CN109938054B - Preparation method of spray for resisting indoor dust mite allergens Der p1 and Der f1 - Google Patents
Preparation method of spray for resisting indoor dust mite allergens Der p1 and Der f1 Download PDFInfo
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Abstract
The invention discloses a preparation method of an indoor dust mite allergen Der p1 and Der f1 resisting spray, which comprises the following steps: pretreating bamboo chips and cinnamomum camphora leaves, and respectively pulverizing into powder by a pulverizer for later use; carrying out chemical degumming treatment on the bamboo chip powder, separating to obtain a bamboo fiber extract, weighing a certain amount of camphor leaf powder, placing in a distillation flask, uniformly dispersing, and distilling under reduced pressure; then removing chlorophyll; carrying out primary separation on the crude product by a chromatography method to obtain a crude product; refining by liquid chromatography to obtain high-purity pure natural plant extract; recrystallizing and purifying the bamboo fiber to obtain white powder; the two effective components are uniformly mixed with a buffering agent, a surfactant, a quick-drying agent and a solvent according to certain mass percentage to prepare the dust mite anti-allergic spray. The preparation process is simple and easy to operate, has low cost, has good anti-allergic effect on household dust mites, and has no side effect on human bodies, so the preparation method has wide application market in the field of indoor dust mite allergic protein modification.
Description
Technical Field
The invention belongs to the field of modification of indoor dust mite allergens, and particularly relates to a preparation method of an indoor dust mite allergen Der p1 and Der f1 resisting spray.
Background
Dust Mites (House Dust Mites) are an important allergen widely existing in human life and working environments, the body size of Mites is only about 0.5-0.1 mm, and mite bodies, mite eggs, excrement, dead mite bodies and the like which are difficult to see by naked eyes of people can become allergens to cause various allergic diseases such as allergic asthma, allergic rhinitis, dermatitis and the like. At present, more than 800 million allergic asthma patients in children in China exist, wherein the number of asthma cases accounts for 80%. The research finds that the number of allergenic proteins in the dust mites is more than 20, and the household/house dust mites (Der p) and the dust mites (Der f) are the two most common dominant lethal mites, have strong vitality and are hidden in the living environment of people for a long time. It is statistical that western countries have 90% of their time in indoor environments and 50% of their time indoors, and the problem of dust mite allergy is increasingly appreciated.
Dust mites mainly feed on animal skin dust, and since one person can produce 0.5-1.0 g of skin dust per day, the dust mites are not limiting factors for the breeding of dust mites, and humidity and ambient temperature are main factors for the proliferation of dust mites. The dust mites do not resist high temperature, generally propagate and survive in an environment lower than 35 ℃, have strong low temperature resistance, and have high propagation speed when the Relative Humidity (RH) is 70-80%. Dust mites often grow in furnishings such as carpets, sofas, mattresses, bedding and the like, but the level of dust mite allergens in the room cannot be effectively reduced by simply changing the indoor furnishings. The airing mode is the most common mite removing mode, but the effect is slow, and mite sources hidden in bedding, carpets, pillow cores, mattresses and the like are difficult to thoroughly clean and easy to repeat. There have been reported a freezing method (freezing objects such as blankets, toys, pillow cases, etc. using a refrigerator or liquid nitrogen), a dry heating method (electric blanket or other heating methods), a steam mite killing method, chemical mite killing using lindane, benzyl toluate, etc., and physical methods such as "ultraviolet irradiation", "strong beating", etc., which cannot achieve the intended effect or have a great disadvantage in home promotion.
Therefore, the method which has simple preparation process, easy operation, low cost, good anti-allergic effect of the dust mites, no side effect on human bodies and is popular with the people is found, and the method has important significance for the happy and healthy life of people.
Disclosure of Invention
Aiming at the defects of the prior art, the invention takes natural bamboo chips and cinnamomum camphora leaves as raw materials of anti-allergic active ingredients of the indoor dust mites, adopts a pure natural plant extraction method, and simply and quickly prepares the anti-allergic spray for the indoor dust mites.
