach refined extract comprises the following components in percentage by weight: 3% of periplaneta americana refined extract, 0.5% of prinsepia utilis royle oil, 16% of octadecyl trimethyl ammonium chloride, 5% of isopropyl lanolate, 4% of glycerol, 0.01% of grapefruit essence and the balance of water. The moistening and repairing hair conditioner containing the American cockroach refined extract is prepared.
The periplaneta americana extract is prepared by refining the liquid medicine and the water washing liquid discarded in the step E in the preparation process of the periplaneta americana extract disclosed in the Chinese patent 201210446628.5 according to the following process:
a. inactivation and crushing: killing fresh Periplaneta americana with 85 deg.C hot water, oven drying at 60 + -5 deg.C, pulverizing, and sieving with 24 mesh sieve to obtain Periplaneta americana coarse powder;
b. extraction: c, performing reflux extraction on the periplaneta americana coarse powder obtained in the step a for 4 times at the temperature of 75 ℃, and adding 90% ethanol in an amount which is 6 times the weight of the coarse powder when the coarse powder is extracted for 5 hours; adding 90% ethanol with a concentration 4 times the weight of the coarse powder for 4 hr each time; in the extraction process, the temperature of ethanol is kept at 80 ℃, after the extraction is finished, the extracting solutions are combined and filtered to obtain an ethanol extract;
c. primary concentration: c, concentrating the ethanol extract obtained in the step b under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa until the specific gravity is 1.1 to obtain an ethanol concentrated solution;
d. degreasing and adsorbing: c, adding distilled water which is 8 times of the weight of the ethanol concentrated solution into the ethanol concentrated solution obtained in the step c, heating to 85 ℃ while stirring, stirring for 40 minutes at the stirring speed of 40 revolutions per minute, and then keeping the temperature and standing for 3 hours to separate oil from water; collecting lower layer water solution, filtering with filter paper, adding 0.6 times of medicinal active carbon into the filtrate, stirring at 50 deg.C for 50 min for full adsorption;
e. and (3) elution: d, filling the liquid medicine containing the activated carbon obtained in the step d into a chromatographic column, discharging the liquid medicine, washing the liquid medicine with distilled water 20 times of the amount of the medicinal activated carbon, and collecting and uniformly mixing the liquid medicine and the washing liquid;
f. membrane separation: under the pressure of 150kPa, collecting the liquid medicine and the water washing liquid which are uniformly mixed in the step e, passing through an ultrafiltration ceramic membrane with the molecular cut-off value of 50kD, discarding the cut-off liquid, and collecting penetrating fluid;
g. secondary concentration: concentrating the penetrating fluid obtained in the step f under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa to 1/30 of the original volume;
h. ion exchange: taking the secondary concentrated solution obtained in the step g, using hydrochloric acid with the concentration of 1mol/L and sodium hydroxide with the concentration of 1mol/L to adjust the pH value of the concentrated penetrating fluid obtained in the step g to be 6, then passing through a regenerated sodium type HD-8 strong-acid styrene type cation exchange resin column, using sodium type HD-8 strong-acid styrene type cation exchange resin which is 5 times of the concentrated penetrating fluid obtained in the step g according to the volume, after the adsorption of the sodium type HD-8 strong-acid styrene type cation exchange resin column is finished, firstly using deionized water with the volume of 3 times of the amount of the sodium type HD-8 strong-acid styrene type cation exchange resin, then using ammonia water with the concentration of 1.5mol/L to elute, wherein the using amount of the ammonia water with the concentration of 1.5mol/L is 6 times of the amount of the sodium type HD-8 strong-acid styrene type cation exchange resin, controlling the flow rate of the eluent to ensure that the time of the whole elution process is 10 hours, and collecting the eluent;
i. and (3) third-stage concentration: and (5) concentrating the eluent obtained in the step h under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa to obtain an extract with the specific gravity of 1.25, thus obtaining the periplaneta americana refined extract.
The hair conditioner prepared in this example has the comprehensive effects shown in Table 1. The periplaneta americana refined extract prepared in the embodiment contains up to 26 pure natural small molecular amino acids, and the total amino acid content in the refined extract is up to 73.9%.
Example 4
The moistening and repairing hair conditioner containing the American cockroach refined extract comprises the following components in percentage by weight: 0.5% of periplaneta americana extract, 4% of prinsepia utilis royle oil, 20% of octadecyl trimethyl ammonium chloride, 3% of isopropyl lanolate, 5% of glycerol, 0.08% of pomegranate essence and the balance of water. The moistening and repairing hair conditioner containing the American cockroach refined extract is prepared.
