CN114588199A - Lonicera and Forsythia extract, and preparation method and application thereof - Google Patents

Lonicera and Forsythia extract, and preparation method and application thereof Download PDF

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CN114588199A
CN114588199A CN202011412268.8A CN202011412268A CN114588199A CN 114588199 A CN114588199 A CN 114588199A CN 202011412268 A CN202011412268 A CN 202011412268A CN 114588199 A CN114588199 A CN 114588199A
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acid
forsythia
extract
honeysuckle
decoction
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CN114588199B (en
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邓声菊
闫小君
罗进
车雨轩
车雨桐
顾馨云
黄鹏华
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Jiangsu Antae Biotechnology Co ltd
Chart Biotechnology Shanghai Co ltd
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Jiangsu Antae Biotechnology Co ltd
Chart Biotechnology Shanghai Co ltd
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Abstract

The invention relates to a honeysuckle and forsythia extract, a preparation method and application thereof, in particular to a process for ethanol extraction and chloroform extraction of the honeysuckle and forsythia extract and preparation conditions thereof, and the honeysuckle and forsythia extract is further prepared by acidified ethanol extraction and chloroform extraction and is used for preparing a pharmaceutical composition. The method provided by the invention obviously improves the content and extraction rate of chlorogenic acid in the lonicera and forsythia extract, and the chlorogenic acid is widely applied to preparation of medicines, health-care products, foods, cosmetics, special medical foods and the like, so that the effectiveness and safety of the products are guaranteed, and the method has the advantages of simplicity and convenience in operation, high extraction yield, high resource utilization rate, higher cost, greenness, environmental friendliness, suitability for industrial mass production and the like.

Description

Lonicera and Forsythia extract, and preparation method and application thereof
Technical Field
The invention relates to the field of traditional Chinese medicines, and in particular relates to a lonicera and forsythia extract, and a preparation method and application thereof.
Background
The flos Lonicerae is flower bud of Lonicera japonica Thunb, Lonicera japonica Thunb (Sweet) DC, Lonicera japonica Thunb, Lonicera hyogluca Miq, Lonicera fulvotomosa Hsu et S.C.Cheng. Honeysuckle is originally seen in Li Shizhen Ben Cao gang mu and loaded in Chinese pharmacopoeia, and has other names such as honeysuckle, honeysuckle flower, Erhua flower, Erbaohua flower and Shubaohua flower. Fructus forsythiae (Forsythia subspensa, Latin's name) is a shrub of Forsythia, Oleaceae, and Podophyllum of Dicotyledoneae. Fructus forsythiae can be used as a medicine.
The honeysuckle and the forsythia have the effects of clearing away heat and toxic materials, relieving exterior syndrome with pungent and cool natured drugs and the like, effectively inhibit the growth of various bacteria and viruses, have good effects of resisting inflammation and allergic reaction, improving the immunity of the organism and the like, and are effective components of various Chinese patent medicine compositions (such as Shuanghuanglian, Yinqiao powder and the like). Chlorogenic acid is a main drug effect component in the lonicera and forsythia extract and becomes a key index for testing the quality of the lonicera and forsythia extract. The preparation method of the honeysuckle flower and forsythia extract comprises a water extraction method, a water-alcohol extraction method, an alcohol-water extraction method, an ultrasonic enhanced leaching method and the like.
CN101390956A discloses a method for preparing a honeysuckle flower and forsythia suspense extract, which comprises the steps of soaking honeysuckle flower in warm water at 60-85 ℃ for 0.5-2 hours to obtain a honeysuckle flower warm soaking solution, extracting active ingredients in forsythia suspense by a decoction method to obtain a forsythia suspense decoction, collecting and combining the honeysuckle flower warm soaking solution and the forsythia suspense decoction, concentrating, and carrying out alcohol precipitation to obtain the honeysuckle flower and forsythia suspense extract. However, the chlorogenic acid content and the yield of the lonicera and forsythia extract obtained by the method are all required to be improved. Therefore, there is an urgent need to develop a lonicera and forsythia extract with high chlorogenic acid content and a preparation method thereof, so as to improve the quality and curative effect of the medicine and improve the resource utilization rate.
Disclosure of Invention
The invention aims to provide a honeysuckle and forsythia extract, which is prepared from honeysuckle and forsythia, wherein the mass ratio of the honeysuckle to the forsythia is 1:2-4:1, and the content of chlorogenic acid in the honeysuckle and forsythia extract is not lower than 18%.
In a preferred technical scheme of the invention, the content of chlorogenic acid in the lonicera and forsythia extract is not less than 20%.
In the preferred technical scheme of the invention, the mass ratio of the honeysuckle to the forsythia is 1:2-2: 1.
The invention also aims to provide a preparation method of the lonicera and forsythia extract, wherein the effective components of the lonicera and forsythia are honeysuckle and forsythia, the mass ratio of honeysuckle to forsythia is 1:2-4:1, and the preparation method of the lonicera and forsythia extract comprises the following steps:
1) weighing the required amount of honeysuckle and forsythia, mixing, adding 60-80% (V/V) ethanol solution, wherein the addition amount of the ethanol solution is 1-15 times (volume weight ratio) of the weight of the medicinal materials, heating, refluxing and extracting for 1-5 times, refluxing and extracting for 0.5-5 hours each time, filtering, collecting ethanol extract, adjusting the pH value of the filtrate to 5.5-8.5, standing, filtering, concentrating the filtrate, and preparing concentrated solution;
2) cooling the concentrated solution prepared in the step 1), filtering, extracting the filtrate by using chloroform, separating and removing chloroform extract, and drying to obtain the product.
In the preferred technical scheme of the invention, the mass ratio of the honeysuckle to the forsythia is 1:2-2: 1.
