CN114588199B - A fructus forsythiae extract, and its preparation method and application - Google Patents

A fructus forsythiae extract, and its preparation method and application Download PDF

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CN114588199B
CN114588199B CN202011412268.8A CN202011412268A CN114588199B CN 114588199 B CN114588199 B CN 114588199B CN 202011412268 A CN202011412268 A CN 202011412268A CN 114588199 B CN114588199 B CN 114588199B
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acid
extract
filtrate
fructus forsythiae
concentration
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CN114588199A (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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Chart Biotechnology Shanghai Co ltd
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Abstract

The invention relates to a fructus forsythiae extract, a preparation method and application thereof, in particular to a process for ethanol extraction and chloroform extraction of the fructus forsythiae extract and preparation conditions thereof, wherein the preparation method further comprises the steps of preparing the fructus forsythiae extract by acidified ethanol extraction and chloroform extraction, and using the prepared fructus forsythiae extract for preparing a pharmaceutical composition. The method of the invention obviously improves the content and the extraction rate of the chlorogenic acid in the Yinqiao extract, widens the application of the Yinqiao extract in preparing medicines, health products, foods, cosmetics, special medical foods and the like, ensures the effectiveness and the safety of the products, and has the advantages of simple operation, high extraction yield, high resource utilization rate, better cost, environmental protection, suitability for industrialized mass production and the like.

Description

A fructus forsythiae extract, and its preparation method and application
Technical Field
The invention relates to the field of traditional Chinese medicines, in particular to a Yinqiao extract, a preparation method and application thereof.
Background
The flos Lonicerae is flower bud of Lonicera japonica of Caprifoliaceae Lonicera japonica Thunb, lonicera confusa (Sweet) DC, lonicera japonica Lonicera hypoglauca Miq, and Lonicera falcata Lonicera fulvotomentosa Hsu et S.C.Cheng. The honeysuckle flower is originally found in Li Shizhen (compendium of materia Medica) and loaded in Chinese pharmacopoeia, and is also called as "honeysuckle flower", "double precious flower" and the like. Fructus forsythiae (Latin brand name: forsythia suspensa) is deciduous shrubs of the genus Forsythia of the order Dicotyledonary, order Papaverales, family Oleaceae. Fructus forsythiae fruit can be used as medicine.
The honeysuckle and the weeping forsythiae capsule have the effects of clearing heat and detoxicating, relieving exterior syndrome with pungent and cool natured drugs and the like, effectively inhibit the growth of various bacteria and viruses, have good anti-inflammatory, antiallergic and immunity improving effects and the like, and become the effective components of a plurality of Chinese patent medicine formulas (such as double coptis chinensis, yinqiao powder and the like). Chlorogenic acid is a main medicinal component in the fructus forsythiae extract and becomes a key index for detecting the quality of the fructus forsythiae extract. The preparation method of the fructus forsythiae extract comprises water extraction, hydroalcoholic extraction, alcohol-water extraction, ultrasonic enhanced leaching method, etc.
CN101390956a discloses a preparation method of a fructus forsythiae extract, firstly, soaking flos lonicerae at 60-85 ℃ for 0.5-2 hours to obtain a flos lonicerae warm soaking liquid, then extracting active ingredients in fructus forsythiae by a decoction method to obtain a fructus forsythiae decoction, collecting and combining the flos lonicerae warm soaking liquid and the fructus forsythiae decoction, concentrating and precipitating with alcohol to obtain the fructus forsythiae extract. However, the chlorogenic acid content and the yield of the prepared fructus forsythiae extract are to be improved. Therefore, development of the fructus forsythiae extract with high chlorogenic acid content and a preparation method thereof are urgently needed, and the quality and curative effect of the medicine and the resource utilization rate are improved.
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 chlorogenic acid content in the honeysuckle and forsythia extract is not less than 18%.
In a preferred technical scheme of the invention, the chlorogenic acid content in the fructus forsythiae extract is not less than 20%.
In the preferred technical scheme of the invention, the mass ratio of the honeysuckle to the weeping forsythia is 1:2-2:1.
The invention further provides a preparation method of the fructus forsythiae extract, which comprises the following steps of:
1) Weighing the honeysuckle and the weeping forsythiae capsule in the required amount, mixing, adding an ethanol solution with the concentration of 60-80% (V/V), wherein the adding amount of the ethanol solution is 1-15 times (volume weight ratio) of the weight of the medicinal materials, heating and reflux-extracting for 1-5 times, reflux-extracting for 0.5-5 hours each time, filtering, collecting ethanol extract, regulating the pH of filtrate to 5.5-8.5, standing, filtering, concentrating the filtrate, and preparing concentrated solution;
2) Cooling the concentrated solution obtained in the step 1), filtering, extracting the filtrate by chloroform, separating and removing chloroform extract, and drying to obtain the final product.
In the preferred technical scheme of the invention, the mass ratio of the honeysuckle to the weeping forsythia is 1:2-2:1.
In the preferred technical scheme of the invention, in the step 1), ethanol solution is added into the medicinal materials for soaking, preferably for 1-12h, and more preferably for 2-10h before heating reflux extraction.