The periplaneta americana extract is prepared by refining the liquid medicine and the water washing liquid discarded in the step E in the preparation process of the periplaneta americana extract disclosed in the Chinese patent 201210446628.5 according to the following process:
a. inactivation and crushing: killing fresh Periplaneta americana with hot water at 80 deg.C, oven drying at 60 + -5 deg.C, pulverizing, and sieving with 24 mesh sieve to obtain Periplaneta americana coarse powder;
b. extraction: c, performing reflux extraction on the periplaneta americana coarse powder obtained in the step a for 5 times at the temperature of 75 ℃, and adding 95% ethanol with the concentration being 8 times of the weight of the coarse powder during the first extraction, wherein the extraction time is 4 hours; adding 95% ethanol 4 times the weight of the coarse powder for 4 hr each time; in the extraction process, the temperature of the ethanol is kept at 75 ℃, after the extraction is finished, the extracting solutions are combined and filtered to obtain an ethanol extract;
c. primary concentration: c, concentrating the ethanol extract obtained in the step b under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa until the specific gravity is 1.15 to obtain an ethanol concentrated solution;
d. degreasing and adsorbing: adding distilled water which is 10 times of the weight of the ethanol concentrated solution into the ethanol concentrated solution obtained in the step c, heating to 85 ℃ while stirring, stirring for 30 minutes at the stirring speed of 30 revolutions per minute, and then keeping the temperature and standing for 5 hours to separate oil from water; collecting lower layer water solution, filtering with filter paper, adding 1.0 times of medicinal active carbon into the filtrate, stirring at 40 deg.C for 60 min for full adsorption;
e. and (3) elution: d, filling the liquid medicine containing the activated carbon obtained in the step d into a chromatographic column, discharging the liquid medicine, washing the liquid medicine with distilled water 20 times of the amount of the medicinal activated carbon, and collecting and uniformly mixing the liquid medicine and the washing liquid;
f. membrane separation: under the pressure of 80kPa, collecting the liquid medicine and the water washing liquid which are uniformly mixed in the step e, passing through an ultrafiltration ceramic membrane with the molecular cut-off value of 50kD, discarding the cut-off liquid, and collecting penetrating fluid;
g. secondary concentration: concentrating the penetrating fluid obtained in the step f under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa to 1/20 of the original volume;
h. ion exchange: taking the secondary concentrated solution obtained in the step g, regulating the pH value of the concentrated penetrating fluid obtained in the step g to be 6.0 by using hydrochloric acid with the concentration of 1mol/L and sodium hydroxide with the concentration of 1mol/L, then passing through a regenerated sodium type HD-8 strong-acid styrene type cation exchange resin column, washing the sodium type HD-8 strong-acid styrene type cation exchange resin with deionized water with the volume of 3 times of the amount of the sodium type HD-8 strong-acid styrene type cation exchange resin after the adsorption of the sodium type HD-8 strong-acid styrene type cation exchange resin column is finished, then eluting by using ammonia water with the concentration of 1-3mol/L, wherein the using amount of the ammonia water with the concentration of 1.5mol/L is 6 times of the amount of the sodium type HD-8 strong-acid styrene type cation exchange resin, controlling the flow rate of the eluent to ensure that the time of the whole elution process is 10 hours, and collecting the eluent.
i. And (3) third-stage concentration: and (5) concentrating the eluent obtained in the step h under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa to obtain an extract with the specific gravity of 1.21, thus obtaining the periplaneta americana refined extract.
The hair conditioner prepared in this example has the comprehensive effects shown in Table 1. The periplaneta americana refined extract prepared in the embodiment contains up to 26 pure natural small molecular amino acids, and the total amino acid content in the refined extract is up to 79.7%.
Example 5
The moistening and repairing hair conditioner containing the American cockroach refined extract comprises the following components in percentage by weight: 5% of periplaneta americana refined extract, 1% of prinsepia utilis royle oil, 12% of octadecyl trimethyl ammonium chloride, 10% of isopropyl lanolate, 2% of glycerol, 0.3% of tea flower essence and the balance of water. The moistening and repairing hair conditioner containing the American cockroach refined extract is prepared.