In the preferred technical scheme of the invention, in the step 1), before the heating reflux extraction, the medicinal materials are soaked in the ethanol solution, preferably for 1-12h, and more preferably for 2-10 h.
In a preferred embodiment of the present invention, the concentration of the ethanol solution is 65-75% (V/V), preferably 70% (V/V).
In the preferable technical scheme of the invention, the adding amount of the ethanol in the step 1) is 3-10 times (V/W) of the total weight of the medicinal materials, and preferably 4-8 times (V/W).
In the preferred technical scheme of the invention, the medicinal materials are added with the ethanol solution and are heated, refluxed and extracted for 2-4 times.
In the preferred technical scheme of the invention, the medicinal materials are added with the ethanol water solution and heated and refluxed for extraction for 1.0 to 4 hours, preferably 1.5 to 3 hours.
In the preferable technical scheme of the invention, the pH of the filtrate obtained in the step 1) is adjusted to 6.0-8.0, and the pH is preferably adjusted to 6.5-7.5.
In a preferred technical scheme of the invention, the acid-base substance for adjusting the pH of the filtrate is selected from any one of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, triethylamine, meglumine, hydrochloric acid, sulfuric acid, chloric acid, nitric acid, hydrobromic acid, hydrofluoric acid, phosphoric acid, sulfonic acid, malic acid, fumaric acid, citric acid, carboxylic acid, hydroxy acid, keto acid, oxalic acid, citric acid, succinic acid, formic acid, acetic acid, propionic acid, butyric acid, malonic acid, succinic acid, pyruvic acid, glutamic acid, tartaric acid, lactic acid, itaconic acid, ascorbic acid, fumaric acid, alpha-ketoglutaric acid, and fruit acid, or a combination thereof.
In a preferable technical scheme of the invention, the concentration of the acid-base substance solution is 0.5-8mol/L, preferably 0.8-6mol/L, and more preferably 1-5 mol/L.
In the preferable technical scheme of the invention, the filtrate obtained in the step 1) is kept stand for 2-50h, preferably 5-40h after the pH is adjusted.
In a preferred technical scheme of the invention, the filtrate obtained in the step 1) is concentrated until no alcohol smell exists.
In a preferred embodiment of the invention, the relative density of the concentrate in step 1) is 1.05 to 1.4 (measured at 60 ℃), preferably 1.10 to 1.35 (measured at 60 ℃).
In a preferred embodiment of the present invention, the concentration is selected from any one or a combination of vacuum concentration, membrane concentration, vacuum concentration and atmospheric concentration.
In the preferable technical scheme of the invention, the dosage of the chloroform in the step 2) is 0.05-0.5 time (V/W), preferably 0.1-0.4 time (V/W) of the weight of the medicinal materials.
According to the preferable technical scheme of the invention, the dosage of the chloroform in the step 2) is any one of 0.1 time, 0.11 time, 0.12 time, 0.13 time, 0.14 time, 0.15 time, 0.16 time, 0.17 time, 0.18 time, 0.19 time, 0.2 time, 0.25 time, 0.3 time, 0.35 time, 0.4 time, 0.45 time and 0.5 time of the weight (V/W) of the medicinal materials.
In a preferred embodiment of the invention, the cooling in step 2) is carried out to a temperature of 4 to 35 ℃, preferably 10 to 25 ℃.
According to the preferable technical scheme, after the filtrate in the step 2) is extracted by chloroform, standing is carried out for 0.5-12h, and preferably standing is carried out for 2-10 h.
In a preferred embodiment of the present invention, the drying is selected from any one or a combination of reduced pressure drying, vacuum drying, spray drying, atmospheric drying, and ebullient drying.
In a preferred technical scheme of the invention, the dried forsythia suspense extract prepared in the step 2) is pulverized, and preferably, the pulverization method is any one or a combination of an air flow pulverization method, a fluid grinding method, a colloid grinding method, a jet grinding method, a co-grinding method and a ball grinding method.
In a preferred technical scheme of the invention, the chlorogenic acid content in the lonicera and forsythia extract is not lower than 18%, and preferably not lower than 20%.
The invention also aims to provide a preparation method of the lonicera and forsythia extract, wherein the effective components of the lonicera and forsythia are honeysuckle and forsythia, the mass ratio of honeysuckle to forsythia is 1:2-4:1, and the preparation method of the lonicera and forsythia extract comprises the following steps:
1) weighing honeysuckle and fructus forsythiae in required amount, mixing, adding acidified ethanol solution with concentration of 60-80% (V/V), wherein the added amount of the acidified ethanol solution is 1-15 times (V/W) of the weight of the medicinal materials, heating and refluxing for 1-5 times, refluxing for 0.5-5 hours each time, filtering, collecting acidified ethanol extract, adjusting pH of the filtrate to 5.5-8.5, standing, filtering, and concentrating the filtrate to obtain concentrated solution;
2) cooling the concentrated solution prepared in the step 1), filtering, extracting the filtrate by using chloroform, separating and removing chloroform extract, and drying to obtain the product.
In the preferred technical scheme of the invention, the mass ratio of the honeysuckle to the forsythia is 1:2-2: 1.
In the preferable technical scheme of the invention, in the step 1), before the heating reflux extraction, the medicinal materials are soaked in the acidified ethanol solution, preferably for 1-12h, and more preferably for 2-10 h.
In a preferred embodiment of the present invention, the concentration of the acidified ethanol solution is 65-75% (V/V), preferably 70% (V/V).
In the preferable technical scheme of the invention, the adding amount of the acidified ethanol in the step 1) is 3-10 times (V/W) of the total weight of the medicinal materials, and preferably 4-8 times (V/W).
In a preferred technical scheme of the invention, the pH of the acidified ethanol solution is 3-6, and the pH of the acidified ethanol solution is preferably 4-5.
