CN110917232A - Method for applying medical natural product targeted medicine of dandelion extracted by hydrothermal method to mainly treat dermatitis allergy - Google Patents
Method for applying medical natural product targeted medicine of dandelion extracted by hydrothermal method to mainly treat dermatitis allergy Download PDFInfo
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- CN110917232A CN110917232A CN201911254090.6A CN201911254090A CN110917232A CN 110917232 A CN110917232 A CN 110917232A CN 201911254090 A CN201911254090 A CN 201911254090A CN 110917232 A CN110917232 A CN 110917232A
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- dandelion
- sodium
- solution
- temperature
- hydrothermal
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- 239000000284 extract Substances 0.000 claims description 34
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- 235000020691 dandelion extract Nutrition 0.000 claims description 28
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
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- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 6
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- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 4
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Abstract
The invention discloses a method for extracting medical natural product targeted drugs of dandelion by a hydrothermal method and applying the medical natural product targeted drugs to mainly treat dermatitis allergy, which is a method for efficiently extracting natural product active substances of chlorogenic acid, luteolin 7-O-glucoside, caffeic acid, quercetin glucoside, dandelion glue- β -D-glucoside, tranexamic acid- β -D-glucoside, chitin acid, taraxasterol, tetrahydrocoumarin B and stigmasterol from dandelion by using water, ethanol or a mixture of water and ethanol as a solvent.
Description
[ technical field ]: mainly applied to the field of medicines, in particular to a method for applying a medical natural product targeted medicine of dandelion extracted by a hydrothermal method to mainly treat dermatitis allergy.
[ technical background ]: allergic dermatitis is a skin health problem caused by internal and external infections or noninfectious factors such as endocrine dyscrasia or food allergy, and is generally erythema, pimple, blister, and the like. The etiology and clinical manifestation are many, and the attack is easy to repeat and difficult to cure radically. Currently, antibiotic therapy is mostly adopted in the aspect of clinical treatment of inflammation, but antibiotic treatment of inflammation has three major problems: (1) when the antibiotic is used for treatment, the organism is easy to generate drug resistance, and the drug effect is gradually reduced; (2) the medicine is three-way toxic, and the antibiotic treatment on inflammation can generate side effects, for example, the vehicle is easy to be dizzy and fatigued after the antibiotic is taken, and the potential safety hazard of human body is certainly brought; (3) the Treatment effect is not ideal, the Treatment effect is easy to relapse, and the Treatment cannot be radically cured (fatigue C.Siegfried.et al.A systematic screening mutation Review of publication presenting Treatment Guidelines for peptide antigenic derivatives in Contrast to Clinical Practice Patterns [ J ]. Dermatol Ther (Heidelb), 2018, 8: 349 377; Margarete Niebuhr, et al.Antibiotreatment of Clinical infections with Staphylococcus aureus in peptides with Clinical reactivity: Clinical reactivity inhibitors in surgery, 2008, 957). Therefore, it is important to find a green, safe and non-recurrence anti-inflammatory drug to replace antibiotics.
It is worth noting that Dandelion (FIG. 1), also known as famotidine and rustica herb, belongs to the family of the Compositae, is a perennial herb consisting of four parts of flowers (FIG. 2), stems (FIG. 3), leaves (FIG. 4) and roots (FIG. 5), has more than 70 kinds in China and is abundant in resources, widely distributed in most provinces in China, is not only a long-history traditional herbal medicine, but also one of the common wild vegetables on the table, the main ingredients in Dandelion flowers are green cloves, luteolin 7-O-glucoside, caffeic acid (FIG. 6), the main ingredients in Dandelion stems and leaves are quercetin glucoside, Dandelion glue- β -D-glucoside, tranexamic acid- β -D-glucoside, crustacean acid (FIG. 7), the main ingredients in roots are taraxasterol, tetrahydrocoumarin B, stigmasterol (FIG. 8) (Yueyun, Yan acid, Yan milk extract-additive extract-glycoside, Dandelion, vitamin J, Dandelion, etc. 8, having various anti-infection, anti-inflammation, and anti-inflammation, oral-inflammation, and anti-inflammation, oral effects, and anti-inflammation, and anti-infection, and anti-inflammation, drugs, and anti-inflammation, respectively, and anti-inflammation, drugs, and anti-cancer, and anti-inflammation, and anti-cancer, and anti-cancer, drug, anti-cancer, anti-.
The traditional extraction method of active ingredients of natural plants mainly comprises continuous extraction method and microwave extraction method (NadezdaPetkova, et al. analytical and carbonate content in injections and microwave extracts from organic Biological plants [ J ]. Journal of applied pharmaceutical Science, 2017, 7(10), 055-. Although the continuous leaching method is simple to operate and high in extraction efficiency, the reaction process is long in time consumption and high in energy consumption, and the advantages of industrial production are not achieved. Although the ultrasonic extraction method has wide extraction adaptability, the liquid medicine has less impurities and is simple and easy to implement; however, the temperature can only be controlled at about 50 ℃, so that the optimal extraction of partial active ingredients of natural products is limited.
The invention relates to a hydrothermal extraction process of active ingredients of dandelion natural products mainly treating allergic dermatitis, which takes one or two mixtures of water and ethanol as a solvent, and puts the solvent into a reaction kettle (figure 9), and the continuous multiple reaction extraction is carried out at constant temperature in different sections, the reaction is easy to control, the operation is simple, efficient and environment-friendly, the product purity is high, the operation efficiency is high, and the method is suitable for the low-cost and large-scale production of dandelion extracts; meanwhile, the natural product active substance extracted by the method has obvious treatment and inhibition effects on various skin diseases such as dermatitis, skin itch, pustular cyst and the like, meets the requirements of effective medicines of patients, and has great application potential.
