CN114601857B - Honeysuckle extract with high chlorogenic acid content as well as preparation method and application thereof - Google Patents

Honeysuckle extract with high chlorogenic acid content as well as preparation method and application thereof Download PDF

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CN114601857B
CN114601857B CN202011412785.5A CN202011412785A CN114601857B CN 114601857 B CN114601857 B CN 114601857B CN 202011412785 A CN202011412785 A CN 202011412785A CN 114601857 B CN114601857 B CN 114601857B
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acid
filtrate
preparation
extract
concentration
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CN114601857A (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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    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/35—Caprifoliaceae (Honeysuckle family)
    • A61K36/355—Lonicera (honeysuckle)
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Abstract

The invention relates to a honeysuckle extract with high chlorogenic acid content, a preparation method and application thereof. The invention particularly relates to a honeysuckle extract with high chlorogenic acid content, wherein the chlorogenic acid content in the honeysuckle extract is not lower than 26%. In addition, the invention provides an alcohol extraction process of the honeysuckle extract with high chlorogenic acid content and preparation conditions thereof, and the honeysuckle extract is further extracted by adopting acidified ethanol solution and is used for preparing the pharmaceutical composition containing the honeysuckle extract, so that the chlorogenic acid content and extraction rate in the extract are obviously improved, the product quality is controllable, the effectiveness and safety of the medicine are further obviously improved, the resource utilization rate is obviously improved, the cost is obviously reduced, and the alcohol extraction process is suitable for industrial production.