In a preferred embodiment of the present invention, the acid used for adjusting the pH of the acidified ethanol solution is selected from any one of hydrochloric acid, sulfuric acid, chloric acid, nitric acid, hydrobromic acid, hydrofluoric acid, phosphoric acid, sulfonic acid, malic acid, fumaric acid, citric acid, carboxylic acid, hydroxy acid, keto acid, acetic acid, oxalic acid, citric acid, succinic acid, formic acid, acetic acid, propionic acid, butyric acid, malonic acid, succinic acid, pyruvic acid, glutamic acid, tartaric acid, lactic acid, itaconic acid, ascorbic acid, fumaric acid, α -ketoglutaric acid, and fruit acid, or a combination thereof.
In a preferred embodiment of the present invention, the acid concentration used to adjust the pH of the acidified aqueous ethanol solution is 0.5 to 8mol/L, preferably 0.8 to 6mol/L, more preferably 1 to 5 mol/L.
In the preferred technical scheme of the invention, the medicinal materials are added with acidified ethanol solution and are heated, refluxed and extracted for 2-4 times.
In the preferred technical scheme of the invention, the acidified ethanol water solution is added into the medicinal materials, and the heating reflux extraction time is 1.0-4h, preferably 1.5-3 h.
In the preferable technical scheme of the invention, the pH of the filtrate obtained in the step 1) is adjusted to 6.0-8.0, and the pH is preferably adjusted to 6.5-7.5.
In a preferred technical scheme of the present invention, the acid-base substance for adjusting the pH of the filtrate is selected from any one of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, triethylamine, meglumine, hydrochloric acid, sulfuric acid, chloric acid, nitric acid, hydrobromic acid, hydrofluoric acid, phosphoric acid, sulfonic acid, malic acid, fumaric acid, citric acid, carboxylic acid, hydroxy acid, keto acid, oxalic acid, citric acid, succinic acid, formic acid, acetic acid, propionic acid, butyric acid, malonic acid, succinic acid, pyruvic acid, glutamic acid, tartaric acid, lactic acid, itaconic acid, ascorbic acid, fumaric acid, alpha-ketoglutaric acid, and fruit acid, or a combination thereof.
In a preferable scheme of the invention, the concentration of the acid-base substance for adjusting the pH of the filtrate is 0.5-8mol/L, preferably 0.8-6mol/L, and more preferably 1-5 mol/L.
In the preferable technical scheme of the invention, the filtrate obtained in the step 1) is kept stand for 2-50h, preferably 5-40h after the pH is adjusted.
In a preferred technical scheme of the invention, the filtrate obtained in the step 1) is concentrated until no alcohol smell exists.
In a preferred embodiment of the invention, the relative density of the concentrate in step 1) is 1.05 to 1.4 (measured at 60 ℃), preferably 1.10 to 1.35 (measured at 60 ℃).
In a preferred embodiment of the present invention, the concentration is selected from any one or a combination of vacuum concentration, membrane concentration, vacuum concentration and atmospheric concentration.
In the preferable technical scheme of the invention, the dosage of the chloroform in the step 2) is 0.05-0.5 time (V/W), preferably 0.1-0.4 time (V/W) of the weight of the medicinal materials.
According to the preferable technical scheme of the invention, the dosage of the chloroform in the step 2) is any one of 0.1 time, 0.11 time, 0.12 time, 0.13 time, 0.14 time, 0.15 time, 0.16 time, 0.17 time, 0.18 time, 0.19 time, 0.2 time, 0.25 time, 0.3 time, 0.35 time, 0.4 time, 0.45 time and 0.5 time of the weight (V/W) of the medicinal materials.
In a preferred embodiment of the invention, the cooling in step 2) is carried out to a temperature of 4 to 35 ℃, preferably 10 to 25 ℃.
According to the preferable technical scheme, after the filtrate in the step 2) is extracted by chloroform, standing is carried out for 0.5-12h, and preferably standing is carried out for 2-10 h.
In a preferred embodiment of the present invention, the drying is selected from any one or a combination of reduced pressure drying, vacuum drying, spray drying, atmospheric drying, and ebullient drying.
In the preferable technical scheme of the invention, the dry extract prepared in the step 2) is crushed, and the crushing method is preferably selected from any one or the combination of a jet milling method, a fluid milling method, a colloid milling method, a jet milling method, a co-milling method and a ball milling method.
In a preferred technical scheme of the invention, the chlorogenic acid content in the lonicera and forsythia extract is not lower than 18%, and preferably not lower than 20%.
The invention also aims to provide a lonicera and forsythia pharmaceutical composition which comprises a lonicera and forsythia extract and a pharmaceutically acceptable carrier.
In a preferred embodiment of the present invention, the pharmaceutical composition further comprises other pharmaceutically active ingredients.
The pharmaceutical compositions of the present invention may be in various dosage forms well known in the art and may be prepared using formulation techniques conventional in the art.
In a preferred embodiment of the present invention, the preparation of the present invention is selected from any one of an injection, an oral preparation and an external preparation.
In a preferred technical scheme of the invention, the injection preparation comprises but is not limited to any one of injection or freeze-dried powder.
In a preferred technical scheme of the invention, the oral preparation is selected from any one of oral liquid preparation, tablets, capsules, granules, syrup, powder, distillate, effervescent agent, spray, suspension, pills, dripping pills, mixture, paste, emulsion and tea.
In a preferred technical scheme of the invention, the external preparation is any one selected from gels, ointments, emplastrums, creams, ointments, liniments, lotions, suppositories, smearing agents, jellies, ointments and atomizing agents.
In a preferred embodiment of the present invention, the pharmaceutically acceptable carrier is a conventional excipient or adjuvant known in the art for preparing a desired preparation.