With the aging of the population and the increasing environmental pollution, patients with allergic dermatitis are at an increasing potential. Therefore, the treatment of the molecular targeted drug is more popular with the majority of medical people, because the molecular targeted drug can specifically act on a target spot, directly inhibit the growth of malignant cells, can be used for a long time, effectively kill diseased cells, has small damage to organisms, small side effect, difficult generation of drug resistance and good tolerance. More importantly, the Hyaluronic Acid (HA) -Polyethyleneimine (PEI) targeted drug HAs selectivity, and the release rate just accords with the absorption rate of a human body, so that a good slow release effect is achieved; in the synthesis process of the HA-PEI material, initiators of N-hydroxysuccinimide (NHS) and 1- (3-dimethylaminopropyl) -3-Ethylcarbodiimide (EDC) are required to be added. If the targeted medicine can be combined with the effective components of the dandelion, good medical clinical effect can be achieved.
Aiming at the urgent needs of the existing science and technology, the invention relates to a method for extracting a targetable medical natural product targeted drug from dandelion by a hydrothermal method and applying the targetable medical natural product targeted drug to mainly treat dermatitis allergy, in particular introduces a high-yield preparation HA-PEI targeted drug carrier, and develops a new method for extracting the targetable medical natural product targeted drug from dandelion by the hydrothermal method and applying the targetable medical natural product targeted drug to mainly treat dermatitis allergy; the preparation method has the advantages of simple operation, convenient raw material acquisition and high synthesis efficiency, the prepared medicine can be slowly released, the release rate meets the absorption rate of a human body, and the curative effect on allergic dermatitis is remarkable.
[ summary of the invention ]: the main contents of the patent of the invention are respectively as follows: (1) one or two mixtures of water and ethanol are used as a solvent, and the dandelion is subjected to multi-stage constant-temperature continuous extraction in a closed hydrothermal reaction kettle with high temperature and high pressure by regulating and controlling reaction parameters, so that the solubility of each component of the raw material can be increased, and the high extraction yield can be obtained; (2) the targetable medicine extracted from the medical natural dandelion product by the hydrothermal method is mainly used for treating allergic dermatitis, and has the advantages of simple preparation method, easily controlled conditions, high efficiency, environmental protection, abundant raw material resources and suitability for low-cost mass production; (3) the designed and synthesized HA-PEI targeted drug carrier HAs proper polymerization degree, is beneficial to absorption by human body, and HAs controllable spherical structure and appearance; (4) from the clinical application perspective, the dandelion extract can be directly applied and prepared into cream or solid products to treat allergic dermatitis, skin itch, pustular cyst, and has obvious skin nourishing effect and no recurrence.
[ technical solution of the present invention ]:
the invention relates to a method for applying medical natural dandelion product targeted drugs extracted by a hydrothermal method to mainly treat dermatitis allergy; the specific synthetic process comprises 2 steps: the first step is the synthesis of a targeted drug carrier of the HA-PEI hollow microsphere, and the second step is the preparation of a targeted drug composite material of the dandelion natural active substance extracted by a hydrothermal method.
The preparation method of the HA-PEI targeted drug carrier comprises the following specific steps: firstly, weighing 0.1000 g-2.0000 g of sodium salt, dissolving in 20ml of deionized water, and heating the solution to 30 ℃ to form a sodium salt solution; the sodium salt is one, two or more of sodium sulfite, sodium phosphite, sodium bromate, sodium bromide, sodium nitrate, sodium bicarbonate, sodium carbonate, sodium gluconate, sodium chlorate, sodium chloride, sodium sulfate, sodium thiosulfate, sodium phosphate, sodium pyrophosphate, sodium formate, sodium persulfate, sodium silicate, sodium perchlorate, sodium iodide, sodium acetate, sodium hypochlorite, sodium acrylate, sodium propionate and sodium benzoate.
Secondly, weighing 0.0100 g-1.8000 g of HA and 0.0010 g-1.0000 g of PEI respectively in 2 beakers, adding 5ml of the prepared sodium salt solution respectively, and carrying out ultrasonic oscillation for 5-120 min for later use after the ultrasonic oscillation is finished;
thirdly, weighing 0.0100-0.2200 g of NHS and 0.0100-0.3550 g of EDC, dissolving in 30 ml of deionized water, and ultrasonically oscillating for 5-120 min for later use after the ultrasonic oscillation is finished;
fourthly, transferring the prepared solution of 30 ml of NHS/EDC into a 200ml round-bottom flask, transferring the solution containing 0.0100g to 0.2000g of HA into the round-bottom flask, and dropwise adding the solution containing 0.0100g to 0.2500g of PEI to obtain a precursor solution;
fifthly, transferring the precursor solution to a microwave reactor with normal pressure and reflux condensation, adjusting the microwave radiation power to be 100-1200W, heating the solution to 10-100 ℃, and continuously reacting for 1-120 minutes to stop; after the microwave reaction is finished, cooling the obtained solution to room temperature;
and sixthly, pouring the solution after the reaction into a dialysis bag with the aperture of 5-20 microns, placing the dialysis bag into constant-temperature circulating high-purity water, dialyzing for 12 hours at normal temperature, pouring the product into a sterilized clean 200ml beaker, freeze-drying for 12-120 hours at the low temperature of-40-60 when the color gradually turns white and the impurity content in the dialysis bag is equal to the number of the high-purity water, and collecting a sample for later use. The nuclear magnetic spectrogram of the synthesized HA-PEI targeted drug carrier shows that the HA-PEI targeted drug carrier HAs good high-molecular polymerization degree, and realizes the ordered polymerization of molecular chains; a scanning electron microscope of the sample shows that the sample is a hollow spherical material with the diameter of 1-3 microns, and conditions are provided for bearing more natural extraction active substances.