In a preferred embodiment of the invention, the concentration of the ethanol solution is 65-75% (V/V), preferably 70% (V/V).
In the preferred technical scheme of the invention, the ethanol addition amount in the step 1) is 3-10 times (V/W), preferably 4-8 times (V/W) of the total weight of the medicinal materials.
In the preferred technical scheme of the invention, ethanol solution is added into the medicinal materials for heating reflux extraction for 2-4 times.
In the preferred technical scheme of the invention, the ethanol water solution is added into the medicinal materials, and the heating reflux extraction time is 1.0-4h, preferably 1.5-3h.
In a preferred embodiment of the invention, the pH of the filtrate in step 1) is adjusted to 6.0-8.0, preferably to 6.5-7.5.
In a preferred embodiment of the present invention, the acid-base substance that adjusts 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, α -ketoglutaric acid, and tartaric acid, or a combination thereof.
In a preferred embodiment of the present invention, the concentration of the acid-base substance solution is 0.5 to 8mol/L, preferably 0.8 to 6mol/L, and more preferably 1 to 5mol/L.
In a preferred embodiment of the invention, the filtrate from step 1) is subjected to pH adjustment and then allowed to stand for 2 to 50 hours, preferably 5 to 40 hours.
In a preferred embodiment of the invention, the filtrate from step 1) is concentrated to an alcohol-free taste.
In a preferred embodiment of the invention, the relative density of the concentrate in step 1) is 1.05-1.4 (measured at 60 ℃), preferably 1.10-1.35 (measured at 60 ℃).
In a preferred embodiment of the present invention, the concentration is selected from any one of reduced pressure concentration, film concentration, vacuum concentration, and normal pressure concentration, or a combination thereof.
In a preferred embodiment of the present invention, the chloroform is used in step 2) in an amount of 0.05 to 0.5 times (V/W), preferably 0.1 to 0.4 times (V/W), the weight of the medicinal material.
According to the preferred technical scheme, the chloroform dosage in the step 2) is any one of 0.1 times, 0.11 times, 0.12 times, 0.13 times, 0.14 times, 0.15 times, 0.16 times, 0.17 times, 0.18 times, 0.19 times, 0.2 times, 0.25 times, 0.3 times, 0.35 times, 0.4 times, 0.45 times and 0.5 times of the weight (V/W) of the medicinal materials.
According to a preferred embodiment of the invention, in step 2) the cooling is carried out to a temperature of 4-35 ℃, preferably 10-25 ℃.
According to the preferred technical scheme of the invention, after the filtrate in the step 2) is extracted by chloroform, the filtrate is kept stand for 0.5-12h, preferably 2-10h.
In a preferred embodiment of the present invention, the drying is selected from any one of reduced pressure drying, vacuum drying, spray drying, normal pressure drying, and boiling drying, or a combination thereof.
In a preferred embodiment of the present invention, the dried fructus forsythiae extract obtained in step 2) is crushed, preferably the crushing method is selected from any one of a jet crushing method, a fluid grinding method, a colloid grinding method, a jet grinding method, a co-grinding method, a ball milling method or a combination thereof.
In a preferred embodiment of the present invention, the chlorogenic acid content of the fructus forsythiae extract is not less than 18%, preferably not less than 20%.
The invention further provides a preparation method of the fructus forsythiae extract, which comprises the following steps of:
1) Weighing the honeysuckle and the weeping forsythiae capsule in the required amount, mixing, adding an acidified ethanol solution with the concentration of 60-80% (V/V), wherein the adding amount of the acidified ethanol solution is 1-15 times (V/W) of the weight of the medicinal materials, heating and reflux-extracting for 1-5 times, reflux-extracting for 0.5-5 hours each time, filtering, collecting an acidified ethanol extract, regulating the pH of the filtrate to 5.5-8.5, standing, filtering, and concentrating the filtrate to obtain a concentrated solution;
2) Cooling the concentrated solution obtained in the step 1), filtering, extracting the filtrate by chloroform, separating and removing chloroform extract, and drying to obtain the final product.
In the preferred technical scheme of the invention, the mass ratio of the honeysuckle to the weeping forsythia is 1:2-2:1.
In the preferred technical scheme of the invention, in the step 1), the medicinal materials are added with acidified ethanol solution for soaking, preferably for 1-12h, and more preferably for 2-10h before heating reflux extraction.
In a preferred embodiment of the invention, the concentration of the acidified ethanol solution is 65-75% (V/V), preferably 70% (V/V).
In the preferred technical scheme of the invention, the addition amount of the acidified ethanol in the step 1) is 3-10 times (V/W), preferably 4-8 times (V/W), of the total weight of the medicinal materials.
In a preferred embodiment of the present invention, the pH of the acidified ethanol solution is 3-6, preferably the pH of the acidified ethanol solution is 4-5.
In a preferred embodiment of the present invention, the acid used to adjust the pH of the acidified ethanol solution is selected from any one or a combination 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, alpha-ketoglutaric acid, and tartaric acid.
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 5mol/L.
In the preferred technical scheme of the invention, the acidified ethanol solution is added into the medicinal materials for heating reflux extraction for 2-4 times.