The invention relates to a preparation method of a spray for resisting indoor dust mite allergens Der p1 and Der f1, which mainly comprises the following steps:
(1) pretreating bamboo chips and cinnamomum camphora leaves, and respectively processing the bamboo chips and the cinnamomum camphora leaves by a pulverizer to obtain powder for later use;
(2) weighing the bamboo chip powder in the step (1), carrying out chemical degumming treatment, and separating to obtain a bamboo fiber extract;
(3) weighing the camphor leaf powder (1), placing the camphor leaf powder in a distillation flask, adding an organic solvent according to a certain liquid-material ratio, and uniformly dispersing and dissolving the camphor leaf powder in a certain manner;
(4) distilling the solution (3) under reduced pressure for a period of time at a certain temperature, collecting distillate, and extracting for 3-5 times by using an organic reagent to obtain a camphor essential oil concentrated solution;
(5) respectively carrying out chlorophyll removal treatment on the bamboo fiber extract and the camphor essential oil concentrated solution in the steps (2) and (4) by adopting an organic reagent;
(6) preliminarily separating the two concentrated solutions by chromatography to respectively obtain crude products;
(7) refining by preparative liquid chromatography to obtain high-purity pure natural plant extracts;
(8) recrystallizing and purifying the bamboo fiber (7) at a certain temperature to obtain white powder;
(9) mixing the two effective components with a buffering agent, a surfactant, a quick-drying agent and a solvent according to a certain mass ratio to prepare the anti-allergic spray for house dust mites.
The preparation method of the spray for resisting indoor dust mite allergens Der p1 and Der f1 is characterized by comprising the following steps: the pretreatment in the step (1) is carried out by washing for 3-10 times, drying for 1-48 h at 40-120 ℃, preferably washing for 3-5 times, and drying for 5-7 h at 70-120 ℃.
The preparation method of the spray for resisting indoor dust mite allergens Der p1 and Der f1 is characterized by comprising the following steps: the chemical degumming treatment in the step (2) is that 4-12 g/L NaOH is used as a refining agent and 3g/L Na2SiO3And (3) as a boiling auxiliary agent, performing an alkali boiling process at a reaction temperature of 80-130 ℃, a reaction time of 90-150 min and a bath ratio of 1:25, preferably selecting 5-9 g/L NaOH, and performing a reaction at a reaction temperature of 90-105 ℃ for 110-130 min.
The preparation method of the spray for resisting indoor dust mite allergens Der p1 and Der f1 is characterized by comprising the following steps: in the step (3), the organic solvent is absolute ethyl alcohol, the material-liquid ratio is 15: 1-8: 1, and the certain mode is high-speed stirring, ultrasonic dispersion, grinding dispersion or ball milling dispersion, preferably the material-liquid ratio is 10:1, and the high-speed stirring is carried out to ensure that the organic solvent is uniformly dispersed.
The preparation method of the spray for resisting indoor dust mite allergens Der p1 and Der f1 is characterized by comprising the following steps: the certain temperature in the step (4) is 40-90 ℃, the extraction time is 50-100 min, the extraction reagent is petroleum ether, and the preferred extraction temperature is 40 ℃, 50 ℃, 60 ℃, 70 ℃ and 80 ℃, and the extraction time is 65-75 min.
The preparation method of the spray for resisting indoor dust mite allergens Der p1 and Der f1 is characterized by comprising the following steps: in the step (5), the organic reagent is n-hexane.
The preparation method of the spray for resisting indoor dust mite allergens Der p1 and Der f1 is characterized by comprising the following steps: the chromatography in step (6) is silica gel column chromatography, and the eluent is one or more of ethyl acetate, petroleum ether, methanol, chloroform, n-butanol, n-hexane, dichloroethane, acetone, and ethanol, preferably ethyl acetate, petroleum ether, and n-hexane.
The preparation method of the spray for resisting indoor dust mite allergens Der p1 and Der f1 is characterized by comprising the following steps: in the liquid chromatography in the step (7), the stationary phase is one of silica gel with a cyano functional group bonded on the surface, silica gel with an amino functional group bonded on the surface and silica gel with an octadecyl functional group bonded on the surface; the mobile phase is one or more of ethyl acetate, petroleum ether, methanol, chloroform, n-butanol, n-hexane, dichloroethane, acetone and ethanol; the pH value of the mobile phase is controlled to be 2-8, the preferable mobile phase is ethyl acetate, petroleum ether and n-hexane, and the pH value of the mobile phase is controlled to be 4-6.