The common excipients or auxiliary materials of the injection, oral preparation or external preparation include but are not limited to solvents, cosolvents, isotonic regulators, pH regulators, adsorbents, complexing agents, fillers (also called diluents), lubricants (also called glidants or antiadherents), dispersants, wetting agents, binders, disintegrants, regulators, solubilizers, antioxidants, bacteriostats, emulsifiers, flavoring agents, perfuming agents and the like. The solvent comprises water for injection and non-aqueous solvent, wherein the non-aqueous solvent comprises ethanol, propylene glycol, vegetable oil (soybean oil, safflower oil, sesame oil, cottonseed oil, fish oil, etc.); the cosolvent comprises organic acid and its sodium salt and amide and amine, such as malic acid, methionine, arginine, sodium benzoate, sodium salicylate, sodium p-aminobenzoate, urethane, urea, nicotinamide, glucose, meglumine, vitamin B6, etc.; isotonic regulators, such as sodium chloride, glucose, mannitol, fructose, glycerol, sorbitol, xylitol, magnesium chloride, phosphate, sodium citrate, etc.; pH regulators, hydrochloric acid, sulfuric acid, lactic acid, malic acid, acetic acid, citric acid, sodium hydroxide, sodium carbonate, sodium bicarbonate, sodium hydroxide, potassium hydroxide, sodium citrate, potassium citrate, sodium malate, potassium malate, disodium hydrogen phosphate, dipotassium hydrogen phosphate, sodium dihydrogen phosphate, potassium carbonate, potassium hydrogen carbonate, and the like; a binder, such as syrup, acacia, gelatin, sorbitol, tragacanth, cellulose or a derivative thereof selected from any one or a combination of microcrystalline cellulose, sodium carboxymethylcellulose, ethylcellulose, hydroxypropylmethylcellulose, polyvinylpyrrolidone, or the like, a starch derivative selected from any one or a combination of sodium carboxymethyl starch, sodium starch glycolate, pregelatinized starch, modified starch, hydroxypropyl starch, corn starch; fillers, such as lactose, powdered sugar, dextrin, starch or derivatives thereof, cellulose or derivatives thereof, inorganic calcium salts, sorbitol, glycine and the like, preferably the inorganic calcium salts are selected from calcium chloride, calcium sulfate, calcium phosphate, calcium hydrogen phosphate, precipitated calcium carbonate and the like, preferably the cellulose derivatives are selected from any one of microcrystalline cellulose, sodium carboxymethyl cellulose, ethyl cellulose, hydroxypropyl methyl cellulose, preferably the starch derivatives are selected from any one of sodium carboxymethyl starch, sodium starch glycolate, pregelatinized starch, modified starch, hydroxypropyl starch, corn starch or combinations thereof; lubricants such as aerosil, magnesium stearate, talc, colloidal silica, aluminum hydroxide, boric acid, hydrogenated vegetable oil, polyethylene glycol and the like; disintegrants, such as starch or its derivatives, polyvinylpyrrolidone, cross-linked polyvinylpyrrolidone, microcrystalline cellulose, etc., preferably starch derivatives selected from any one or combination of sodium carboxymethyl starch, sodium starch glycolate, pregelatinized starch, modified starch, hydroxypropyl starch, corn starch; wetting agents such as sodium lauryl sulfate, water or alcohols, and the like. Antioxidants such as L-cysteine hydrochloride, sodium sulfite, sodium bisulfite, sodium metabisulfite, propyl gallate, glutathione, sodium thiosulfate, thiourea, thioglycolic acid, sodium metabisulfite, potassium metabisulfite, dibutylphenylic acid, vitamin E, and the like; bacteriostatic agents (bactericides) such as 0.5% phenol, 0.3% cresol, 0.5% chlorobutanol and the like; emulsifiers such as polysorbate-80, sorbitan elaeate, pluronic F-68, lecithin, soy lecithin, poloxamers, cholesterol, glycerol monooleate, and the like; solubilizers, such as poloxamers, tween-80, bile, glycerol, and the like; flavoring agents, such as honey, syrup, and the like.
In a preferred technical scheme of the invention, the lonicera and forsythia extract is mixed with a pharmaceutically acceptable slow release preparation carrier or controlled release preparation carrier according to the preparation requirements, and then the lonicera and forsythia extract is prepared into pellets, such as slow release pellets or controlled release pellets, according to the preparation method of the slow release preparation or controlled release preparation known in the art, such as adding a retardant coating or microencapsulating the lonicera extract. The slow release preparation carrier or the controlled release preparation carrier comprises but is not limited to an oil-fat doping agent, a hydrophilic colloid or a coating retarder and the like, wherein the oil-fat doping agent is selected from glyceryl monostearate, hydrogenated castor oil, mineral oil, polysiloxane or dimethyl siloxane and the like; the hydrophilic colloid is selected from any one or combination of sodium carboxymethylcellulose, hydroxypropyl cellulose, hydroxypropyl methylcellulose, polyvinylpyrrolidone (PVP), acacia gum, tragacanth gum or carbopol; the coating retarder is selected from Ethyl Cellulose (EC), hydroxypropyl methyl cellulose (HMPC), polyvinylpyrrolidone (PVP), Cellulose Acetate Phthalate (CAP), acrylic resin, etc.
In a preferred embodiment of the present invention, the amount or type of the pharmaceutically acceptable carrier in the pharmaceutical composition is determined by the physicochemical properties and content of the active ingredient in the pharmaceutical composition, the type of the preparation, the dissolution and bioavailability of the preparation, and other factors.
In a preferred embodiment of the present invention, the pharmaceutical composition further comprises other pharmaceutically active ingredients.