In the preferred technical scheme of the invention, the heating reflux extraction time of adding the acidified ethanol aqueous solution into the medicinal materials is 1.0-4h, preferably 1.5-3h.
In a preferred embodiment of the invention, the pH of the filtrate in step 1) is adjusted to 6.0-8.0, preferably to 6.5-7.5.
In a preferred embodiment of the present invention, the acid-base substance that adjusts 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, α -ketoglutaric acid, and tartaric acid, or a combination thereof.
In a preferred embodiment of the present invention, the concentration of the acid-base substance for adjusting the pH of the filtrate is 0.5 to 8mol/L, preferably 0.8 to 6mol/L, more preferably 1 to 5mol/L.
In a preferred embodiment of the invention, the filtrate from step 1) is subjected to pH adjustment and then allowed to stand for 2 to 50 hours, preferably 5 to 40 hours.
In a preferred embodiment of the invention, the filtrate from step 1) is concentrated to an alcohol-free taste.
In a preferred embodiment of the invention, the relative density of the concentrate in step 1) is 1.05-1.4 (measured at 60 ℃), preferably 1.10-1.35 (measured at 60 ℃).
In a preferred embodiment of the present invention, the concentration is selected from any one of reduced pressure concentration, film concentration, vacuum concentration, and normal pressure concentration, or a combination thereof.
In a preferred embodiment of the present invention, the chloroform is used in step 2) in an amount of 0.05 to 0.5 times (V/W), preferably 0.1 to 0.4 times (V/W), the weight of the medicinal material.
According to the preferred technical scheme, the chloroform dosage in the step 2) is any one of 0.1 times, 0.11 times, 0.12 times, 0.13 times, 0.14 times, 0.15 times, 0.16 times, 0.17 times, 0.18 times, 0.19 times, 0.2 times, 0.25 times, 0.3 times, 0.35 times, 0.4 times, 0.45 times and 0.5 times of the weight (V/W) of the medicinal materials.
According to a preferred embodiment of the invention, in step 2) the cooling is carried out to a temperature of 4-35 ℃, preferably 10-25 ℃.
According to the preferred technical scheme of the invention, after the filtrate in the step 2) is extracted by chloroform, the filtrate is kept stand for 0.5-12h, preferably 2-10h.
In a preferred embodiment of the present invention, the drying is selected from any one of reduced pressure drying, vacuum drying, spray drying, normal pressure drying, and boiling drying, or a combination thereof.
In a preferred embodiment of the present invention, the dry extract obtained in step 2) is pulverized, and preferably the pulverizing method is selected from any one of a jet milling method, a fluid milling method, a colloid milling method, a jet milling method, a co-milling method, a ball milling method, or a combination thereof.
In a preferred embodiment of the present invention, the chlorogenic acid content of the fructus forsythiae extract is not less than 18%, preferably not less than 20%.
It is another object of the present invention to provide a pharmaceutical composition comprising a fructus forsythiae 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 a variety of 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 embodiment of the present invention, the injection preparation includes, but is not limited to, any of injection or lyophilized powder for injection.
In a preferred embodiment of the present invention, the oral preparation is any one selected from the group consisting of oral liquid, tablets, capsules, granules, syrups, powders, lotions, effervescent agents, sprays, suspensions, pills, dripping pills, mixtures, pastes, emulsions, and teas.
In a preferred embodiment of the present invention, the external preparation is selected from any one of a gel, a paste, a patch, a cream, an ointment, a liniment, a lotion, a suppository, a smear, a cream, an ointment, and an aerosol.
In a preferred embodiment of the present invention, the pharmaceutically acceptable carrier is a common excipient or adjuvant well known in the art for preparing the desired formulation.