The preparation method of the spray for resisting indoor dust mite allergens Der p1 and Der f1 is characterized by comprising the following steps: and (3) recrystallizing in the step (8), wherein the selected solvent is one or more of water, methanol, ethanol, isopropanol, acetone, ethyl acetate, chloroform, glacial acetic acid, dioxane, carbon tetrachloride, benzene, petroleum ether, toluene, nitromethane, diethyl ether, dimethylformamide and dimethyl sulfoxide, and preferably the solvents of ethyl acetate and petroleum ether.
The preparation method of the spray for resisting indoor dust mite allergens Der p1 and Der f1 is characterized by comprising the following steps: the buffer in the step (9) is an acid-base buffer, and refers to one or more of citric acid/citrate, ammonium salt, acetate, sodium dihydrogen phosphate and various biological buffers, and preferably citric acid/citrate and sodium dihydrogen phosphate.
The preparation method of the spray for resisting indoor dust mite allergens Der p1 and Der f1 is characterized by comprising the following steps: the surfactant in the step (9) is a polyethylene type nonionic surfactant, such as didecyl dimethyl ammonium chloride, sodium dodecyl benzene sulfonate, dodecyl trimethyl ammonium chloride, and the like, preferably didecyl dimethyl ammonium chloride, sodium dodecyl benzene sulfonate, dodecyl trimethyl ammonium chloride.
The preparation method of the spray for resisting indoor dust mite allergens Der p1 and Der f1 is characterized by comprising the following steps: and (4) the quick drying agent in the step (9) is absolute ethyl alcohol.
The preparation method of the spray for resisting indoor dust mite allergens Der p1 and Der f1 is characterized by comprising the following steps: and (4) in the step (9), the solvent is deionized water.
The preparation method of the spray for resisting indoor dust mite allergens Der p1 and Der f1 is characterized by comprising the following steps: in the step (9), the certain mass ratio is 1-10% of effective component bamboo fiber, 1-10% of effective component camphor essential oil, 0.01-5% of buffering agent, 0.01-6% of surfactant, 1-15% of quick-drying agent and 50-95% of solvent, preferably 4-7% of effective component bamboo fiber, 1-4% of effective component camphor essential oil, 0.05-0.4% of buffering agent, 0.1-4% of surfactant, 7-10% of quick-drying agent and 70-90% of solvent.
The preparation method disclosed by the invention is simple and easy to operate, low in cost, good in anti-allergic effect of indoor dust mites and free of any side effect on human bodies, so that the preparation method has a wide application market in the field of indoor dust mite allergic protein modification.
Drawings
FIG. 1 is a graph showing the effect of reducing dust mite allergen protein Der p1 in the chamber according to examples 1 to 5 of the present invention;
FIG. 2 is a graph showing the effect of examples 1 to 5 of the present invention on reduction of house dust mite allergen protein Der f 1;
FIG. 3 is a graph showing the effect of reducing the allergen protein Der p1 acting on household blankets according to examples 1 to 5 of the present invention;
FIG. 4 is a graph showing the effect of reducing the allergen protein Der f1 acting on the household blanket according to examples 1 to 5 of the present invention;
FIG. 5 is a graph showing the effect of example 1 of the present invention on the reduction of the indoor dust mite allergen protein Der p1 with time;
FIG. 6 is a graph showing the effect of example 1 of the present invention on the reduction of house dust mite allergen protein Der f1 with time.
Detailed Description
The method of the present invention will be described in detail with reference to specific examples, which are carried out on the premise of the technical solution of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
Washing bamboo strips with length of about 6cm and width of about 2cm and 10g of Cinnamomum camphora leaf with deionized water for 3 times, placing in oven at 120 deg.C for 5 hr, oven drying, and pulverizing into powder with pulverizer. Boiling the bamboo chip powder in NaOH boiling liquid, wherein the concentration of NaOH is 5g/L, and the boiling auxiliary agent is 3g/L Na2SiO3The bath ratio is 1:25, the reaction temperature is 100 ℃, the reaction time is 110min, and after alkali boiling is finished, the bamboo fiber extracting solution is obtained by filtration and separation for later use. Weighing 6g of crushed camphor leaves, putting the crushed camphor leaves into a three-necked flask, selecting an absolute ethyl alcohol organic solvent, controlling the material-liquid ratio to be 10:1, extracting at 50 ℃, reacting for 75min, and extracting distillate for 3 times by using organic reagent petroleum ether to obtain camphor essential oil concentrated solution. Removing chlorophyll from the bamboo fiber extract and the camphor essential oil concentrate with organic reagent n-hexane, subjecting the two concentrates to silica gel column chromatography with ethyl acetate as eluent, primarily separating to obtain crude products, refining by liquid chromatography to obtain high-purity extracts, recrystallizing the bamboo fiber concentrate, and purifyingWhite powder can be obtained. Mixing and stirring 5% of active ingredient bamboo fibril, 2% of active ingredient cinnamomum camphora essential oil, 0.3% of citric acid/sodium citrate, 0.2% of didecyl dimethyl ammonium chloride, 5% of absolute ethyl alcohol, 87.5% of deionized water and pH of 5.93 for 30min according to the mass ratio to obtain the indoor dust mite anti-allergy spray solvent.