The invention provides a method for extracting a targetable drug serving as a medical natural product of dandelion by a hydrothermal method and applying the targetable drug to mainly treat dermatitis allergy, which is characterized by comprising the following steps:
firstly, washing 3g of fresh and healthy dandelion whole plant for 3-5 times, airing, cutting into small sections of 2-3 cm, and taking water, ethanol or a mixture of water and ethanol as a solvent, wherein the solid-liquid ratio is 1: 10-1: 100;
secondly, putting the reactant obtained in the step one into a hydrothermal reaction kettle with the inner container volume of 200ml, wherein the outer container of the hydrothermal reaction kettle is made of 304 stainless steel materials, and the inner container is made of polytetrafluoroethylene materials; the kettle filling rate is 60-80%, the heating temperature is set to 2-5 heating sections, the temperature interval is 40-70 ℃, the heating interval time is 0.5-2 h, the reaction time of the constant temperature section is 4-12 h, and the heating rate is 2-5 ℃/min; the process can be combined randomly within the range of the number of hydrothermal reaction sections, the range of reaction temperature, the range of constant temperature reaction time and the range of interval temperature;
thirdly, centrifuging the product obtained in the second step for 4-10 min at the rotating speed of 5000-8000 r/min, and taking supernatant liquid, namely dandelion extracting solution; evaporating for 8 hours at 65 ℃ by using a reduced pressure distillation device under the vacuum degree of-0.1 MPa, and evaporating the volatile ethanol solvent to obtain a high-concentration natural product concentrated solution; the obtained extractive solution is composed of taraxasterol with molecular formula of C30H50O, the concentration range is 10-100 mug/ml; tetrahydrocoumarin B of formula C19H16O3The concentration range is 20-40 mu g/ml; caffeic acid with molecular formula C9H8O4The concentration range is 20-100 mu g/ml; chlorogenic acid with molecular formula of C16H18O9The concentration range is 10-50 mu g/ml; quercetin glycoside with molecular formula of C15H14O9The concentration range is 10-70 mu g/ml, stigmasterol, chitosan, dandelion glue- β -D-glucoside, tranexamic acid- β -D-glucoside and luteolin 7-O-glucoside;
fourthly, directly applying the extract obtained in the third step on the affected part of dermatitis to play a role in treating the dermatitis;
fifthly, the extract obtained in the step three is prepared into cream for face care, and the cream has the effects of removing freckles and acne;
sixthly, mixing the extract obtained in the step three with a soap liquid to prepare the soap for resisting oxidation and inhibiting bacteria of the skin.
The method for extracting the targetable medicine serving as the medical natural product of the dandelion by the hydrothermal method and applying the targetable medicine to mainly treat dermatitis allergy is characterized by comprising the following steps: the raw material is fresh and healthy dandelion, the dried dandelion is crushed into 30-60 meshes, and the concentration of solvent ethanol is 40% -70%, or the mixed solution of ethanol and water with the ratio of 1: 1-1: 100.
The method for extracting the targetable medicine serving as the medical natural product of the dandelion by the hydrothermal method and applying the targetable medicine to mainly treat dermatitis allergy is characterized by comprising the following steps: the cream is prepared by fully stirring 3-5 g of dandelion extract, 1-10 g of HA-PEI targeted drug carrier for 15 minutes, and fully stirring and emulsifying with 20-30 g of polydimethylsiloxane, 20-30 g of dipropylene glycol, 20-30 g of butanediol, 20-25 g of glycerol and 30-40 g of water for 30-60 minutes to obtain the cream-like skin care product, wherein the emulsifying temperature is 20-50 ℃, and the stirring speed is 1200-1600 r/min.
The method for extracting the targetable medicine serving as the medical natural product of the dandelion by the hydrothermal method and applying the targetable medicine to mainly treat dermatitis allergy is characterized by comprising the following steps: the soap solution is prepared by fully stirring 3-5 g of dandelion extract, 1-10 g of HA-PEI targeted drug carrier for 15 minutes, mixing with 20-30 g of sodium fatty acid, 30-40 g of water, 20-30 g of glycerol, 15-20 g of corn starch, potato starch, sweet potato starch or pea starch, 10-15 g of talcum powder and 10-15 g of coconut oil acid, heating to 60-80 ℃, adding 20-30% sodium hydroxide to adjust the pH to be neutral, stirring for 30-50 min at the stirring speed of 1200-1600 r/min to obtain viscous soap solution, and putting the viscous soap solution into a mold for condensation and demolding to obtain the targeted drug soap containing the natural active dandelion extract.
The method for extracting the targetable medicine serving as the medical natural product of the dandelion by the hydrothermal method and applying the targetable medicine to mainly treat dermatitis allergy is characterized by comprising the following steps: the method has the advantages that the dandelion is subjected to continuous extraction in a closed hydrothermal reaction kettle at a constant temperature and a high pressure in different sections, the solubility of each component in the dandelion raw material is increased by regulating and controlling reaction parameters, the method is high in extraction efficiency and product purity, the extract has a remarkable effect on treating various dermatitis, skin itch and pustular cyst, the recurrence phenomenon is avoided, the application potential in pharmacological research and medical drugs is large, and the extraction method has feasibility, high efficiency and novelty.
[ advantages and effects of the invention ]: the method for extracting the targetable medicine serving as the medical natural product of dandelion by the hydrothermal method, which is disclosed by the invention, is applied to mainly treating dermatitis allergy, and has the remarkable advantages that: (1) the raw material resources are rich, the distribution is wide, the price is low, no by-product is generated in the extraction process, and the method is green and environment-friendly; (2) the dandelion is subjected to constant-temperature continuous extraction in different sections in a closed hydrothermal reaction kettle with high temperature and high pressure by regulating and controlling reaction parameters, so that the solubility of each component in the raw material is increased, and a high-purity product is obtained with high extraction efficiency; (3) the method for extracting the dandelion active substance by the hydrothermal method is simple to operate, high in equipment repeatability, easy to regulate and control experimental conditions, and suitable for large-scale low-cost industrial production; (4) the dandelion extract has obvious effect on treating various dermatitis, skin itch and pustular cyst, has no recurrence phenomenon, and has great potential in pharmacological research and medical drug application.