The common excipients or auxiliary materials of the injection, the oral preparation or the external preparation of the invention include, but are not limited to, solvents, cosolvent, isotonic regulator, pH regulator, adsorbent, complexing agent, filler (also known as diluent), lubricant (also known as glidant or anti-adhesion agent), dispersing agent, wetting agent, adhesive, disintegrating agent, regulator, solubilizer, antioxidant, bacteriostat, emulsifier, flavoring agent and the like. The solvent includes water for injection and nonaqueous solvent, and the nonaqueous solvent includes ethanol, propylene glycol, vegetable oil (soybean oil, safflower oil, sesame oil, cotton seed oil, fish oil, etc.); the cosolvent comprises organic acid and its sodium salt, amide and amine, such as malic acid, methionine, arginine, sodium benzoate, sodium salicylate, sodium p-aminobenzoate, uratein, urea, nicotinamide, glucose, meglumine, vitamin B6, etc.; isotonic regulators such as sodium chloride, glucose, mannitol, fructose, glycerol, sorbitol, xylitol, magnesium chloride, phosphate, sodium citrate and the like; pH adjusters, 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 derivatives thereof, gelatin slurry, starch slurry, polyvinylpyrrolidone and the like, the cellulose derivatives being selected from any one of microcrystalline cellulose, sodium carboxymethyl cellulose, ethyl cellulose, hydroxypropyl methylcellulose, or a combination thereof, the starch derivatives being selected from any one of sodium carboxymethyl starch, sodium starch glycolate, pregelatinized starch, modified starch, hydroxypropyl starch, corn starch, or a combination thereof; fillers such as lactose, powdered sugar, dextrin, starch or derivatives thereof, cellulose or derivatives thereof, inorganic calcium salts, sorbitol, glycine, etc., preferably the inorganic calcium salts are selected from calcium chloride, calcium sulfate, calcium phosphate, calcium hydrogen phosphate, precipitated calcium carbonate, etc., preferably the cellulose derivatives are selected from any one of microcrystalline cellulose, sodium carboxymethyl cellulose, ethylcellulose, hydroxypropyl methylcellulose, 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 silica fume, magnesium stearate, talc, colloidal silica, aluminum hydroxide, boric acid, hydrogenated vegetable oil, polyethylene glycol, etc.; disintegrants, such as starch or derivatives thereof, polyvinylpyrrolidone, crosslinked polyvinylpyrrolidone, microcrystalline cellulose, etc., preferably starch derivatives selected from any one of sodium carboxymethyl starch, sodium starch glycolate, pregelatinized starch, modified starch, hydroxypropyl starch, corn starch, or combinations thereof; humectants, 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, thioglycollic acid, sodium metabisulfite, potassium metabisulfite, dibutyl benzoic acid, vitamin E and the like; bacteriostats (bactericides) such as 0.5% phenol, 0.3% cresol, 0.5% chlorobutanol and the like; emulsifying agents, such as polysorbate-80, sorbitan without acid, pluronic F-68, lecithin, soybean lecithin, poloxamer, cholesterol, glycerol monooleate, and the like; solubilizing agents such as poloxamer, tween-80, bile, glycerol, and the like; flavoring agents, such as honey, syrup, and the like.
In the preferred technical scheme of the invention, the honeysuckle extract of the invention is mixed with a pharmaceutically acceptable slow-release preparation carrier or a controlled-release preparation carrier according to the preparation requirement, and then prepared into pellets, such as slow-release pellets or controlled-release pellets, and the like according to the preparation method of slow-release preparations or controlled-release preparations which are well known in the art, such as adding a retarder coating or microencapsulating the honeysuckle extract of the invention. The slow release preparation carrier or the controlled release preparation carrier comprises but is not limited to a greasy doping agent, a hydrocolloid, a coating retarder and the like, wherein the greasy doping agent is selected from glyceryl monostearate, hydrogenated castor oil, mineral oil, polysiloxane or dimethyl siloxane and the like; the hydrocolloid is selected from any one or combination of sodium carboxymethyl cellulose, hydroxypropyl methylcellulose, polyvinylpyrrolidone (PVP), acacia, tragacanth or carbopol; the coating retarder is selected from Ethyl Cellulose (EC), hydroxypropyl Methylcellulose (HMPC), polyvinylpyrrolidone (PVP), cellulose Acetate Phthalate (CAP), acrylic resin, etc.
In a preferred technical scheme of the invention, the dosage of the pharmaceutically acceptable carrier in the pharmaceutical composition or the type of the pharmaceutically acceptable carrier depends on factors such as physicochemical properties and content of active ingredients in the pharmaceutical composition, preparation type, dissolution of the preparation, bioavailability and the like.
In a preferred embodiment of the present invention, the pharmaceutical composition further comprises other pharmaceutically active ingredients.
Another object of the present invention is to provide an application of the honeysuckle flower and forsythia fruit extract or the pharmaceutical composition thereof in preparing a medicament, wherein the medicament has any one or combination of efficacy of relieving exterior syndrome, purging, clearing heat, cooling blood, stopping dysentery, dispelling summer heat, eliminating phlegm, tonifying, detoxicating, eliminating dampness, curing carbuncle, treating wind, resisting bacteria, resisting inflammation, resisting viruses and/or enhancing immunity.