The anti-allergic spray prepared in the example, and indoor dust mite allergen protein extracts Der p1 and Der f1 were mixed at a volume ratio of 1:9 for 30min, and then tested, the activity reduction rates of the corresponding allergen proteins were 90.3% and 88.5%, respectively. The same test method was used on blankets in homes, and the corresponding allergen protein activity reduction rates were 82.7% and 77.1%, respectively.
Example 2
Washing bamboo strips with length of about 6cm and width of about 2cm and 10g of Cinnamomum camphora leaf with deionized water for 3 times, placing in oven at 120 deg.C for 5 hr, oven drying, and pulverizing into powder with pulverizer. Boiling the bamboo chip powder in NaOH boiling liquid, wherein the concentration of NaOH is 5g/L, and the boiling auxiliary agent is 3g/L Na2SiO3The bath ratio is 1:25, the reaction temperature is 100 ℃, the reaction time is 110min, and after alkali boiling is finished, the bamboo fiber extracting solution is obtained by filtration and separation for later use. Weighing 6g of crushed camphor leaves, putting the crushed camphor leaves into a three-necked flask, selecting an absolute ethyl alcohol organic solvent, controlling the material-liquid ratio to be 10:1, extracting at 50 ℃, reacting for 75min, and extracting distillate for 3 times by using organic reagent petroleum ether to obtain camphor essential oil concentrated solution. And then carrying out chlorophyll removal treatment on the bamboo fiber extract and the camphor essential oil concentrated solution by using an organic reagent n-hexane, then carrying out silica gel column chromatography by using ethyl acetate as an eluent, carrying out primary separation on the two concentrated solutions to respectively obtain crude products, finally refining by using liquid chromatography to respectively obtain high-purity extracts, and recrystallizing and purifying the bamboo fiber concentrated solution to obtain white powder. Mixing and stirring 2% of bamboo fibril serving as an effective component, 2% of camphor essential oil serving as an effective component, 0.3% of citric acid/sodium citrate, 0.2% of didecyl dimethyl ammonium chloride, 5% of absolute ethyl alcohol, 90.5% of deionized water and pH of 7.98 for 30min according to the mass ratio to obtain the indoor dust mite anti-allergy spraying agentAnd (4) atomizing the solvent.
The anti-allergic spray prepared in the example, and indoor dust mite allergen protein extracts Der p1 and Der f1 were mixed at a volume ratio of 1:9 for 30min, and then tested, the activity reduction rates of the corresponding allergen proteins were 45.5% and 50.2%, respectively. The same test method was used on blankets in homes, with the corresponding allergen protein activity reduction rates of 42.6% and 45.3%, respectively.