Drawings
FIG. 1 is a diagram of a whole plant of fresh dandelion
FIG. 2 is a partial view of fresh dandelion flowers
FIG. 3 is a partial view of fresh dandelion stems
FIG. 4 is a partial view of fresh dandelion leaves
FIG. 5 is a partial view of fresh dandelion root
FIG. 6 shows the structural formulas of chlorogenic acid, luteolin 7-O-glucoside and caffeic acid in herba Taraxaci
FIG. 7 shows the structural formulas of quercetin glycoside, taraxacum gum- β -D-glucoside, tranexamic acid- β -D-glucoside and chitin acid in herba Taraxaci
FIG. 8 shows the structural formulas of taraxasterol, tetrahydrocoumarin B and stigmasterol in Taraxacum officinale
FIG. 9 is a diagram of a working section of putting the reaction kettle into an oven after the reaction kettle is filled with reactants
Detailed Description
The following embodiments and effects of the present invention are further described with reference to the following examples:
example 1: method for preparing cream from herba Taraxaci extract for caring face
The preparation method of the HA-PEI targeted drug carrier comprises the following steps: 1.5000g of sodium chloride was weighed, dissolved in 20ml of deionized water, and the solution was heated to 30 ℃ to form a sodium chloride solution. Respectively weighing 1.8000g of HA and 0.0500g of PEI in 2 beakers, respectively adding 5ml of the prepared sodium chloride solution, and ultrasonically vibrating for 60min for later use after the ultrasonic treatment; weighing 0.1200g of NHS and 0.2500g of EDC, dissolving in 30 ml of deionized water, ultrasonically oscillating for 5min, and standing by after the ultrasonic oscillation is finished; firstly, transferring a prepared 30 ml NHS/EDC solution into a 200ml round-bottom flask, then transferring an HA solution containing 1.8000g into the round-bottom flask, and dropwise adding a PEI solution containing 0.0500g to obtain a precursor solution; transferring the precursor solution to a microwave reactor with normal pressure and reflux condensation, adjusting the microwave radiation power to 1200W, heating the solution to 40 ℃, and continuously reacting for 2 minutes to stop; after the microwave reaction is finished, cooling the obtained solution to room temperature; pouring the reacted solution into a dialysis bag with the aperture of 15 microns, placing the dialysis bag into constant-temperature circulating high-purity water, dialyzing at normal temperature for 12 hours, pouring the product into a sterilized clean 200ml beaker, and freeze-drying the product at the low temperature of minus 40 ℃ to minus 60 ℃ for 12 to 120 hours when the color gradually turns white and the impurity content in the dialysis bag is equal to the high-purity water value, and collecting a white powder sample for later use; the nuclear magnetic spectrogram of the synthesized HA-PEI targeted drug carrier shows that the HA-PEI targeted drug carrier HAs good high-molecular polymerization degree, and realizes the ordered polymerization of molecular chains; a scanning electron microscope of the sample shows that the sample is a hollow spherical material with the diameter of 1-3 microns, and conditions are provided for bearing more natural extraction active substances.
Washing 3g of fresh and healthy whole dandelion (figure 1) for 3 times, cutting flowers (figure 2), stems (figure 3), leaves (figure 4) and roots (figure 5) into 2cm small segments, taking water as a solvent, putting raw materials and 1: 48 of the solvent into a hydrothermal reaction kettle (figure 9) with the pot filling rate of 72%, setting 3 heating sections, heating the hydrothermal reaction to 40 ℃ at the speed of 2 ℃/min, reacting at constant temperature for 4h, further heating to 45 ℃ for 4h, further heating to 50 ℃ for reaction for 4h until the 3 sections are completely finished, cooling to room temperature, taking out the product, centrifuging for 5min at the speed of 6000r/min, taking the supernatant to obtain a product containing chlorogenic acid, luteolin 7-O-glucoside, caffeic acid, quercetin glucoside, dandelion glue- β -D-glucoside, tranexamic acid- β -D-glucoside, PEI, tetrahydrochysenol B, propylene glycol 7-O-glucoside, 20g of a natural dandelion extract, extracting a butylene glycol-20 g of a concentrated solution by using 20g of distilled water, stirring at the vacuum degree of 60 g of distilled water, extracting a volatile glycerol for 20.8 g of a volatile carrier under the condition of 20-20 MPa, and evaporating the concentration of a 20g of a volatile alcohol-20 g of a skin-20 g of a distilled liquid for obtaining a skin-eliminating the finished cream-eliminating the finished product, and a skin-protecting emulsion.
Example 2: method for extracting dandelion medical natural product for mainly treating dermatitis by hydrothermal method
Washing 3g of dried and healthy dandelion whole plant for 3 times, mixing flowers, stems, leaves and roots of the dandelion, cutting the flowers, stems, leaves and roots into 40 meshes, taking 70% ethanol as a solvent, putting the raw materials and the solvent in a ratio of 1: 50 into a hydrothermal reaction kettle, setting the kettle filling rate to be 75%, setting 3 heating sections in the hydrothermal reaction process, heating the hydrothermal reaction set temperature to 40 ℃ at the speed of 2 ℃/min, carrying out constant-temperature reaction for 4 hours at the temperature, continuing heating to 50 ℃ for reaction for 4 hours, continuing heating to 55 ℃ for reaction for 4 hours until 3 sections are completely finished, cooling to room temperature, centrifuging the dandelion crude extract liquid for 5 minutes at the rotating speed of 6000r/min, taking the supernatant to obtain the dandelion extract containing chlorogenic acid, luteolin 7-O-glucoside, caffeic acid, quercetin glucoside, taraxacumin- β -D-glucoside, tranexamic acid- β -D-glucoside, crustacean acid, taraxasterol, tetrahydrocoumarin B, stigmasterol (figure 6, figure 7, figure 8), concentrating the dandelion extract under the vacuum degree of vacuum for 0.65 hours, concentrating the dandelion extract liquid, and evaporating the volatile ethanol to obtain the volatile alcohol.