The invention also aims to provide application of the honeysuckle and forsythia extract or the pharmaceutical composition thereof in preparing a medicament, wherein the medicament has any one or combination of efficacies of relieving exterior syndrome, purging, clearing heat, cooling blood, stopping dysentery, dispelling summer heat, eliminating phlegm, tonifying, detoxifying, clearing damp, treating carbuncle, treating wind, resisting bacteria, resisting inflammation, resisting viruses and/or enhancing immunity.
In a preferred technical scheme, the medicament is selected from yinqiao powder, shuanghuanglian oral liquid, yinqiao tablet, vic yinqiao tablet, yinqiao detoxicating tablet, qingying decoction, newly flavored elsholtzia drink, antelope cold capsule, lianhua antipyretic capsule, yinqiao detoxifying pill, yinqiao powder and plus and minus prescription thereof, honeysuckle decoction, yinqiao puffball powder, heat-clearing and detoxifying mixture, eruption cooling and detoxifying decoction, throat-clearing and diaphragm-relieving decoction, yin-blossom detoxifying decoction, wind-dispelling and heat-clearing decoction, summer-heat-clearing decoction, platycodon almond decoction, forsythia detoxifying powder, hydrangea agglomerans, pus-drawing ointment, baifang live-relieving decoction, baihu detoxifying and yin-nourishing decoction, baijie-resolving powder, septicemia decoction, mint forsythia formula, mint decoction, saliva or, radix bupleuri liver-clearing decoction, intestinal abscess decoction, pus-drawing powder, dampness-eliminating decoction, hemorrhoid-eliminating pill, hemorrhoid-eliminating and detoxifying pill, elephant prescription, large nourishing decoction, angelica decoction, decoction for treating furuncle, decoction for treating, Two-activating powder, twenty-four-ingredient feng liu yin, ledebouriella root bi xiao powder, ledebouriella root-angelica decoction, lung abscess decoction, monkshood toxin-vanquishing decoction, compound sargentgloryvine decoction, compound detumescence and collateral-dredging decoction, recovery qi-dredging powder, recovery vital qi powder, cold decoction No. 1, pathogen-attacking and flow-stopping decoction, yin-returning and toxin-removing decoction, fleece-flower root decoction, pus-expelling and flesh-strengthening ointment, pus-expelling and flesh-growing ointment, flax decoction, toxin-removing and swelling-relieving and toxin-expelling powder, toxin-removing decoction, muscle-changing and disinfection powder, jaundice decoction, golden toxin-removing decoction, golden thread toxin-removing and flavoring decoction, golden thread bitter-saving decoction, Huangqi yin-dispersing decoction, milk-returning formula, life-activating decoction, acute white decoction, lung-clearing and swelling-eliminating decoction, modified Sheng Ge decoction, modified Zhu Yu Shi Gao decoction, modified Zhu Shi Gao Shi decoction, modified zhu Shi Ji Zhu Ji Tang (decoction), yin-removing and toxin-removing decoction, modified decoction, yin-removing and phlegm-removing decoction, added heat-clearing and toxin-removing decoction, added heat-clearing and dampness-removing decoction, yin-clearing and toxin-removing decoction, added heat-clearing decoction, added Bai-removing decoction, yin-removing and toxin-removing decoction, yin-removing decoction, added Bai decoction, yin-removing and toxin-removing decoction, yin-removing and toxin-removing decoction, added heat-removing decoction, added heat-removing decoction, heat-removing and toxin-removing decoction, heat-removing and dampness-removing decoction, and dampness removing decoction, and toxin-removing decoction, added Bai-removing decoction, and toxin-removing decoction for nourishing decoction, and toxin-removing decoction for nourishing decoction, and toxin-removing decoction, and nourishing decoction, and toxin-removing, Detoxifying yin-nourishing decoction, detoxifying interior-supporting powder, detoxifying interior-eliminating decoction, detoxifying yinqiang decoction, detoxifying and heat-clearing decoction, detoxifying Tianjiang powder, antipyretic and toxin-resolving decoction, golden shellfish decoction, small rat sticking decoction, golden pill, golden-silk wanying paste, honeysuckle and bunge corydalis powder, golden silver five spice decoction, Jingfang detoxification decoction, Jingfang burdock decoction, Jingfang Xiahua powder, Schizonepeta herba vendor toxicity powder, Jiwei detoxification decoction, Jiwei flowing qi decoction, Kai-shui qi detoxification decoction, antitoxic pill, Kunhua decoction, trichosanthes and burdock decoction, appendicitis mixture, appendicitis decoction, forsythia antiphlogistic ointment, forsythia antiphlogistic pill, forsythia tail decoction, forsythia astragalus decoction, forsythia detoxication decoction, forsythia antidotal pill, forsythia bulbus fritillariae thunbergii decoction, forsythia orange decoction, forsythia radix rehmanniae decoction, forsythia tropis powder, chrysanthemum wild chrysanthemum powder, blood-cooling wind-cooling pill, scrofula liver-soothing pill, interior-supporting disinfection powder, gold interior-clearing decoction, throat-clearing decoction, forsythia toxin-clearing decoction, Qianjin-throat powder, Qianjin-clearing decoction, and throat-clearing decoction, The decoction can be any one of a appendicitis clearing liquid, a heat-clearing and detoxifying decoction, a heat-clearing and detoxifying and detumescence decoction, a heat-clearing and detoxifying powder, a stomach-clearing and detoxifying powder, a throat-clearing and diaphragm-benefiting decoction, a wind-dispelling powder, a mulberry soup, a profuse health decoction, a cimicifuga foetida sterilizing decoction, a liver-soothing and detoxifying decoction, a toxin-expelling decoction, a Torilis honeysuckle and bunge corydalis powder, a Torilis pus-expelling decoction, a perfect pill, a Xianyi grain decoction, a sterilizing powder, a wind-dispelling and detoxifying powder, a breast cancer-eliminating pill, an carbuncle-eliminating decoction, a pungent-cool heat-clearing and detoxifying decoction, a honeysuckle and a Yinji decoction.