Example 3
Washing bamboo strips with length of about 6cm and width of about 2cm and 10g of Cinnamomum camphora leaf with deionized water for 3 times, placing in oven at 120 deg.C for 5 hr, oven drying, and pulverizing into powder with pulverizer. Boiling the bamboo chip powder in NaOH boiling liquid, wherein the concentration of NaOH is 5g/L, and the boiling auxiliary agent is 3g/L Na2SiO3The bath ratio is 1:25, the reaction temperature is 100 ℃, the reaction time is 110min, and after alkali boiling is finished, the bamboo fiber extracting solution is obtained by filtration and separation for later use. Weighing 6g of crushed camphor leaves, putting the crushed camphor leaves into a three-necked flask, selecting an absolute ethyl alcohol organic solvent, controlling the material-liquid ratio to be 10:1, extracting at 50 ℃, reacting for 75min, and extracting distillate for 3 times by using organic reagent petroleum ether to obtain camphor essential oil concentrated solution. And then carrying out chlorophyll removal treatment on the bamboo fiber extract and the camphor essential oil concentrated solution by using an organic reagent n-hexane, then carrying out silica gel column chromatography by using ethyl acetate as an eluent, carrying out primary separation on the two concentrated solutions to respectively obtain crude products, finally refining by using liquid chromatography to respectively obtain high-purity extracts, and recrystallizing and purifying the bamboo fiber concentrated solution to obtain white powder. Mixing and stirring 5% of active ingredient bamboo fibril, 2% of active ingredient cinnamomum camphora essential oil, 0.8% of citric acid/sodium citrate, 0.2% of didecyl dimethyl ammonium chloride, 5% of absolute ethyl alcohol and 87% of deionized water according to the mass ratio, wherein the pH value is 3.92, and stirring for 30min to obtain the indoor dust mite anti-allergy spray solvent.
The anti-allergic spray prepared in the example, and indoor dust mite allergen protein extracts Der p1 and Der f1 were mixed at a volume ratio of 1:9 for 30min, and then tested, the activity reduction rates of the corresponding allergen proteins were 76.2% and 70.4%, respectively. The same test method was used on blankets in homes, and the corresponding allergen protein activity reduction rates were 60.6% and 53.3%, respectively.
Example 4
Washing bamboo strips with length of about 6cm and width of about 2cm and 10g of Cinnamomum camphora leaf with deionized water for 3 times, placing in oven at 120 deg.C for 5 hr, oven drying, and pulverizing into powder with pulverizer. Boiling the bamboo chip powder in NaOH boiling liquid, wherein the concentration of NaOH is 5g/L, and the boiling auxiliary agent is 3g/L Na2SiO3The bath ratio is 1:25, the reaction temperature is 100 ℃, the reaction time is 110min, and after alkali boiling is finished, the bamboo fiber extracting solution is obtained by filtration and separation for later use. Weighing 6g of crushed camphor leaves, putting the crushed camphor leaves into a three-necked flask, selecting an absolute ethyl alcohol organic solvent, controlling the material-liquid ratio to be 10:1, extracting at 50 ℃, reacting for 75min, and extracting distillate for 3 times by using organic reagent petroleum ether to obtain camphor essential oil concentrated solution. And then carrying out chlorophyll removal treatment on the bamboo fiber extract and the camphor essential oil concentrated solution by using an organic reagent n-hexane, then carrying out silica gel column chromatography by using ethyl acetate as an eluent, carrying out primary separation on the two concentrated solutions to respectively obtain crude products, finally refining by using liquid chromatography to respectively obtain high-purity extracts, and recrystallizing and purifying the bamboo fiber concentrated solution to obtain white powder. Mixing and stirring 2% of bamboo fibril serving as an effective component, 2% of camphor essential oil serving as an effective component, 0.8% of citric acid/sodium citrate, 0.2% of didecyl dimethyl ammonium chloride, 5% of absolute ethyl alcohol, 90% of deionized water and pH 6.03 for 30min according to the mass ratio to obtain the indoor dust mite anti-allergy spray solvent.
The anti-allergic spray prepared in the example, and indoor dust mite allergen protein extracts Der p1 and Der f1 were mixed at a volume ratio of 1:9 for 30min, and then tested, the activity reduction rates of the corresponding allergen proteins were 80.1% and 82.3%, respectively. The same test method was used on blankets in homes, and the corresponding allergen protein activity reduction rates were 69.0% and 61.1%, respectively.