In a preferred technical solution of the present invention, the medicine is selected from YINQIAOSAN, SHUANGHUANGLIAN oral liquid, YINQIAOPIAN, WEICHUANQIAOJIEDU tablet, QINGYINGYING decoction, XINZHONGXIAOYIN, LINGYANGGANMAO Capsule, LIANHUAQIAOWEN Capsule, YINQIAOJIEDU pill, YINQIAOSAN and its modified formula, YINYINYINQIAOTANG, YINQIAO Ma Bosan, QINGHUAJIEDU mixture, TONGZHENGGAOLIJIE decoction, YINQIAOJIEDU decoction, QINGFENGQINGQINGTANG, QINGTANG, JIUTANG, radix Platycodi semen Armeniacae amarum decoction fructus forsythiae toxin-vanquishing powder, hydrangea macrophylla pill, toxin-drawing paste, white-control live-action decoction, white tiger toxin-expelling and yin-nourishing decoction, baijiu powder, toxin-vanquishing decoction, mint decoction, medicinal liquor for treating general sores, xanthium sibiricum powder, bupleurum liver-clearing decoction, intestinal abscess decoction, pus-drawing powder, dampness-removing and toxin-removing decoction, hemorrhoid-removing pill, extract prescription, large-patch decoction, angelica and fructus forsythiae decoction, angelica beverage, trichomonas decoction, furuncle-reviving decoction, second-activity powder fructus forsythiae toxin-vanquishing powder, hydrangea macrophylla pill, toxin-drawing paste, white-guard live-action drink, white tiger toxin-vanquishing soup, baijisan, toxin-vanquishing powder, toxin-vanquishing soup, herba Menthae and fructus forsythiae formula, herba Menthae and fructus forsythiae soup, herba Menthae soup, and medicinal liquor for treating general sore Xanthium sibiricum powder, bupleurum liver-clearing decoction, acute appendicitis decoction, pus drawing powder, dampness removing and toxin removing decoction, hemorrhoid eliminating pill, extract prescription, dabu decoction, angelica sinensis and fructus forsythiae decoction, angelica sinensis decoction, trichomonas decoction, furuncle revitalizing decoction, two-stage active powder, the preparation comprises the following raw materials of detoxicating white tiger decoction, detoxicating and yin-relieving decoction, detoxicating and internal supporting powder, detoxicating and internal eliminating decoction, detoxicating and qi-flowing decoction, detoxicating and nutrient-clearing decoction, detoxifying and paste-dispersing, antipyretic and toxin-resolving decoction, golden bell decoction, golden mouse sticky decoction, jin Shengwan, jin Simo should paste, honeysuckle Ding San, golden silver spiced decoction, golden larch anti-toxin decoction, golden larch anti-burdock decoction, golden larch anti-diarrhea white powder, schizonepeta and toxin-expelling powder, nine-taste detoxicating powder, nine-taste detoxifying decoction, nine-taste qi-flowing decoction, depression-dispelling and qi-flowing and toxin-expelling decoction, anti-toxin pill, kunfu decoction, trichosanthes kirilowii Maxim decoction, appendicitis mixture, appendicitis decoction, weeping forsythiae and toxin-expelling paste, weeping forsythiae and toxin-expelling pill, weeping forsythia tail-returning decoction, weeping forsythia Huang Qishang, weeping forsythiae and toxin-dispelling pill, weeping forsythia golden bell decoction, weeping Forsythia orange leaf decoction fructus forsythiae radix rehmanniae decoction, fructus forsythiae toli powder, fructus forsythiae wild chrysanthemum powder, blood cooling wind-saving medicinal liquor, scrofula liver-soothing pill, interior-supporting disinfection powder, interior-eliminating snow decoction, qianjin interior-supporting powder, qianjin disinfection powder, throat-clearing disinfection powder, liquid for clearing away heat and toxic materials, heat-clearing and detoxifying decoction, heat-clearing and detoxifying swelling decoction, heat-clearing disinfection powder, stomach-clearing and toxin-vanquishing powder, throat-clearing and diaphragm-benefiting decoction, wind-dispelling powder, sang Qingshang, shenshengsanitary decoction, cimicifugae disinfectant decoction, liver-soothing and toxin-expelling decoction, torricea honeysuckle Ding San, torricea pus-expelling decoction, perfecting pill, xianyi grain decoction, disinfection powder, wind-eliminating toxin-vanquishing powder, lactation-eliminating pill, carbuncle-eliminating decoction, pungent and cool and toxin-relieving decoction, honeysuckle toxin-expelling decoction.
Another object of the present invention is to provide an application of the fructus forsythiae extract or the pharmaceutical composition of the present invention in preparing any one of health products, foods, cosmetics, and special medical foods, wherein any one of the health products, foods, cosmetics, and special medical foods has any one of or a combination of effects of relieving exterior syndrome, purging, clearing heat, cooling blood, relieving dysentery, dispelling summer heat, eliminating phlegm, tonifying, detoxicating, eliminating dampness, treating carbuncle, treating wind, resisting bacteria, resisting inflammation, resisting viruses, and/or enhancing immunity.
The term "75% ethanol solution" as used herein refers to an aqueous ethanol solution having a volume fraction of 75%. Other concentrations of ethanol are also referred to as volume fractions.
The method for measuring chlorogenic acid content in the Yinqiao extract refers to the new drug conversion standard of' Shuanghuanglian powder injection (freeze-drying) [ WS 3-054 (Z-011) -99 (Z) ].
Unless otherwise indicated, when the invention relates to a percentage between liquids, the 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 percentage between solids and liquids, the percentage being weight/volume percentage; the balance being weight/weight percent.
Compared with the prior art, the invention has the following beneficial effects:
1. the fructus forsythiae extract has high chlorogenic acid content, is in loose powder form or is in loose powder form after being crushed, has low water content and is not easy to absorb moisture, the hygroscopicity is obviously lower than that of similar products, the liquid obtained by dissolving and redissolving is clear and transparent, 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 method optimizes the technological parameters and conditions, and obviously improves the content and extraction rate of the chlorogenic acid; the extraction of acidified ethanol and chloroform is creatively adopted, so that the content and the extraction rate of chlorogenic acid are obviously improved, and the method is widely applied to preparing medicines, health-care products, foods, cosmetics, special medical foods and the like, and the effectiveness and the safety of the products are ensured.
3. The preparation method of the Yinqiao extract has the advantages of simple operation, high extraction yield, high resource utilization rate, better cost, environmental protection and suitability for industrialized mass production.