The periplaneta americana extract is prepared by refining the liquid medicine and the water washing liquid discarded in the step E in the preparation process of the periplaneta americana extract disclosed in the Chinese patent 201210446628.5 according to the following process:
a. inactivation and crushing: killing fresh Periplaneta americana with hot water at 80 deg.C, oven drying at 60 + -5 deg.C, pulverizing, and sieving with 24 mesh sieve to obtain Periplaneta americana coarse powder;
b. extraction: c, performing reflux extraction on the periplaneta americana coarse powder obtained in the step a for 5 times at the temperature of 75 ℃, and adding 95% ethanol with the concentration being 8 times of the weight of the coarse powder during the first extraction, wherein the extraction time is 4 hours; adding 95% ethanol 4 times the weight of the coarse powder for 4 hr each time; in the extraction process, the temperature of the ethanol is kept at 75 ℃, after the extraction is finished, the extracting solutions are combined and filtered to obtain an ethanol extract;
c. primary concentration: c, concentrating the ethanol extract obtained in the step b under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa until the specific gravity is 1.15 to obtain an ethanol concentrated solution;
d. degreasing and adsorbing: adding distilled water which is 10 times of the weight of the ethanol concentrated solution into the ethanol concentrated solution obtained in the step c, heating to 85 ℃ while stirring, stirring for 30 minutes at the stirring speed of 30 revolutions per minute, and then keeping the temperature and standing for 5 hours to separate oil from water; collecting lower layer water solution, filtering with filter paper, adding 1.0 times of medicinal active carbon into the filtrate, stirring at 40 deg.C for 60 min for full adsorption;
e. and (3) elution: d, filling the liquid medicine containing the activated carbon obtained in the step d into a chromatographic column, discharging the liquid medicine, washing the liquid medicine with distilled water 20 times of the amount of the medicinal activated carbon, and collecting and uniformly mixing the liquid medicine and the washing liquid;
f. membrane separation: under the pressure of 120kPa, collecting the liquid medicine and the water washing liquid which are uniformly mixed in the step e, passing through an ultrafiltration ceramic membrane with the molecular cut-off value of 50kD, discarding the cut-off liquid, and collecting penetrating fluid;
g. secondary concentration: concentrating the penetrating fluid obtained in the step f under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa to 1/20 of the original volume;
h. ion exchange: taking the secondary concentrated solution obtained in the step g, regulating the pH value of the concentrated penetrating fluid obtained in the step g to be 6.0 by using hydrochloric acid with the concentration of 1mol/L and sodium hydroxide with the concentration of 1mol/L, then passing through a regenerated sodium type HD-8 strong-acid styrene type cation exchange resin column, washing the sodium type HD-8 strong-acid styrene type cation exchange resin with deionized water with the volume of 3 times of the amount of the sodium type HD-8 strong-acid styrene type cation exchange resin after the adsorption of the sodium type HD-8 strong-acid styrene type cation exchange resin column is finished, then eluting by using ammonia water with the concentration of 1-3mol/L, wherein the using amount of the ammonia water with the concentration of 1.5mol/L is 6 times of the amount of the sodium type HD-8 strong-acid styrene type cation exchange resin, controlling the flow rate of the eluent to ensure that the time of the whole elution process is 10 hours, and collecting the eluent.
i. And (3) third-stage concentration: and (5) concentrating the eluent obtained in the step h under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa to obtain an extract with the specific gravity of 1.28, thus obtaining the periplaneta americana refined extract.
The hair conditioner prepared in this example has the comprehensive effects shown in Table 1. The periplaneta americana refined extract prepared in the embodiment contains up to 26 pure natural small molecular amino acids, and the total amino acid content in the refined extract is up to 79.5%.
Example 6
The moistening and repairing hair conditioner containing the American cockroach refined extract comprises the following components in percentage by weight: 2% of periplaneta americana refined extract, 2% of prinsepia utilis royle oil, 15% of octadecyl trimethyl ammonium chloride, 7% of isopropyl lanolate, 3% of glycerol, 0.1% of grapefruit essence and the balance of water. The moistening and repairing hair conditioner containing the American cockroach refined extract is prepared.