Example 5
Washing bamboo strips with length of about 6cm and width of about 2cm and 10g of folium Cinnamomi Porrecti with deionized water for 3 times, respectively, and washing at 12 timesPlacing in a 0 ℃ oven for 5h, drying, and pulverizing the above materials into powder respectively with a pulverizer for later use. Boiling the bamboo chip powder in NaOH boiling liquid, wherein the concentration of NaOH is 5g/L, and the boiling auxiliary agent is 3g/L Na2SiO3The bath ratio is 1:25, the reaction temperature is 100 ℃, the reaction time is 110min, and after alkali boiling is finished, the bamboo fiber extracting solution is obtained by filtration and separation for later use. Weighing 6g of crushed camphor leaves, putting the crushed camphor leaves into a three-necked flask, selecting an absolute ethyl alcohol organic solvent, controlling the material-liquid ratio to be 10:1, extracting at 50 ℃, reacting for 75min, and extracting distillate for 3 times by using organic reagent petroleum ether to obtain camphor essential oil concentrated solution. And then carrying out chlorophyll removal treatment on the bamboo fiber extract and the camphor essential oil concentrated solution by using an organic reagent n-hexane, then carrying out silica gel column chromatography by using ethyl acetate as an eluent, carrying out primary separation on the two concentrated solutions to respectively obtain crude products, finally refining by using liquid chromatography to respectively obtain high-purity extracts, and recrystallizing and purifying the bamboo fiber concentrated solution to obtain white powder. Mixing and stirring 7% of active ingredient bamboo fibril, 2% of active ingredient cinnamomum camphora essential oil, 0.3% of citric acid/sodium citrate, 0.2% of didecyl dimethyl ammonium chloride, 5% of absolute ethyl alcohol, 85.5% of deionized water and pH 6.12 for 30min according to the mass ratio to obtain the indoor dust mite anti-allergy spray solvent.
The anti-allergic spray prepared in the example, and indoor dust mite allergen protein extracts Der p1 and Der f1 were mixed at a volume ratio of 1:9 for 30min, and then tested, the activity reduction rates of the corresponding allergen proteins were 84.0% and 89.2%, respectively. The same test method was used on blankets in homes, which corresponded to allergen protein activity reductions of 82.1% and 79.8%, respectively.
Performance testing
Test one
1ml of indoor dust mite allergen protein extracts Der p1 and Der f1 at a concentration of 6000ng/ml were mixed with a spray solvent (examples 1 to 5 antiallergic) or distilled water, respectively, at a volume ratio of 1:9, shaken for 0.5 hour, and then left to stand. By using
The activity level of house dust mite allergen protein was measured by the (Multiplex Array for indole Allergens) method, and the reduction effect of the detection agent was represented by "%". The test results are shown in the attached figures 1 and 2.
Test two
1ml of indoor dust mite allergen protein extracts Der p1 and Der f1 with a concentration of 6000ng/ml were inoculated on square short pile polyolefin carpets of about 5cm in length, respectively, left to stand for 2 hours, and dried completely. 9ml of the above spray solvent (examples 1 to 5) or distilled water was sprayed on the above-treated carpet, left to stand for 0.5 hour, and then extracted with a buffer solution (filter-sterilized 1% BSA 0.02% PBS Tween 20, pH 7.4). By using
Method the activity level of the house dust mite allergen protein is detected, and the reduction effect of the detection agent is represented by "%". The test results are shown in the attached figures 3 and 4.
Test three
1ml of indoor dust mite allergen protein extracts Der p1 and Der f1 with the concentration of 6000ng/ml are respectively mixed with the spray solvent in the embodiment 1 according to the volume ratio of 1:9, the shaking time is respectively selected from 10min, 20min, 30min, 60min, 120min and 12h, and then the mixture is kept stand. By using
The activity level of house dust mite allergen protein was measured by the (Multiplex Array for indole Allergens) method, and the reduction effect of the detection agent was represented by "%". The test results are shown in the attached figures 5 and 6.
Claims (10)
1. A preparation method of a spray for resisting indoor dust mite allergens Der p1 and Der f1 is characterized by comprising the following steps: the preparation method mainly comprises the following steps:
(1) pretreating bamboo chips and cinnamomum camphora leaves, and respectively processing the bamboo chips and the cinnamomum camphora leaves by a pulverizer to obtain powder for later use;
(2) weighing the bamboo chip powder in the step (1), carrying out chemical degumming treatment, and separating to obtain a bamboo fiber extract;
(3) weighing the camphor leaf powder (1), placing the camphor leaf powder in a distillation flask, adding an organic solvent according to a certain liquid-material ratio, and uniformly dispersing and dissolving the camphor leaf powder in a certain manner;
(4) distilling the solution (3) under reduced pressure for a period of time at a certain temperature, collecting distillate, and extracting for 3-5 times by using an organic reagent to obtain a camphor essential oil concentrated solution;
(5) respectively carrying out chlorophyll removal treatment on the bamboo fiber extract and the camphor essential oil concentrated solution in the steps (2) and (4) by adopting an organic reagent;
(6) primarily separating the bamboo fiber extract and the camphor essential oil concentrated solution by chromatography to respectively obtain crude products;
(7) refining by preparative liquid chromatography to obtain high-purity pure natural plant extracts respectively;
(8) recrystallizing and purifying the bamboo fiber (7) at a certain temperature to obtain white powder;
(9) mixing the two effective components with a buffering agent, a surfactant, a quick-drying agent and a solvent according to a certain mass ratio to prepare the anti-allergic spray for house dust mites.