The invention also aims to provide application of the lonicera and forsythia extract or the pharmaceutical composition in preparing any one of health-care products, food, cosmetics and special medical food, wherein any one of the health-care products, the food, the cosmetics and the special medical food has any one or combination of efficacies of relieving exterior syndrome, purging, clearing heat, cooling blood, stopping dysentery, dispelling summer heat, eliminating phlegm, tonifying, detoxifying, clearing damp, treating carbuncle, treating wind, resisting bacteria, resisting inflammation, resisting viruses and/or enhancing immunity.
The 75% ethanol solution refers to 75% ethanol water solution by volume fraction. Other concentrations of ethanol are also referred to as volume fractions.
The method for measuring the content of chlorogenic acid in the lonicera and forsythia extract refers to the new medicine conversion standard of 'Shuanghuanglian powder injection (freeze-dried)' [ WS 3-054 (Z-011) '-99 (Z)'.
Unless otherwise indicated, when the present invention relates to percentages between liquids, said percentages are volume/volume percentages; the invention relates to the percentage between liquid and solid, said percentage being volume/weight percentage; the invention relates to the percentages between solid and liquid, said percentages being weight/volume percentages; the balance being weight/weight percent.
Compared with the prior art, the invention has the following beneficial effects:
1. the honeysuckle and forsythia extract has high chlorogenic acid content, is loose powder or is loose powder after dry paste is crushed, has low water content and is difficult to absorb moisture, the hygroscopicity is obviously lower than that of similar products, the dissolution is easy, and the redissolved liquid is clear and transparent, so that the quality and the curative effect of the medicine are obviously improved, and the effectiveness and the medication safety of the medicine are ensured.
2. The invention optimizes the technological parameters and conditions, and obviously improves the content and extraction rate of chlorogenic acid; the method creatively adopts acidified ethanol extraction and chloroform extraction, so that the content and the extraction rate of the chlorogenic acid are obviously improved, the chlorogenic acid is widely applied to preparation of medicines, health-care products, foods, cosmetics, special medical foods and the like, and the effectiveness and the safety of the products are guaranteed.
3. The preparation method of the lonicera and forsythia extract has the advantages of simple and convenient operation, high extraction yield, high resource utilization rate, more excellent cost, greenness and environmental protection, and is suitable for industrial mass production.
Detailed Description
The present invention will be specifically described with reference to examples. The embodiments of the present invention are only for illustrating the technical solutions of the present invention, and do not limit the essence of the present invention.
Example 1Preparation method of Lonicera and Forsythia extract
The preparation method of the lonicera and forsythia extract comprises the following steps:
1) weighing 50g of honeysuckle and 100g of fructus forsythiae, crushing, sieving by a 12mm sieve, adding 70% ethanol solution (V/W) which is 8 times of the weight of the medicinal materials, standing and soaking for 10 hours, performing reflux extraction for 3 hours, filtering, and collecting filtrate;
2) adding 3mol/L sodium hydroxide solution into the filtrate, adjusting pH to 7.0, standing for 6h, filtering, concentrating the filtrate, recovering ethanol until no alcohol smell exists, obtaining concentrated solution, measuring the relative density at 60 ℃ to be 1.05, cooling the concentrated solution to be 15 ℃, filtering, adding 27ml chloroform for extraction, standing for 0.5h, removing chloroform extract, and drying at the temperature of below 90 ℃ to obtain the lonicera and forsythia extract with the chlorogenic acid content of 22.62%, the yield is 10%, and the water content is 2.07%.
Example 2Preparation of Lonicera and Forsythia extract
The preparation method of the lonicera and forsythia extract comprises the following steps:
1) weighing 75g of honeysuckle and 150g of fructus forsythiae, crushing, sieving by a 12mm sieve, adding a 65% ethanol solution (V/W) which is 8 times of the weight of the medicinal materials, standing, soaking for 8.5h, performing reflux extraction for 1.5h, and filtering to obtain a filtrate;
2) adding 65% ethanol solution (V/W) 6 times the weight of the medicinal materials into the filter residue, reflux extracting for 1.5 hr, filtering, and collecting filtrate;
3) mixing the two filtrates, adding 5mol/L sodium carbonate solution into the filtrate, adjusting pH to 7.0, standing for 6h, filtering, concentrating the filtrate, recovering ethanol until no alcohol smell is obtained to obtain concentrated solution, measuring relative density at 60 deg.C to 1.10, cooling the concentrated solution to 30 deg.C, filtering, adding 45ml chloroform for extraction, standing for 1h, removing chloroform extract, and oven drying at 90 deg.C or below to obtain Lonicera Fortunei extract with chlorogenic acid content of 21.94%, yield of 13.78%, and water content of 2.08%.
Example 3Preparation of Lonicera and Forsythia extract
The preparation method of the lonicera and forsythia extract comprises the following steps:
1) weighing 100g of honeysuckle and 200g of fructus forsythiae, adding 70% ethanol solution (V/W) 6 times of the weight of the medicinal materials, standing, soaking for 4 hours, extracting for 1.5 hours under reflux, and filtering to obtain filtrate;
2) adding 70% (V/V) ethanol solution (V/W) 5 times the weight of the medicinal materials into the filter residue, reflux-extracting for 1h, filtering, and collecting filtrate;
3) mixing the two filtrates, adding 5mol/L triethylamine into the filtrate to adjust pH to 7.0, standing for 6h, filtering, concentrating the filtrate to recover ethanol until no alcohol smell exists to obtain a concentrated solution, measuring the relative density at 60 ℃ to be 1.15, cooling the concentrated solution to 10 ℃, filtering, adding 45ml chloroform for extraction, standing for 3h, removing the chloroform extract, and drying at the temperature of below 90 ℃ to obtain the lonicera and forsythia extract with the chlorogenic acid content of 26.59%, wherein the yield is 15.33% and the water content is 2.68%.