The periplaneta americana extract is prepared by refining the liquid medicine and the water washing liquid discarded in the step E in the preparation process of the periplaneta americana extract disclosed in the Chinese patent 201210446628.5 according to the following process:
a. inactivation and crushing: killing fresh Periplaneta americana with 85 deg.C hot water, oven drying at 60 + -5 deg.C, pulverizing, and sieving with 24 mesh sieve to obtain Periplaneta americana coarse powder;
b. extraction: c, performing reflux extraction on the periplaneta americana coarse powder obtained in the step a for 3 times at the temperature of 80 ℃, and adding 95% ethanol in an amount which is 7 times the weight of the coarse powder during the first extraction for 6 hours; adding 95% ethanol 6 times the weight of the coarse powder for 4 hr each time; in the extraction process, the temperature of the ethanol is kept at 75 ℃, after the extraction is finished, the extracting solutions are combined and filtered to obtain an ethanol extract;
c. primary concentration: c, concentrating the ethanol extract obtained in the step b under reduced pressure under the conditions of vacuum degree of-0.06 MPa and temperature of 55 ℃ until the specific gravity is 1.05 to obtain an ethanol concentrated solution;
d. degreasing and adsorbing: adding distilled water which is 10 times of the weight of the ethanol concentrated solution into the ethanol concentrated solution obtained in the step c, heating to 85 ℃ while stirring, stirring for 40 minutes at the stirring speed of 40 revolutions per minute, and then keeping the temperature and standing for 5 hours to separate oil from water; collecting lower layer water solution, filtering with filter paper, adding ethanol concentrated solution into the filtrate, and stirring with 0 times of medicinal active carbon at 45 deg.C for 40 min for full adsorption;
e. and (3) elution: d, filling the liquid medicine containing the activated carbon obtained in the step d into a chromatographic column, discharging the liquid medicine, washing the liquid medicine with distilled water 15 times of the medicinal activated carbon, and collecting and uniformly mixing the liquid medicine and the washing liquid;
f. membrane separation: passing through ultrafiltration ceramic membrane with molecular cut-off of 50kD under 80kPa, discarding the cut-off solution, and collecting the penetrating fluid.
g. Secondary concentration: and f, concentrating the penetrating fluid obtained in the step f under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa to 1/20 of the original volume.
h. Ion exchange: taking the secondary concentrated solution obtained in the step g, regulating the pH value of the concentrated penetrating fluid obtained in the step g to be 6.0 by using hydrochloric acid with the concentration of 1mol/L and sodium hydroxide with the concentration of 1mol/L, then passing through a regenerated sodium type HD-8 strong-acid styrene type cation exchange resin column, washing the sodium type HD-8 strong-acid styrene type cation exchange resin with deionized water with the volume of 3 times of the amount of the sodium type HD-8 strong-acid styrene type cation exchange resin after the adsorption of the sodium type HD-8 strong-acid styrene type cation exchange resin column is finished, then eluting by using ammonia water with the concentration of 1-3mol/L, wherein the using amount of the ammonia water with the concentration of 1.5mol/L is 6 times of the amount of the sodium type HD-8 strong-acid styrene type cation exchange resin, controlling the flow rate of the eluent to ensure that the time of the whole elution process is 10 hours, and collecting the eluent.
i. And (3) third-stage concentration: and (5) concentrating the eluent obtained in the step h under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa to obtain an extract with the specific gravity of 1.30, thus obtaining the periplaneta americana refined extract.
The hair conditioner prepared in this example has the comprehensive effects shown in Table 1. The periplaneta americana refined extract prepared in the embodiment contains up to 26 pure natural small molecular amino acids, and the total amino acid content in the refined extract is up to 79.2%.
Example 7
The moistening and repairing hair conditioner containing the American cockroach refined extract comprises the following components in percentage by weight: periplaneta americana extract 4%, Prinsepia utilis oil 5%, octadecyl trimethyl ammonium chloride 18%, isopropyl lanolate 6%, glycerol 2.5%, tea flower essence 0.15%, and water in balance. The moistening and repairing hair conditioner containing the American cockroach refined extract is prepared.