Example 3: method for extracting dandelion medical natural product for mainly treating dermatitis by hydrothermal method
Washing 3g of fresh and healthy whole dandelion, cutting flowers, stems, leaves and roots of the dandelion into 2cm segments, taking water as a solvent, putting the raw materials and the solvent in a proportion of 1: 40 into a hydrothermal reaction kettle, setting the kettle filling rate to be 60%, setting 3 heating sections in the hydrothermal reaction process, heating the hydrothermal reaction set temperature to 40 ℃ at the speed of 2 ℃/min, carrying out constant temperature reaction for 4h at the temperature, continuing heating to 55 ℃ for reaction for 4h, continuing heating to 60 ℃ for reaction for 4h until the 3 sections are completely finished, cooling to room temperature, taking out the product, centrifuging for 5min at the rotating speed of 6000r/min, taking supernatant to obtain the dandelion extract containing chlorogenic acid, luteolin 7-O-glucoside, caffeic acid, quercetin glucoside, dandelion glue- β -D-glucoside, tranexamic acid- β -D-glucoside, chitosan, taraxasterol, tetrahydrocoumarin B, stigmasterol (fig. 6, fig. 7 and fig. 8), distilling the dandelion extract under the vacuum degree of 0.65 MPa for distillation for 8 h, and evaporating the volatile ethanol extract at the vacuum degree of 3 hours to obtain the volatile ethanol extract, thereby eliminating symptoms.
Example 4: method for preparing cream from herba Taraxaci extract for caring face
The synthesis method of the HA-PEI targeted drug carrier is the same as that of example 1.
Washing 3g of dried and healthy dandelion whole plant for 3 times, mixing and cutting flowers, stems, leaves and roots of the dandelion into 40 meshes, taking 40% ethanol as a solvent, putting the raw materials and the solvent in a ratio of 1: 45 into a hydrothermal reaction kettle, wherein the kettle filling rate is 67.5%, heating the hydrothermal reaction at a set temperature of 2 ℃/min to 60 ℃, carrying out constant temperature reaction for 4 hours at the temperature, cooling the whole workshop section to room temperature, centrifuging the crude dandelion extract at a rotating speed of 6000r/min for 5 minutes, taking supernatant to obtain a dandelion extract containing chlorogenic acid, luteolin 7-O-glucoside, caffeic acid, quercetin glucoside, dandelion glue- β -D-glucoside, tranexamic acid- β -D-glucoside, crustacean acid, taraxasterol, tetrahydrocoumarin B, stigmasterol (fig. 6, 7 and 8), evaporating the dandelion extract at a vacuum degree of-0.1 MPa for 8 hours at 65 ℃, evaporating the volatile ethanol solvent to obtain a high-concentration PEI solution, evaporating the crude dandelion extract for 5g, concentrating the crude dandelion extract for 20g, 20g of the skin-protecting glycerol, fully stirring the skin and finally obtaining a skin-protecting emulsion, and further mixing the skin-20 g of the PEI extract under the conditions of 20g of 20 minutes to obtain a skin-20 g of the PEI.
Example 5: method for preparing soap from herba Taraxaci extract
The synthesis method of the HA-PEI targeted drug carrier is the same as that of example 1.
Washing 3g of fresh and healthy whole dandelion, cutting flowers, stems, leaves and roots of the dandelion into small segments of 2cm, taking water as a solvent, putting the raw materials and the solvent with the weight ratio of 1: 42 into a hydrothermal reaction kettle, keeping the kettle filling rate at 63%, heating the hydrothermal reaction at the set temperature of 2 ℃/min to 35 ℃, carrying out constant temperature reaction for 4 hours at the temperature, continuing to heat to 40 ℃ for 4 hours, continuing to heat to 45 ℃ for 4 hours until all 3 sections are finished, cooling to room temperature, taking out the product, centrifuging for 5 minutes at the rotating speed of 6000r/min, taking the supernatant to obtain the dandelion extract containing chlorogenic acid, luteolin 7-O-glucoside, caffeic acid, quercetin glucoside, dandelion glue- β -D-glucoside, tranexamic acid- β -D-glucoside, crustacean acid, taraxasterol, tetrahydrocoumarin B, stigmasterol (figure 6, figure 7 and figure 8), distilling under the vacuum degree of vacuum for 8 hours under the reduced pressure, adding 65 g of ethanol, concentrating the dandelion extract for 8g, evaporating the concentration of the supernatant to 20g of sodium hydroxide, concentrating the supernatant to 20g of sodium stearate, stirring to 20g of sodium hydroxide, stirring to obtain a starch-20 g, concentrating the supernatant to obtain a supernatant, concentrating the extract of the dandelion extract, and concentrating the extract under the concentration of 20g of sodium stearate, and stirring to obtain the extract, and concentrating the extract of the.
Example 6: method for preparing soap from herba Taraxaci extract
The synthesis method of the HA-PEI targeted drug carrier is the same as that of example 1.
Washing 3g of dried and healthy dandelion whole plant for 3 times, mixing flowers, stems, leaves and roots of the dandelion, cutting the dandelion into 40 meshes, taking a mixed solution of water and ethanol in a ratio of 1: 50 as a solvent, mixing the dandelion small segments with the solvent, putting the dandelion into a hydrothermal reaction kettle, wherein the kettle filling rate is 70%, setting the hydrothermal reaction temperature, heating the mixture to 30 ℃ at a speed of 2 ℃/min, carrying out a constant temperature reaction for 4 hours, further heating to 40 ℃ for 4 hours, further heating to 50 ℃ for 4 hours, cooling to room temperature until all 3 sections are finished, centrifuging the dandelion crude extract at a speed of 6000r/min for 5 minutes, taking the supernatant to obtain a soap containing chlorogenic acid, luteolin 7-O-glucoside, caffeic acid, quercetin glucoside, taraxacumin- β -D-glucoside, tranexamic acid- β -D-glucoside, caraboxylic acid, taraxasterol, tetrahydrocoumarin B, stigmasterol (fig. 6, fig. 7 and fig. 8), distilling under a vacuum degree of vacuum of 0.1.1.8.8.10 MPa, concentrating the dandelion extract under vacuum, adding a vacuum degree of distillation, concentrating the concentrated solution to obtain a concentrated solution containing sodium hydroxide, concentrating the extract containing sodium stearate, concentrating the extract at a concentration of 10g of 25-10 g of sodium stearate, stirring to obtain a sodium stearate, concentrating the extract with a high concentration of 25-20 g of sodium stearate, stirring to obtain a high-20 g of a high-20-10-20-10-20-purity-10-concentration-10.