Description

Honeysuckle extract with high chlorogenic acid content as well as preparation method and application thereof
Technical Field
The invention relates to the field of traditional Chinese medicines, and in particular relates to a honeysuckle extract with high chlorogenic acid content, 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 it is also called Yinhua, shuanghua, erhua, erbaohua and Shuangbaohua.
The honeysuckle has the effects of clearing away heat and toxic materials, relieving exterior syndrome with pungent and cool natured drugs and the like, effectively inhibits the growth of various bacteria and viruses, has good effects of resisting inflammation and allergic reaction, improving the immunity of the organism and the like, and is one of effective components of a plurality of Chinese patent medicine compositions (such as Shuanghuanglian, yinqiao powder and the like). Chlorogenic acid is a main drug effect component of honeysuckle and the extract thereof, and becomes a key index for testing the quality of the honeysuckle and the extract thereof.
Document 1 (lindane, etc., comparative research on chlorogenic acid of different extraction methods of honeysuckle, 2003, 15 (2), 124-126) relatively researches preparation methods (including water extraction method, water extraction and alcohol precipitation method, enzymolysis method, alcohol extraction method, etc.) of honeysuckle extract and technical effects thereof, and the prepared honeysuckle extract has chlorogenic acid content not higher than 15.28%, and has the defects of dark color, strong hygroscopicity, easy hardening, low clarity after redissolution, and the like. Therefore, the preparation method of the honeysuckle extract needs to be optimized, and the quality, the curative effect and the resource utilization rate of the medicine are improved.
Disclosure of Invention
The invention aims to provide a honeysuckle extract with high chlorogenic acid content, wherein the chlorogenic acid content in the honeysuckle extract is not lower than 26%.
In a preferred technical scheme of the invention, the chlorogenic acid content in the honeysuckle extract is not lower than 28%, preferably not lower than 30%.
Another objective of the present invention is to provide a method for preparing a honeysuckle extract with high chlorogenic acid content, comprising the following steps:
1) Weighing required amount of flos Lonicerae, adding 60-80% (V/V) ethanol solution with the addition amount of 1-15 times (V/W) of the weight of the medicinal materials, heating and reflux-extracting for 1-5 times, each time reflux-extracting for 0.5-5 hr, filtering, collecting ethanol extract, adjusting pH of filtrate to 5.5-8.5, standing, filtering, 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 a preferred technical scheme of the invention, before heating reflux extraction in step 1), the honeysuckle is soaked after being added with an ethanol solution, preferably for 1-12h, and more preferably for 2-10h.
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 solution 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 heating reflux extraction is carried out for 2-4 times.
In the preferred technical scheme of the invention, the heating reflux extraction time is 1.0-4 hours, preferably 1.5-3 hours.
In a preferable technical scheme of the invention, the pH of the filtrate obtained in the step 1) is adjusted to be 6.0-8.0, and the pH is preferably 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, hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, sulfonic acid, malic acid, fumaric acid, citric 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 the preferable technical scheme of the invention, the concentration of the acid-base substance solution for adjusting the pH of the filtrate is 0.5-8mol/L, preferably 0.8-6mol/L, and more preferably 1-5mol/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 value 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 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 or 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 2-10h.
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 boiling drying.
In a preferred technical scheme of the invention, the dry extract prepared in the step 2) is pulverized, and a preferred pulverizing method is any one or a 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 the preferred technical scheme of the invention, the chlorogenic acid content of the prepared honeysuckle extract is not lower than 26%, preferably not lower than 28%.
Another objective of the present invention is to provide a preparation method of a honeysuckle extract with high chlorogenic acid content, comprising the following steps:
1) Weighing flos Lonicerae with required amount, adding acidified ethanol solution with concentration of 60% -80% (V/V), the adding amount of acidified ethanol solution is 1-15 times (V/W) of the weight of the medicinal materials, heating and reflux extracting for 1-5 times, each reflux extracting for 0.5-5 hr, filtering, collecting acidified ethanol extractive solution, adjusting pH of the filtrate to 5.5-8.5, standing, filtering, 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 preferable technical scheme of the invention, before heating reflux extraction in step 1), the honeysuckle is soaked after being added with the acidified ethanol solution, preferably for 1-12h, and more preferably for 2-10h.
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 solution 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 embodiment of the invention, the pH of the acidified ethanol solution is 3 to 6, preferably 4 to 5.
In a preferred embodiment of the present invention, the acidic substance 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 concentration of the acidic substance solution for adjusting the pH of the acidified aqueous ethanol solution is 0.5 to 8mol/L, preferably 0.8 to 6mol/L, and more preferably 1 to 5mol/L.
In the preferred technical scheme of the invention, the heating reflux extraction is carried out for 2-4 times.
In the preferred technical scheme of the invention, the heating reflux extraction time is 1.0-4 hours, preferably 1.5-3 hours.
In a preferred technical scheme of the invention, the pH of the filtrate obtained in the step 1) is adjusted to 6.0-8.0, and preferably 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, hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, sulfonic acid, malic acid, fumaric acid, citric 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 the preferable technical scheme of the invention, the concentration of the acid and alkali substance solution for adjusting the pH of the filtrate is 0.5-8mol/L, preferably 0.8-6mol/L, and more preferably 1-5mol/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 preferable 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.
In the preferable technical scheme of the invention, the dosage of the chloroform in the step 2) is 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 or 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 2-10h.
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 dry extract prepared in the step 2) is pulverized, and a preferred pulverizing method is any one or a 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 the preferred technical scheme of the invention, the chlorogenic acid content of the prepared honeysuckle extract is not less than 28%, preferably not less than 30%.