The periplaneta americana extract is prepared by refining the liquid medicine and the water washing liquid discarded in the step E in the preparation process of the periplaneta americana extract disclosed in the Chinese patent 201210446628.5 according to the following process:
a. inactivation and crushing: killing fresh Periplaneta americana with 85 deg.C hot water, oven drying at 60 + -5 deg.C, pulverizing, and sieving with 24 mesh sieve to obtain Periplaneta americana coarse powder;
b. extraction: c, performing reflux extraction on the periplaneta americana coarse powder obtained in the step a for 3 times at the temperature of 80 ℃, and adding 95% ethanol in an amount which is 7 times the weight of the coarse powder during the first extraction for 6 hours; adding 95% ethanol 6 times the weight of the coarse powder for 4 hr each time; in the extraction process, the temperature of the ethanol is kept at 75 ℃, after the extraction is finished, the extracting solutions are combined and filtered to obtain an ethanol extract;
c. primary concentration: c, concentrating the ethanol extract obtained in the step b under reduced pressure under the conditions of vacuum degree of-0.06 MPa and temperature of 55 ℃ until the specific gravity is 1.05 to obtain an ethanol concentrated solution;
d. degreasing and adsorbing: adding distilled water which is 10 times of the weight of the ethanol concentrated solution into the ethanol concentrated solution obtained in the step c, heating to 85 ℃ while stirring, stirring for 40 minutes at the stirring speed of 40 revolutions per minute, and then keeping the temperature and standing for 5 hours to separate oil from water; collecting lower layer water solution, filtering with filter paper, adding ethanol concentrated solution into the filtrate, and stirring with 0 times of medicinal active carbon at 45 deg.C for 40 min for full adsorption;
e. and (3) elution: d, filling the liquid medicine containing the activated carbon obtained in the step d into a chromatographic column, discharging the liquid medicine, washing the liquid medicine with distilled water 15 times of the medicinal activated carbon, and collecting and uniformly mixing the liquid medicine and the washing liquid;
f. membrane separation: passing through ultrafiltration ceramic membrane with molecular cut-off of 50kD under 80kPa, discarding the cut-off solution, and collecting the penetrating fluid.
g. Secondary concentration: and f, concentrating the penetrating fluid obtained in the step f under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa to 1/20 of the original volume.
h. Ion exchange: taking the secondary concentrated solution obtained in the step g, regulating the pH value of the concentrated penetrating fluid obtained in the step g to be 6.0 by using hydrochloric acid with the concentration of 1mol/L and sodium hydroxide with the concentration of 1mol/L, then passing through a regenerated sodium type HD-8 strong-acid styrene type cation exchange resin column, washing the sodium type HD-8 strong-acid styrene type cation exchange resin with deionized water with the volume of 3 times of the amount of the sodium type HD-8 strong-acid styrene type cation exchange resin after the adsorption of the sodium type HD-8 strong-acid styrene type cation exchange resin column is finished, then eluting by using ammonia water with the concentration of 1-3mol/L, wherein the using amount of the ammonia water with the concentration of 1.5mol/L is 6 times of the amount of the sodium type HD-8 strong-acid styrene type cation exchange resin, controlling the flow rate of the eluent to ensure that the time of the whole elution process is 10 hours, and collecting the eluent.
i. And (3) third-stage concentration: and (5) concentrating the eluent obtained in the step h under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa to obtain an extract with the specific gravity of 1.30, thus obtaining the periplaneta americana refined extract.
The hair conditioner prepared in this example has the comprehensive effects shown in Table 1. The periplaneta americana refined extract prepared in the embodiment contains up to 26 pure natural small molecular amino acids, and the total amino acid content in the refined extract is up to 79.3%.
Examination of comprehensive effects of Hair conditioner
The efficacy of the conditioners manufactured in examples 1 to 7 was evaluated by the use of a feeling of trial. 80 persons of 25 to 65 years old are selected as trial objects by adopting a civil survey grading method, are randomly and equally divided into six groups, and are respectively treated by the hair conditioner prepared in the embodiment 1 to 7. The hair is washed twice a week and then is nursed for two months. The using effects of the ingredients are divided into 5 points: a score of 5 is the highest score, indicating very good, very satisfactory; 4, the classification is very good; 3 is acceptable; when the amount is less than 3 points, the results are not acceptable. The average scores for each are as follows, and the results are shown in table 1:
Figure 542309DEST_PATH_IMAGE002
in conclusion, the hair conditioner is fine, smooth, fine in nourishment, moisture retention and repair, smooth in use, and good in wet combing property and dry combing property.
The above is only a preferred embodiment of the present invention, and it should be noted that the above preferred embodiment should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and these modifications and adaptations should be considered within the scope of the invention.