Detailed Description
The present invention will be specifically described below with reference to examples. The embodiments of the present invention are only for illustrating the technical solution of the present invention, and are not intended to limit the essence of the present invention.
Example 1Extraction of YinqiaoPreparation of the article
The preparation of the fructus forsythiae extract comprises the following steps:
1) Weighing 50g of honeysuckle and 100g of weeping forsythiae, crushing, sieving with a 12mm sieve, adding 70% ethanol solution (V/W) with the weight of 8 times of the weight of the medicinal materials, standing and soaking for 10h, extracting under reflux for 3h, filtering, and collecting filtrate;
2) Adding 3mol/L sodium hydroxide solution into the filtrate, regulating pH to 7.0, standing for 6h, filtering, concentrating the filtrate, recovering ethanol until no ethanol smell exists, obtaining concentrated solution, measuring relative density at 60 ℃ to 1.05, cooling the concentrated solution to 15 ℃, filtering, adding 27ml chloroform for extraction, standing for 0.5h, removing chloroform extract, drying below 90 ℃ to obtain the fructus forsythiae extract with chlorogenic acid content of 22.62%, yield of 10% and water content of 2.07%.
Example 2Preparation of Yinqiao extract
The preparation of the fructus forsythiae extract comprises the following steps:
1) Weighing 75g of honeysuckle and 150g of weeping forsythiae, crushing, sieving with a 12mm sieve, adding 65% ethanol solution (V/W) with the weight of 8 times of the weight of the medicinal materials, standing and soaking for 8.5h, extracting under reflux for 1.5h, and filtering to obtain filtrate;
2) Reflux extracting the residue with 65% ethanol solution (V/W) 6 times the weight of the medicinal materials for 1.5 hr, filtering, and collecting filtrate;
3) Mixing the two filtrates, adding 5mol/L sodium carbonate solution into the filtrate to adjust pH7.0, standing for 6h, filtering, concentrating the filtrate, recovering ethanol until no alcohol smell is present to obtain concentrated solution, measuring relative density at 60deg.C to 1.10, cooling the concentrated solution to 30deg.C, filtering, extracting with 45ml chloroform, standing for 1h, removing chloroform extract, and oven drying below 90deg.C to obtain fructus forsythiae extract with chlorogenic acid content of 21.94% with yield of 13.78% and water content of 2.08%.
Example 3Preparation of Yinqiao extract
The preparation of the fructus forsythiae extract comprises the following steps:
1) Weighing 100g of honeysuckle and 200g of weeping forsythiae capsule, adding 70% ethanol solution (V/W) with the weight of 6 times of the weight of the medicinal materials, standing and soaking for 4 hours, extracting under reflux for 1.5 hours, and filtering the filtrate;
2) Adding 70% (V/V) ethanol solution (V/W) with an amount 5 times of 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 to the filtrate, regulating pH7.0, standing for 6 hr, filtering, concentrating the filtrate, recovering ethanol until no ethanol smell is present to obtain concentrated solution, measuring relative density at 60deg.C to 1.15, cooling the concentrated solution to 10deg.C, filtering, adding 45ml chloroform for extraction, standing for 3 hr, removing chloroform extract, and oven drying below 90deg.C to obtain fructus forsythiae extract with chlorogenic acid content of 26.59%, yield of 15.33% and water content of 2.68%.
Example 4Preparation of Yinqiao extract
The preparation of the fructus forsythiae extract comprises the following steps:
1) Weighing 50g of honeysuckle and 100g of weeping forsythiae capsule, crushing, sieving with a 12mm sieve, adding 70% acidified ethanol solution (0.5 mol/L hydrochloric acid for regulating pH to 6) (V/W) with the weight of 6 times of the weight of the medicinal materials, standing and soaking for 5h, extracting under reflux for 1.5h, and filtering to obtain filtrate;
2) Adding 70% acidified ethanol solution (0.5 mol/L hydrochloric acid to adjust pH to 6) (V/W) into the residue for reflux extraction for 2 hr, filtering, and collecting filtrate;
3) Mixing the two filtrates, adding 5mol/L sodium hydroxide solution into the filtrate to adjust pH7.0, standing for 8 hr, filtering, concentrating the filtrate, recovering ethanol until no ethanol smell exists to obtain concentrated solution, and measuring relative density at 60deg.C to 1.20; cooling the concentrated solution to 4deg.C, filtering, adding 25ml chloroform into the filtrate, extracting, standing for 5 hr, removing chloroform extract, oven drying below 90deg.C to obtain fructus forsythiae extract with chlorogenic acid content of 20.88%, pulverizing to obtain brown powder with yield of 21.67% and water content of 3.02%.