Comparative example 1: publication No. CN 105287682 a (publication No. 2016.02.03) provides a preparation method:
1) extracting herba Taraxaci with water, filtering, mixing filtrates, and concentrating under reduced pressure to obtain concentrated solution;
2) step 1), adding ethanol into the concentrated solution until the ethanol content is 40-70%, standing, filtering, concentrating under reduced pressure, and recovering ethanol to obtain concentrated solution;
3) step 2), adding water into the concentrated solution to dilute the concentrated solution to be equivalent to 1-3 times of the weight of the medicinal materials, adjusting the pH value to 2-6, adding the diluted solution to a pretreated macroporous resin column for adsorption, eluting with a 1-3BV diluted hydrochloric acid solution with the pH value of 3-7 at the flow rate of 1-3BV/h, eluting with 1-3BV pure water at the flow rate of 2-3BV/h, discarding the eluent, eluting with 1-3BV 40-60% ethanol at the flow rate of 1-4 BV/h, and finally eluting with 1-3BV 60-80% ethanol at the flow rate of 2-4 BV/h;
4) mixing the alcohol eluates obtained in step 3), concentrating, and drying to obtain herba Taraxaci extract.
The cited patent adopts a continuous extraction method, water is used as a solvent, and the extraction process of the medical natural dandelion product is adopted.
The invention discloses a method for extracting medical natural product targeted medicine of dandelion by a hydrothermal method and applying the medical natural product targeted medicine to mainly treat dermatitis allergy, as described in example 1, 3g of fresh and healthy whole dandelion is washed for 3 times, flowers, stems, leaves and roots of the dandelion are cut into small sections of 2cm, water is used as a solvent, the raw materials and the solvent are mixed and then put into a hydrothermal reaction kettle, the kettle filling rate is 60%, the temperature of the hydrothermal reaction is set to be heated to 40 ℃ at the speed of 2 ℃/min, the hydrothermal reaction is carried out for 4h at the constant temperature, then the temperature is continuously raised to 50 ℃ for reaction for 4h, the temperature is continuously raised to 55 ℃ for reaction for 4h until all 3 sections are completed, the hydrothermal reaction is cooled to room temperature, the product is taken out and centrifuged for 5min at the rotating speed of 6000r/min, the supernatant is taken, thus obtaining the product containing chlorogenic acid, luteolin 7-O-glucoside, caffeic acid, quercetin glucoside, dandelion glue- β -D-glucoside, tranexamic acid- β -D-glucoside, chitosterol, tetrahydrochysenol, coumarin (6B, coumarin, a picture 7-8.8 MPa) and the extraction liquid is evaporated under the vacuum degree of the alcohol, thus obtaining the extraction liquid, and the volatile alcohol is evaporated under the concentration is further carried out under the concentration of the concentration.
The hydrothermal method can be used for continuously extracting the dandelion in a closed hydrothermal reaction kettle with high temperature and high pressure at constant temperature in different sections by regulating and controlling reaction parameters, so that the solubility of each component of the raw material is increased.
Comparative example 2: publication No. CN 109045094 a (publication No. 2018.08.27) provides a preparation method:
(1) preparing a raw material dandelion, removing impurities, cleaning, cutting into sections, airing and crushing to 40-60 meshes to obtain dandelion powder;
(2) weighing dandelion powder, adding 8-10 times of 70-80% ethanol solution by volume fraction into the dandelion powder, setting the microwave power in a microwave extraction instrument to be 500-600W, extracting for 50-60 seconds to obtain an extracting solution, and concentrating the extracting solution under reduced pressure until no alcohol smell exists to obtain a concentrated solution;
(3) adding water into the concentrated solution obtained in the step (2), wherein the mass ratio of the concentrated solution to the water is 1: 0.5-4, and centrifuging to obtain a supernatant;
(4) and (4) putting the supernatant obtained in the step (3) into a microfiltration membrane for microfiltration to obtain the dandelion extract.
The cited patent adopts microwave extraction method, 70% ethanol is used as solvent, and the extraction process of medical natural dandelion product is adopted.
The invention discloses a method for extracting medical natural product targeted medicine of dandelion by a hydrothermal method and applying the medical natural product targeted medicine to mainly treat dermatitis allergy, as shown in example 2, 3g of dried and healthy dandelion is washed for 3 times, flowers, stems, leaves and roots of the dandelion are mixed and cut into 40 meshes, 70% ethanol is used as a solvent, the raw materials and the solvent are put into a hydrothermal reaction kettle in a ratio of 1: 50, the kettle filling rate is 60%, 3 heating sections are arranged in the hydrothermal reaction process, the hydrothermal reaction temperature is set to be heated to 40 ℃ at a speed of 2 ℃/min, the constant temperature reaction is carried out for 4h at the temperature, the temperature is further heated to 50 ℃ for reaction for 4h, the temperature is further heated to 55 ℃ for reaction for 4h until all the 3 sections are finished and cooled to room temperature, the crude dandelion extract is centrifuged for 5min at a rotating speed of 6000r/min, the supernatant is taken to obtain a chlorogenic acid, luteolin 7-O-glucoside, caffeic acid, quercetin glucoside, dandelion gum- β -D-glucoside, tranexamic acid- β -D, coumarin acid, and concentrated distilled liquor (0.8) under a vacuum degree of 0.8 MPa, so as to obtain a volatile phytosterol extract, and finally, a phytosterol extract, and a phytosterol extract liquid, a phytosterol extract is evaporated and a phytosterol extract is concentrated on an alcohol drawing, and a phytosterol drawing, and a volatile alcohol is obtained by utilizing a device.