Example 4Preparation of Lonicera and Forsythia extract
The preparation method of the lonicera and forsythia extract comprises the following steps:
1) weighing 50g of honeysuckle and 100g of fructus forsythiae, crushing, sieving by a 12mm sieve, adding 70% acidified ethanol solution (pH is adjusted to 6 by 0.5mol/L hydrochloric acid) (V/W) 6 times of the weight of the medicinal materials, standing and soaking for 5h, performing reflux extraction for 1.5h, and filtering to obtain filtrate;
2) adding 70% acidified ethanol solution (pH adjusted by 0.5mol/L hydrochloric acid to 6) 5 times the weight of the medicinal materials into the filter residue, reflux-extracting for 2 hr, filtering, and collecting filtrate;
3) mixing the two filtrates, adding 5mol/L sodium hydroxide solution into the filtrate to adjust pH to 7.0, standing for 8 hr, filtering, concentrating the filtrate, recovering ethanol until no alcohol smell exists to obtain concentrated solution, and measuring relative density at 60 deg.C to obtain 1.20; cooling the concentrated solution to 4 deg.C, filtering, extracting the filtrate with 25ml chloroform, standing for 5 hr, removing chloroform extract, oven drying below 90 deg.C to obtain fructus forsythiae extract with chlorogenic acid content of 20.88%, and pulverizing to obtain brown powder with yield of 21.67% and water content of 3.02%.
Example 5Lonicera and Forsythia extractPreparation of
The preparation method of the lonicera and forsythia extract comprises the following steps:
1) weighing 50g of honeysuckle and 100g of fructus forsythiae, crushing, sieving by a 12mm sieve, adding 70% acidified ethanol solution (pH is adjusted to 4 by 1mol/L hydrochloric acid) (V/W) which is 8 times of the weight of the medicinal materials, standing, soaking for 2h, performing reflux extraction for 3h, and filtering to obtain filtrate;
2) adding 70% acidified ethanol solution (pH adjusted by 1mol/L hydrochloric acid 4) (V/W) with 5 times of the weight of the medicinal materials into the filter residue, reflux-extracting for 1.5h, filtering, and collecting the filtrate;
3) mixing the two filtrates, adding 5mol/L sodium carbonate solution into the filtrate to adjust pH to 7.0, standing for 6 hr, filtering, concentrating the filtrate, recovering ethanol until no alcohol smell is obtained to obtain concentrated solution, and measuring relative density at 60 deg.C to obtain 1.25; cooling the concentrated solution to 20 deg.C, filtering, extracting the filtrate with 35ml chloroform, standing for 7 hr, removing chloroform extract, oven drying below 90 deg.C to obtain fructus forsythiae extract with chlorogenic acid content of 21.29%, yield of 22.15%, and water content of 3.42%.
Example 6Preparation of Lonicera and Forsythia extract
The preparation method of the lonicera and forsythia extract comprises the following steps:
1) weighing 100g of honeysuckle and 100g of fructus forsythiae, crushing, sieving by a 12mm sieve, adding 8 times of 75% acidified ethanol solution (2mol/L acetic acid for regulating pH to 5) (V/W), standing and soaking for 2h, performing reflux extraction for 1.5h, and filtering to obtain filtrate;
2) adding acidified ethanol solution (pH 5 adjusted by 2mol/L acetic acid) (V/W) 6 times of the medicinal materials into the residue, reflux-extracting for 1.5 hr, filtering, and collecting filtrate;
3) mixing the two filtrates, adding 5mol/L triethylamine into the filtrate to adjust the pH value to 7.5, standing for 12h, filtering, concentrating the filtrate to recover ethanol until no alcohol smell exists to obtain a concentrated solution, and measuring the relative density to be 1.30 at 60 ℃; cooling the concentrated solution to 20 deg.C, extracting the filtrate with 43ml chloroform, standing for 10 hr, removing chloroform extract, oven drying below 90 deg.C to obtain fructus forsythiae extract with chlorogenic acid content of 23.71%, yield 25.49%, and water content 2.69%.
Example 7Preparation method of Lonicera and Forsythia extract
The preparation method of the honeysuckle flower and forsythia extract comprises the following steps:
1) weighing 100g of honeysuckle and 100g of fructus forsythiae, crushing, sieving by a 12mm sieve, adding 70% acidified ethanol aqueous solution (pH is adjusted by acetic acid of 5mol/L and 3) (V/W) which is 7 times of the weight of the medicinal materials, standing and soaking for 8 hours, performing reflux extraction for 2 hours, and filtering to obtain filtrate;
2) adding 70% acidified ethanol solution (pH adjusted by 5mol/L acetic acid 3) (V/W) 6 times the weight of the medicinal materials into the filter residue, reflux extracting for 1.5h, filtering, and collecting filtrate;
3) mixing the two filtrates, adding 5mol/L sodium carbonate solution into the filtrate to adjust pH to 7.0, standing for 12 hr, filtering, concentrating the filtrate, recovering ethanol until no alcohol smell exists to obtain concentrated solution, and measuring relative density at 60 deg.C to obtain 1.35; cooling the concentrated solution to 15 deg.C, adding 70ml chloroform for extraction, standing for 12 hr, removing chloroform extract, oven drying at 90 deg.C or below to obtain fructus forsythiae extract with chlorogenic acid content of 22.32%, yield of 24.52%, and water content of 3.30%.
The dried paste of the lonicera and forsythia extract prepared in examples 1-7 is brown powder after being crushed, has no moisture absorption phenomenon after being placed in a natural environment, is clear after being redissolved by water, has no insoluble substance or floccule, and has high light transmittance.