Example 5Preparation of Yinqiao extract
The preparation of the fructus forsythiae extract comprises the following steps:
1) Weighing 50g of honeysuckle and 100g of weeping forsythiae, crushing, sieving with a 12mm sieve, adding 70% acidified ethanol solution (1 mol/L hydrochloric acid for regulating pH 4) (V/W) with the weight of 8 times of the weight of the medicinal materials, standing and soaking for 2h, extracting under reflux for 3h, and filtering to obtain filtrate;
2) Adding 70% acidified ethanol solution (1 mol/L hydrochloric acid to adjust pH 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 filtrate;
3) Mixing the two filtrates, adding 5mol/L sodium carbonate solution into the filtrate to adjust pH7.0, standing for 6h, filtering, concentrating the filtrate, recovering ethanol until no alcohol smell exists to obtain concentrated solution, and measuring relative density at 60deg.C to 1.25; cooling the concentrated solution to 20deg.C, filtering, adding 35ml chloroform into the filtrate, extracting, standing for 7 hr, removing chloroform extract, and oven drying below 90deg.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 Yinqiao extract
The preparation of the fructus forsythiae extract comprises the following steps:
1) Weighing 100g of honeysuckle and 100g of weeping forsythiae capsule, crushing, sieving with a 12mm sieve, adding 75% acidified ethanol solution (2 mol/L acetic acid for regulating pH 5) (V/W) with the weight of 8 times of the weight of the medicinal materials, standing and soaking for 2h, extracting under reflux for 1.5h, and filtering to obtain filtrate;
2) Adding an acidified ethanol solution (2 mol/L acetic acid for regulating pH 5) (V/W) with the weight of 75% of that of the medicine material into the filter residue, reflux-extracting for 1.5h, and filtering to collect filtrate;
3) Mixing the two filtrates, adding 5mol/L triethylamine into the filtrate to adjust pH7.5, standing for 12 hr, filtering, concentrating the filtrate, recovering ethanol until no alcohol smell exists to obtain concentrated solution, and measuring relative density at 60deg.C to 1.30; cooling the concentrated solution to 20deg.C, adding 43ml chloroform into the filtrate, extracting, standing for 10 hr, removing chloroform extract, and oven drying below 90deg.C to obtain fructus forsythiae extract with chlorogenic acid content of 23.71%, yield of 25.49%, and water content of 2.69%.
Example 7Preparation of Yinqiao extract
The preparation of the fructus forsythiae extract comprises the following steps:
1) Weighing 100g of honeysuckle and 100g of weeping forsythiae capsule, crushing, sieving with a 12mm sieve, adding 70% acidified ethanol aqueous solution (5 mol/L acetic acid for regulating pH 3) (V/W) with the weight of 7 times of the weight of the medicinal materials, standing and soaking for 8h, extracting under reflux for 2h, and filtering to obtain filtrate;
2) Adding 70% of acidified ethanol solution (pH 3 is regulated by 5mol/L acetic acid) with the weight of 6 times of 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 pH7.0, standing for 12h, filtering, concentrating the filtrate, recovering ethanol until no alcohol smell exists to obtain concentrated solution, and measuring relative density at 60deg.C to 1.35; cooling the concentrated solution to 15deg.C, extracting with 70ml chloroform, standing for 12 hr, removing chloroform extractive solution, and oven drying below 90deg.C to obtain fructus forsythiae extract with chlorogenic acid content of 22.32%, yield of 24.52% and water content of 3.30%.
The dried extracts of the fructus forsythiae prepared in the examples 1-7 are crushed into brown powder, the brown powder is placed in the natural environment without moisture absorption, the solution is clear after water is added for re-dissolution, insoluble matters or floccules are avoided, and the light transmittance is high.
Comparative example 1Preparation of Yinqiao extract
The preparation of the fructus forsythiae extract comprises the following steps:
1) Soaking 50g of honeysuckle and 100g of weeping forsythiae in water for 30 minutes, decocting twice, each time for 1.5 hours, combining the decoctions, filtering, and concentrating the filtrate into clear paste with the relative density of 1.20-1.25 (70-80 ℃);
2) Slowly adding ethanol when the clear paste obtained in the step 1) is cooled to 40 ℃, fully stirring, standing for 12 hours, filtering to obtain supernatant, adding a proper amount of 75% ethanol into residues, stirring, standing for 12 hours, filtering, combining ethanol solutions, recovering ethanol until no ethanol smell exists, drying, and measuring chlorogenic acid content to be 8.49%, wherein the yield is 10.08%. The obtained fructus forsythiae extract is pulverized into dark brown powder, and the solution contains black insoluble substances and small amount of floccules after redissolution.
The above description of the embodiments of the present invention is not intended to limit the present invention, and those skilled in the art can make various changes or modifications according to the present invention without departing from the spirit of the present invention, and shall fall within the scope of the claims of the present invention.