The hydrothermal method is used for carrying out closed-type environment extraction on the dandelion through multiple sections, and compared with a microwave extraction method, the hydrothermal method is higher in the solubility of active substances in the dandelion, higher in product purity and simple to operate.
Comparative example 3: publication No. CN 107693564 a (publication No. 2018.02.16) provides a preparation method:
(1) removing impurities from the whole dandelion herb, drying until no water exists, crushing, and sieving to 50-60 meshes to obtain dandelion powder;
(2) adding ethanol into an ultrasonic extractor, then adding dandelion powder, wherein the solid-to-liquid ratio of the dandelion powder to the ethanol is 1 g: 70-80 ml, the volume concentration of the ethanol is 73-78%, the extraction power of the ultrasonic extractor is 300-400W, the extraction frequency is 40-45 kHz, the extraction temperature is 40-60 ℃, the extraction time is 10-20 minutes, and filtering is carried out to obtain a primary extracting solution and primary filter residue;
(3) extracting the primary filter residue once again by the same method as the step (2) to obtain a secondary extracting solution and secondary filter residue; mixing the extractive solutions to obtain ethanol extract; concentrating the alcohol extract until no alcohol smell exists;
(4) adding water into the concentrated alcohol extract to prepare an alcohol extract solution with the concentration of 9-12 mg/ml and the pH value of 5-6, carrying out chromatography separation on the alcohol extract solution through macroporous resin, removing impurities by using deionized water, eluting and removing impurities by using dilute ethanol with the volume concentration of 10-15%, eluting by using a mixed solution of ethyl ether, n-butyl alcohol and trichloroethane in a volume ratio of 1: 3-4: 75 as an eluent, collecting eluent, concentrating the eluent, and carrying out low-temperature freeze drying to obtain the dandelion antibacterial component.
The cited patent adopts an ultrasonic extraction method and 75% ethanol as a solvent, and the extraction process of the medical natural dandelion product is carried out.
The invention discloses a method for extracting medical natural product targeted medicine of dandelion by a hydrothermal method and applying the medical natural product targeted medicine to mainly treat dermatitis allergy, as described in example 2, 3g of dried and healthy dandelion is washed for 3 times, flowers, stems, leaves and roots of the dandelion are mixed and cut into 40 meshes, 70% ethanol is used as a solvent, the raw materials and the solvent are mixed and then are put into a hydrothermal reaction kettle, the kettle filling rate is 60%, 3 heating sections are arranged in the hydrothermal reaction process, the temperature is increased to 50 ℃ at the speed of 2 ℃/min, the reaction is carried out for 4h at constant temperature, then the heating is stopped for 30min, the heating is continued to 50 ℃ for reaction for four hours, the reaction kettle is cooled to room temperature after the reaction of the three sections is finished, the crude dandelion extract is centrifuged for 5min at the rotating speed of 6000r/min, the supernatant is taken, the supernatant is obtained, thus obtaining the natural extract containing chlorogenic acid, luteolin 7-O-glucoside, caffeic acid, quercetin glucoside, dandelion glue- β -D-glucoside, tranexamic acid- β -D-glucoside, tetrahydrochysenol, coumarin B, distilled coumarin (shown in a drawing, and a vacuum degree of 0.8-8 MPa, and then the volatile alcohol extract is evaporated in a device, so as to obtain a volatile alcohol extract, and then the volatile alcohol is concentrated solution with the concentration of the device.
The active substances of the dandelion are extracted by a hydrothermal method in a closed multi-section way, the product purity is high, the equipment repeatability is high, the operation is easy to master, and the method is suitable for low-cost industrial production of the dandelion extract.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications, substitutions and the like can be made thereto without departing from the spirit and scope of the invention.
Claims (6)
1. The invention relates to a method for applying medical natural dandelion product targeted drugs extracted by a hydrothermal method to mainly treat dermatitis allergy; the specific synthetic process comprises 2 steps: the first step is the preparation of a targeted drug carrier of the HA-PEI hollow microsphere, and the second step is the preparation of a targeted drug composite material of the dandelion natural active substance extracted by a hydrothermal method;
the preparation method of the HA-PEI targeted drug carrier comprises the following specific synthetic steps: firstly, weighing 0.1000 g-2.0000 g of sodium salt, dissolving in 20ml of deionized water, and heating the solution to 30 ℃ to form a sodium salt solution; the sodium salt is one, two or more of sodium sulfite, sodium phosphite, sodium bromate, sodium bromide, sodium nitrate, sodium bicarbonate, sodium carbonate, sodium gluconate, sodium chlorate, sodium chloride, sodium sulfate, sodium thiosulfate, sodium phosphate, sodium pyrophosphate, sodium formate, sodium persulfate, sodium silicate, sodium perchlorate, sodium iodide, sodium acetate, sodium hypochlorite, sodium acrylate, sodium propionate and sodium benzoate;
secondly, weighing 0.0100 g-1.8000 g of HA and 0.0010 g-1.0000 g of PEI respectively in 2 beakers, adding 5ml of the prepared sodium salt solution respectively, and carrying out ultrasonic oscillation for 5-120 min for later use after the ultrasonic oscillation is finished;
thirdly, weighing 0.0100-0.2200 g of NHS and 0.0100-0.3550 g of EDC, dissolving in 30 ml of deionized water, and ultrasonically oscillating for 5-120 min for later use after the ultrasonic oscillation is finished;
fourthly, transferring the prepared solution of 30 ml of NHS/EDC into a 200ml round-bottom flask, transferring the solution containing 0.0100g to 0.2000g of HA into the round-bottom flask, and dropwise adding the solution containing 0.0100g to 0.2500g of PEI to obtain a precursor solution;
fifthly, transferring the precursor solution to a microwave reactor with normal pressure and reflux condensation, adjusting the microwave radiation power to be 100-1200W, heating the solution to 10-100 ℃, and continuously reacting for 1-120 minutes to stop; after the microwave reaction is finished, cooling the obtained solution to room temperature;
sixthly, pouring the reacted solution into a dialysis bag with the aperture of 5-20 microns, placing the dialysis bag into constant-temperature circulating high-purity water, dialyzing for 12 hours at normal temperature, gradually whitening the color in the dialysis process, pouring the product into a sterilized clean 200ml beaker, freeze-drying for 12-120 hours at the low temperature of-40-60 ℃ and collecting a sample for later use, wherein the impurity content in the dialysis bag is equal to the number of the high-purity water; the nuclear magnetic spectrogram of the synthesized HA-PEI targeted drug carrier shows that the HA-PEI targeted drug carrier HAs good high-molecular polymerization degree, and the realization of ordered polymerization of molecular chains is confirmed; a scanning electron microscope of the sample shows that the sample is a hollow spherical material with the diameter of 1-3 microns, and conditions are provided for bearing more natural extraction active substances.