2. The preparation method of the spray for resisting indoor dust mite allergens Der p1 and Der f1 according to claim 1 is characterized in that: the pretreatment in the step (1) is to carry out water washing for 3-10 times and dry for 1-48 h at 40-120 ℃.
3. The preparation method of the spray for resisting indoor dust mite allergens Der p1 and Der f1 according to claim 1 is characterized in that: the chemical degumming treatment in the step (2) is an alkali boiling process which is carried out at the reaction temperature of 80-130 ℃, the reaction time of 90-150 min and the bath ratio of 1:25 by taking 4-12 g/L NaOH as a refining agent and 3g/L Na2SiO3 as a boiling auxiliary agent.
4. The preparation method of the spray for resisting indoor dust mite allergens Der p1 and Der f1 according to claim 1 is characterized in that: in the step (3), the organic solvent is absolute ethyl alcohol, the material-liquid ratio is 15: 1-8: 1, and the organic solvent is dispersed by high-speed stirring, ultrasonic dispersion, grinding dispersion or ball milling dispersion in a certain mode.
5. The preparation method of the spray for resisting indoor dust mite allergens Der p1 and Der f1 according to claim 1 is characterized in that: the certain temperature in the step (4) is 40-90 ℃, the extraction time is 50-100 min, and the extraction reagent is petroleum ether.
6. The preparation method of the spray for resisting indoor dust mite allergens Der p1 and Der f1 according to claim 1 is characterized in that: in the step (5), the organic reagent is n-hexane.
7. The preparation method of the spray for resisting indoor dust mite allergens Der p1 and Der f1 according to claim 1 is characterized in that: the chromatography in the step (6) is silica gel column chromatography, and the eluent is one or more of ethyl acetate, petroleum ether, methanol, chloroform, n-butanol, n-hexane, dichloroethane, acetone and ethanol.
8. The preparation method of the spray for resisting indoor dust mite allergens Der p1 and Der f1 according to claim 1 is characterized in that: in the liquid chromatography in the step (7), the stationary phase is one of silica gel with a cyano functional group bonded on the surface, silica gel with an amino functional group bonded on the surface and silica gel with an octadecyl functional group bonded on the surface; the mobile phase is one or more of ethyl acetate, petroleum ether, methanol, chloroform, n-butanol, n-hexane, dichloroethane, acetone and ethanol; the pH value of the mobile phase is controlled to be 2-8.
9. The preparation method of the spray for resisting indoor dust mite allergens Der p1 and Der f1 according to claim 1 is characterized in that: and (3) recrystallizing in one or more solvents selected from water, methanol, ethanol, isopropanol, acetone, ethyl acetate, chloroform, glacial acetic acid, dioxane, carbon tetrachloride, benzene, petroleum ether, toluene, nitromethane, diethyl ether, dimethylformamide and dimethyl sulfoxide in the step (8).
10. The preparation method of the spray for resisting indoor dust mite allergens Der p1 and Der f1 according to claim 1 is characterized in that: the buffering agent in the step (9) is an acid-base buffering agent, and refers to one or more of citric acid/citrate, ammonium salt, acetate, sodium dihydrogen phosphate and various biological buffering agents; the surfactant is didecyl dimethyl ammonium chloride, sodium dodecyl benzene sulfonate and dodecyl trimethyl ammonium chloride; the quick-drying agent is absolute ethyl alcohol; the solvent is deionized water; the certain mass ratio is 1-10% of effective component bamboo fibril, 1-10% of effective component camphor essential oil, 0.01-5% of buffering agent, 0.01-6% of surfactant, 1-15% of quick-drying agent and 50-95% of solvent.
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