Claims (18)

1. The preparation method of the fructus forsythiae extract is characterized in that the effective components of the extract are honeysuckle and fructus forsythiae, wherein the mass ratio of the honeysuckle to the fructus forsythiae is 1:2-2:1, and the chlorogenic acid content in the extract is not less than 20 percent, and the preparation method of the fructus forsythiae extract comprises the following steps:
1) Weighing the required amount of honeysuckle and weeping forsythiae capsule, mixing, adding an ethanol solution with the concentration of 60-80% V/V, wherein the addition amount of the ethanol solution is 4-8 times of the weight of the medicinal materials, soaking for 2-10h, heating and reflux-extracting for 1-5 times, reflux-extracting for 1.5-3 hours each time, filtering, collecting ethanol extract, regulating the pH of filtrate to 5.5-8.5, standing for 5-40h, filtering, concentrating the filtrate until no alcohol smell exists, and preparing a concentrated solution with the relative density of 1.05-1.4, wherein the relative density is measured at 60 ℃, and the concentration is any one or combination of reduced pressure concentration, film concentration and vacuum concentration;
2) Cooling the concentrated solution obtained in the step 1) to 4-35 ℃, filtering, adding chloroform with the weight of 0.05-0.5 times of the weight of the medicinal materials into the filtrate, extracting, standing for 0.5-12h, separating and removing chloroform extract, and drying to obtain the final product, wherein the drying is selected from any one or combination of reduced pressure drying, vacuum drying, spray drying and boiling drying.
2. The method of claim 1, wherein the concentration of the ethanol solution is 65-75%.
3. The preparation method according to claim 1, wherein the ethanol solution is added to the medicinal material and the mixture is subjected to reflux extraction for 2 to 4 times.
4. The process according to claim 1, wherein the pH of the filtrate in step 1) is adjusted to 6.5-7.5.
5. The method according to claim 4, wherein the acid-base substance for adjusting the pH of the filtrate is selected from the group consisting of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, triethylamine, meglumine, hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, sulfonic acid, malic acid, fumaric acid, citric acid, oxalic 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, and fumaric acid.
6. The method according to claim 5, wherein the concentration of the acid-base substance solution is 0.5 to 8mol/L.
7. The method according to claim 1, wherein the chloroform is used in the amount of 0.1, 0.11, 0.12, 0.13, 0.14, 0.15, 0.16, 0.17, 0.18, 0.19, 0.2, 0.25, 0.3, 0.35, 0.4, 0.45, or 0.5 times the weight of the medicinal material in step 2).
8. The method of claim 1, wherein the cooling in step 2) is to 10-25 ℃.
9. The preparation method according to claim 1, wherein the dried fructus forsythiae extract obtained in the step 2) is pulverized, and the pulverizing method is selected from any one of a jet milling method, a fluid milling method, a colloid milling method, a jet milling method, a co-milling method, a ball milling method, or a combination thereof.
10. The preparation method of the fructus forsythiae extract is characterized in that the effective components of the extract are honeysuckle and fructus forsythiae, wherein the mass ratio of the honeysuckle to the fructus forsythiae is 1:2-2:1, and the chlorogenic acid content in the extract is not less than 20 percent, and the preparation method of the fructus forsythiae extract comprises the following steps:
1) Weighing the required amount of honeysuckle and weeping forsythiae capsule, mixing, adding an acidified ethanol solution with the concentration of 60-80% V/V, wherein the adding amount of the acidified ethanol solution is 4-8 times of the weight of the medicinal material, soaking for 2-10h, heating and reflux-extracting for 2-4 times, reflux-extracting for 1.5-3h each time, filtering, collecting an acidified ethanol extract, regulating the pH of the filtrate to 5.5-8.5, standing for 5-40h, filtering, concentrating the filtrate until no alcohol smell exists, and preparing a concentrated solution with the relative density of 1.1-1.35, wherein the pH of the acidified ethanol solution is 3-6, the relative density is measured at 60 ℃, and the concentration is any one or combination of reduced pressure concentration, film concentration and vacuum concentration;
2) Cooling the concentrated solution obtained in the step 1) to 4-35 ℃, filtering, adding chloroform with the weight of 0.05-0.5 times of the weight of the medicinal materials into the filtrate, extracting, standing for 0.5-12h, separating and removing chloroform extract, and drying to obtain the final product, wherein the drying is selected from any one or combination of reduced pressure drying, vacuum drying, spray drying and boiling drying.
11. The method of claim 10, wherein the acidified ethanol solution has a concentration of 65 to 75%.
12. The method according to claim 10, wherein the acid used for adjusting the pH of the acidified ethanol solution is selected from any one of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, sulfonic acid, malic acid, fumaric acid, citric acid, oxalic 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, or a combination thereof.
13. The process according to claim 12, wherein the acid concentration used for adjusting the pH of the acidified aqueous ethanol solution is 1 to 5mol/L.
14. The process according to claim 10, wherein the pH of the filtrate in step 1) is adjusted to 6.5-7.5.
15. The method according to claim 14, wherein 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, nitric acid, phosphoric acid, sulfonic acid, malic acid, fumaric acid, citric acid, oxalic 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, or a combination thereof.
16. The method according to claim 15, wherein the concentration of the acid-base substance for adjusting the pH of the filtrate is 1 to 5mol/L.
17. The method according to claim 10, wherein the chloroform is used in the amount of 0.1, 0.11, 0.12, 0.13, 0.14, 0.15, 0.16, 0.17, 0.18, 0.19, 0.2, 0.25, 0.3, 0.35, 0.4, 0.45, or 0.5 times the weight of the medicinal material in step 2).
18. The method according to claim 10, wherein the dry extract obtained in step 2) is pulverized by any one or a combination of jet milling, fluid milling, colloid milling, jet milling, co-milling and ball milling.
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