Claims (2)

1. A moistening and repairing hair conditioner containing periplaneta americana refined extract is characterized by comprising the following components in percentage by weight:
1.5-3.2% of periplaneta americana refined extract, 1.5-3.2% of prinsepia utilis royle oil, 12-17% of octadecyl trimethyl ammonium chloride, 5-8% of isopropyl lanolate, 2.5-4% of glycerol, 0.08-0.2% of essence and the balance of water;
prepared by the following process:
s1, weighing the components of the skin cream according to the parts by weight;
s2, adding water into a pot, heating to 60-70 ℃, adding octadecyl trimethyl ammonium chloride, isopropyl lanolate and glycerol, and uniformly stirring;
s3, cooling the liquid in the pot to 30-40 ℃, adding the periplaneta americana extract, the prinsepia utilis royle oil and the essence, homogenizing at a high speed and stirring for 5-20 minutes, and cooling to obtain the feed additive;
the periplaneta americana extract is prepared by refining the liquid medicine and the water washing liquid discarded in the step E in the preparation process of the periplaneta americana extract disclosed in the Chinese patent 201210446628.5 according to the following process:
a. inactivation and crushing: killing the fresh American cockroach by hot water at 80-90 ℃, controlling the temperature within 60 +/-5 ℃ for drying, crushing, and sieving by a 24-mesh sieve to prepare coarse American cockroach powder;
b. extraction: c, performing 3-5 times of reflux extraction on the periplaneta americana coarse powder obtained in the step a at the temperature of 75-80 ℃, and adding 90-95% ethanol in an amount which is 5-8 times the weight of the coarse powder during the first extraction for 4-6 hours; adding 90-95% ethanol in an amount which is 3-6 times the weight of the coarse powder every time after the second time, wherein the extraction time is 3-5 hours; in the extraction process, the temperature of ethanol is kept at 75-80 ℃, after extraction is finished, the extracting solutions are combined and filtered to obtain an ethanol extracting solution;
c. primary concentration: c, concentrating the ethanol extract obtained in the step b under reduced pressure under the conditions of vacuum degree of-0.05 to-0.06 MPa and temperature of 50 to 60 ℃ until the specific gravity is 1.05 to 1.15 to obtain an ethanol concentrated solution;
d. degreasing and adsorbing: adding distilled water which is 7-10 times of the weight of the ethanol concentrated solution into the ethanol concentrated solution obtained in the step c, heating to 80-90 ℃ while stirring, stirring for 10-60 minutes at a stirring speed of 20-60 revolutions per minute, and then keeping the temperature and standing for 1-5 hours to separate oil from water; collecting the lower-layer water solution, filtering the lower-layer water solution by using filter paper, adding medicinal active carbon which is 0.5 to 1.0 time of the ethanol concentrated solution into the obtained filtrate, and stirring the mixture at the temperature of between 40 and 60 ℃ for 30 to 60 minutes to ensure that the mixture is fully adsorbed;
e. and (3) elution: d, filling the activated carbon-containing liquid medicine obtained in the step d into a chromatographic column, discharging the liquid medicine, washing with distilled water 10-30 times of the amount of the medicinal activated carbon, and collecting and uniformly mixing the liquid medicine and the washing liquid;
f. membrane separation: under the pressure of 80kPa, collecting the liquid medicine and the water washing liquid which are uniformly mixed in the step e, passing through an ultrafiltration ceramic membrane with the molecular cut-off value of 50kD, discarding the cut-off liquid, and collecting penetrating fluid;
g. secondary concentration: concentrating the penetrating fluid obtained in the step f under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa to 1/20 of the original volume
h. Ion exchange: taking the secondary concentrated solution obtained in the step g, regulating the pH value of the concentrated penetrating fluid obtained in the step g to be 6.0 by using hydrochloric acid with the concentration of 1mol/L and sodium hydroxide with the concentration of 1mol/L, then passing through a regenerated sodium type HD-8 strong-acid styrene type cation exchange resin column, washing the sodium type HD-8 strong-acid styrene type cation exchange resin with deionized water with the volume of 3 times of the amount of the sodium type HD-8 strong-acid styrene type cation exchange resin after the adsorption of the sodium type HD-8 strong-acid styrene type cation exchange resin column is finished, then eluting by using ammonia water with the concentration of 1-3mol/L, wherein the using amount of the ammonia water with the concentration of 1.5mol/L is 6 times of the amount of the sodium type HD-8 strong-acid styrene type cation exchange resin, controlling the flow rate of the eluent to ensure that the time of the whole elution process is 10 hours, and collecting the eluent;
i. and (3) third-stage concentration: and (5) concentrating the eluent obtained in the step h under reduced pressure at the temperature of 50-60 ℃ and the vacuum degree of-0.05-0.06 MPa to obtain an extract with the specific gravity of 1.20-1.30, thus obtaining the periplaneta americana refined extract.
2. The moistening and repairing hair conditioner containing periplaneta americana essence according to claim 1, wherein the essence is one or a mixture of more of pomegranate essence, tea plant essence and grapefruit essence.
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