Comparative example 1Preparation of Lonicera and Forsythia extract
The preparation method of the lonicera and forsythia extract comprises the following steps:
1) soaking 50g of honeysuckle and 100g of weeping forsythia in warm water for 30 minutes, decocting twice, each time lasts for 1.5 hours, combining the decoctions, filtering, and concentrating the filtrate to obtain clear paste with the relative density of 1.20-1.25 (70-80 ℃);
2) cooling the clear paste prepared in the step 1) to 40 ℃, slowly adding ethanol to ensure that the ethanol content reaches 75%, fully stirring, standing for 12 hours, filtering to obtain supernatant, adding a proper amount of 75% ethanol into residues, uniformly stirring, standing for 12 hours, filtering, combining ethanol solutions, recovering ethanol until no ethanol smell exists, drying, measuring the content of chlorogenic acid to be 8.49%, and obtaining the yield of 10.08%. The honeysuckle and forsythia extract is smashed into dark brown powder, and black insoluble substances and a small amount of floccules exist in the re-dissolved solution.
The above description of the specific embodiments of the present invention is not intended to limit the present invention, and those skilled in the art may make various changes and modifications according to the present invention without departing from the spirit of the present invention, which is defined in the appended claims.

Claims (10)

1. The preparation method of the honeysuckle and forsythia extract is characterized in that the honeysuckle extract and the forsythia are prepared, wherein the weight ratio of the honeysuckle to the forsythia is 1:2-4:1, and the preparation method of the honeysuckle extract comprises the following steps:
1) weighing the required amount of honeysuckle and forsythia, mixing, adding 60-80% (V/V) ethanol solution, wherein the addition amount of the ethanol solution is 1-15 times (volume weight ratio) of the weight of the medicinal materials, heating, refluxing and extracting for 1-5 times, refluxing and extracting for 0.5-5 hours each time, filtering, collecting ethanol extract, adjusting the pH value of the filtrate to 5.5-8.5, standing, filtering, concentrating the filtrate, and preparing concentrated solution;
2) cooling the concentrated solution prepared in the step 1), filtering, extracting the filtrate by using chloroform, separating and removing chloroform extract, and drying to obtain the product.
2. The preparation method of the honeysuckle and forsythia extract is characterized in that the honeysuckle extract and the forsythia are prepared, wherein the weight ratio of the honeysuckle to the forsythia is 1:2-4:1, and the preparation method of the honeysuckle extract comprises the following steps:
1) weighing the required amount of honeysuckle and forsythia, mixing, adding 60-80% acidified ethanol solution, wherein the adding amount of the acidified ethanol solution is 1-15 times of the weight of the medicinal materials, heating, refluxing and extracting for 1-5 times, refluxing and extracting for 0.5-5 hours each time, filtering, collecting acidified ethanol extract, adjusting the pH value of the filtrate to 5.5-8.5, standing, filtering, concentrating the filtrate, and preparing concentrated solution;
2) cooling the concentrated solution prepared in the step 1), filtering, extracting the filtrate by using chloroform, separating and removing chloroform extract, and drying to obtain the product.
3. The method according to claim 2, wherein the acid for adjusting the pH of the acidified ethanol solution is selected from any one of hydrochloric acid, sulfuric acid, chloric acid, nitric acid, hydrobromic acid, hydrofluoric acid, phosphoric acid, sulfonic acid, malic acid, fumaric acid, citric acid, carboxylic acid, hydroxy acid, keto acid, glacial acetic acid, oxalic acid, citric acid, succinic acid, formic acid, acetic acid, propionic acid, butyric acid, malonic acid, succinic acid, pyruvic acid, glutamic acid, tartaric acid, lactic acid, itaconic acid, ascorbic acid, fumaric acid, alpha-ketoglutaric acid, and fruit acid, or a combination thereof.
4. The process according to any one of claims 2 or 3, wherein the pH of the acidified ethanol solution is adjusted with an acid concentration of 0.5 to 8mol/L, preferably 0.8 to 6mol/L, more preferably 1 to 5 mol/L.
5. The honeysuckle and forsythia suspense extract is characterized by being prepared from honeysuckle and forsythia suspense, wherein the weight ratio of the honeysuckle to the forsythia suspense is 1:2-4:1, and the content of chlorogenic acid in the honeysuckle and forsythia suspense extract is not lower than 18%.
6. The extract as claimed in claim 5, wherein the weight ratio of honeysuckle flower to forsythia suspensa is 1:2-2: 1.
7. The extract according to any one of claims 5 to 6, wherein the content of chlorogenic acid in the lonicera and forsythia extract is not less than 18%.
8. A pharmaceutical composition comprising the lonicera and forsythia extract as claimed in any one of claims 1 to 7 and a pharmaceutically acceptable carrier.
9. Use of the lonicera and forsythia extract or the pharmaceutical composition of any one of claims 1 to 8 for preparing a medicament, wherein the medicament has any one or a combination of efficacies of relieving exterior syndrome, purging, clearing heat, cooling blood, stopping dysentery, dispelling summer heat, eliminating phlegm, tonifying, detoxifying, eliminating dampness, treating carbuncle, treating wind, resisting bacteria, resisting inflammation, resisting viruses and/or enhancing immunity.
10. Use of the lonicera and forsythia extract or the pharmaceutical composition according to any one of claims 1 to 8 for preparing any one of health products, foods, cosmetics and special medical foods, wherein any one of the health products, the foods, the cosmetics and the special medical foods has any one or combination of efficacies of relieving exterior syndrome, purging, clearing heat, cooling blood, stopping dysentery, dispelling summer heat, eliminating phlegm, tonifying, detoxifying, clearing damp, treating carbuncle, treating wind, resisting bacteria, resisting inflammation, resisting viruses and/or enhancing immunity.
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