2. The invention provides a method for extracting a targetable drug serving as a medical natural product of dandelion by a hydrothermal method and applying the targetable drug to mainly treat dermatitis allergy, which is characterized by comprising the following steps:
firstly, washing 3g of fresh and healthy dandelion whole plant for 3-5 times, airing, cutting into small sections of 2-3 cm, and taking water, ethanol or a mixture of water and ethanol as a solvent, wherein the solid-liquid ratio is 1: 10-1: 100;
secondly, putting the reactant obtained in the step one into a hydrothermal reaction kettle with the inner container volume of 200ml, wherein the outer container of the hydrothermal reaction kettle is made of 304 stainless steel materials, and the inner container is made of polytetrafluoroethylene materials; the kettle filling rate is 60-80%, the heating temperature is set to 2-5 heating sections, the temperature interval is 40-70 ℃, the heating interval time is 0.5-2 h, the reaction time of the constant temperature section is 4-12 h, and the heating rate is 2-5 ℃/min; the process can be combined randomly within the range of the number of hydrothermal reaction sections, the range of reaction temperature, the range of constant temperature reaction time and the range of interval temperature;
thirdly, centrifuging the product obtained in the second step for 4-10 min at the rotating speed of 5000-8000 r/min, and taking supernatant liquid, namely dandelion extracting solution; evaporating for 8 hours at 65 ℃ by using a reduced pressure distillation device under the vacuum degree of-0.1 MPa, and evaporating the volatile ethanol solvent to obtain a high-concentration natural product concentrated solution; the obtained extractive solution is composed of taraxasterol with molecular formula of C30H50O, the concentration range is 10-100 mug/ml; tetrahydrocoumarin B of formula C19H16O3The concentration range is 20-40 mu g/ml; caffeic acid with molecular formula C9H8O4The concentration range is 20-100 mu g/ml; chlorogenic acid with molecular formula of C16H18O9The concentration range is 10-50 mu g/ml; quercetin glycoside with molecular formula of C15H14O9The concentration range is 10-70 mu g/ml, stigmasterol, chitosan, dandelion glue- β -D-glucoside, tranexamic acid- β -D-glucoside and luteolin 7-O-glucoside;
fourthly, directly applying the extract obtained in the third step on the affected part of dermatitis to play a role in treating the dermatitis;
fifthly, the extract obtained in the step three is prepared into cream for face care, and the cream has the effects of removing freckles and acne;
sixthly, mixing the extract obtained in the step three with a soap liquid to prepare the soap for resisting oxidation and inhibiting bacteria of the skin.
3. The method for applying the targetable medicine of medical natural dandelion product extracted by the hydrothermal method of claim 2 to mainly treat dermatitis allergy is characterized in that: the raw material is fresh and healthy dandelion, the dried dandelion is crushed into 30-60 meshes, and the concentration of solvent ethanol is 40% -70%, or the mixed solution of ethanol and water with the ratio of 1: 1-1: 100.
4. The method for applying the targetable medicine of medical natural dandelion product extracted by the hydrothermal method of claim 2 to mainly treat dermatitis allergy is characterized in that: the cream is prepared by fully stirring 3-5 g of dandelion extract concentrate and 1-10 g of HA-PEI targeted drug carrier for 15 minutes, and fully stirring and emulsifying with 20-30 g of polydimethylsiloxane, 20-30 g of dipropylene glycol, 20-30 g of butanediol, 20-25 g of glycerol and 30-40 g of water for 30-60 minutes to obtain the cream-like skin care product, wherein the emulsifying temperature is 20-50 ℃, and the stirring speed is 1200-1600 r/min.
5. The method for applying the targetable medicine of medical natural dandelion product extracted by the hydrothermal method of claim 2 to mainly treat dermatitis allergy is characterized in that: the soap solution is prepared by fully stirring 3-5 g of dandelion extract, 1-10 g of HA-PEI targeted drug carrier for 15 minutes, mixing with 20-30 g of sodium fatty acid, 30-40 g of water, 20-30 g of glycerol, 15-20 g of corn starch, potato starch, sweet potato starch or pea starch, 10-15 g of talcum powder and 10-15 g of coconut oil acid, heating to 60-80 ℃, adding 20-30% sodium hydroxide to adjust the pH to be neutral, stirring for 30-50 min at the stirring speed of 1200-1600 r/min to obtain viscous soap solution, and putting the viscous soap solution into a mold for condensation and demolding to obtain the targeted drug soap containing the natural active dandelion extract.
6. The method for applying the targetable medicine of medical natural dandelion product extracted by the hydrothermal method of claim 2 to mainly treat dermatitis allergy is characterized in that: the method has the advantages that the dandelion is subjected to continuous extraction in a closed hydrothermal reaction kettle at a constant temperature and a high pressure in different sections, the solubility of each component in the dandelion raw material is increased by regulating and controlling reaction parameters, the method is high in extraction efficiency and product purity, the extract has a remarkable effect on treating various dermatitis, skin itch and pustular cyst, the recurrence phenomenon is avoided, the application potential in pharmacological research and medical drugs is large, and the extraction method has feasibility, high efficiency and novelty.
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