Another object of the present invention is to provide a pharmaceutical composition, which comprises the honeysuckle extract of the present invention and a pharmaceutically acceptable carrier.
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 is selected from any one of injection and freeze-dried powder for injection.
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 selected from any one of gels, ointments, emplastrums, creams, ointments, liniments, lotions, suppositories, smearing agents, ointment 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, and 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, 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, for example, sodium chloride, glucose, mannitol, fructose, glycerol, sorbitol, xylitol, magnesium chloride, phosphates, sodium citrate, etc.; pH regulators such as 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, and potassium hydrogen carbonate; 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, etc.; 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 honeysuckle extract is mixed with a pharmaceutically acceptable sustained-release preparation carrier or controlled-release preparation carrier according to the preparation requirements, and then the mixture is prepared into pellets, such as sustained-release pellets or controlled-release pellets and the like, according to the preparation method of the sustained-release preparation or controlled-release preparation known in the art, such as adding a retardant coating or microencapsulating the honeysuckle 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 according to physicochemical properties and content of the active ingredient in the pharmaceutical composition, the type of the preparation, 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 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.
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The invention also aims to provide application of the honeysuckle extract or the pharmaceutical composition thereof in 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.
The 75% ethanol solution refers to 75% ethanol water solution by volume fraction. Other concentrations of ethanol are also referred to as volume fractions.
Unless otherwise stated, the present invention detects the content of chlorogenic acid in honeysuckle by High Performance Liquid Chromatography (HPLC) disclosed in document 2 (huangyun et al, comparative study of honeysuckle extract components of different processes, 2005, vol 11, no. 6). The detection conditions mainly include:
the instrument comprises the following steps: waters hplc, detector: a Waters 2996 diode array detector, a chromatographic column, a Symm entry ODS column (4.6X 150mm,5 μm), an ODS protection column, a mobile phase, acetonitrile-0.4% phosphoric acid (8 92), a detection wavelength of 327nm, a flow rate of 1.0ml/min, a column temperature of 40 ℃, and a theoretical plate number of not less than 3000 according to chlorogenic acid peak calculation.
Unless otherwise indicated, when the present invention relates to percentages between liquids, said percentages are volume/volume percentages; when the invention relates to percentages between liquid and solid, said percentages are volume/weight percentages; the present invention relates to percentages between solids and liquids, 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 chlorogenic acid in the honeysuckle extract is not less than 26% and has excellent quality, the obtained honeysuckle extract is loose golden yellow powder or loose golden yellow powder formed by crushing dry paste, the water content is low, moisture absorption is difficult, the hygroscopicity is obviously lower than that of similar products, the dissolution is easy, the obtained liquid is clear and transparent, the quality and the curative effect of the honeysuckle extract and products thereof are obviously improved, the resource utilization rate is obviously improved, and the preparation and application of the honeysuckle extract are expanded.
2. The preparation process of the honeysuckle extract optimized by the invention has the advantages of simple operation, high yield, more excellent cost, environmental protection, suitability for industrial production and the like.
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 spirit of the present invention.
Example 1 preparation of honeysuckle extract
The preparation method of the honeysuckle extract comprises the following steps:
1) Weighing 1Kg of honeysuckle, crushing the honeysuckle into coarse powder, sieving the coarse powder by a 12mm sieve, adding 65% ethanol solution (V/W) which is 6 times of the weight of the medicinal materials, standing and soaking for 8 hours, performing reflux extraction for 1.5 hours, filtering, and collecting filtrate;
2) Adding 65% ethanol solution (V/W) 5 times the weight of the medicinal materials into the residue, reflux extracting for 1.5 hr, filtering, and collecting filtrate;
3) Mixing the two filtrates, adding 3 mol/sodium hydroxide solution into the filtrate to adjust pH to 7.0, standing for 5h, filtering, concentrating the filtrate to recover ethanol until no ethanol smell exists, to obtain concentrated solution, measuring relative density at 60 deg.C to 1.10, cooling the concentrated solution to 20 deg.C, filtering, adding 200ml chloroform into the filtrate, extracting, standing for 1h, removing chloroform extract, and spray drying at 80 deg.C or below to obtain flos Lonicerae extract with chlorogenic acid content of 29.83%, yield of 22%, and water content of 4.24%.
Example 2 preparation of honeysuckle extract
The preparation method of the honeysuckle extract comprises the following steps:
1) 1Kg of honeysuckle is crushed, sieved by a 12mm sieve, added with 70 percent ethanol solution (V/W) which is 8 times of the weight of the medicinal materials, kept stand and soaked for 10 hours, extracted for 2 hours by reflux, and filtered to obtain filtrate;
2) Adding 70% 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 7.5, standing for 12h, filtering, concentrating the filtrate, recovering ethanol until no ethanol smell exists to obtain concentrated solution, measuring relative density at 60 deg.C to 1.15, cooling the concentrated solution to 15 deg.C, filtering, adding 400ml chloroform into the filtrate, extracting, standing for 2h, removing chloroform extract, and oven drying at 80 deg.C or below to obtain flos Lonicerae extract with chlorogenic acid content of 29.83%, yield of 27% and water content of 5.28%.
Example 3 preparation of honeysuckle extract
The preparation method of the honeysuckle extract comprises the following steps:
1) 1Kg of honeysuckle is crushed, sieved by a 12mm sieve, added with 75 percent ethanol solution (V/W) which is 7 times of the weight of the medicinal materials, kept stand and soaked for 5 hours, extracted for 2 hours by reflux, and filtered to obtain filtrate;
2) Adding 75% ethanol solution (V/W) 4 times 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 triethylamine, adjusting pH to 7.0, standing for 8h, filtering, concentrating the filtrate, recovering ethanol until no alcohol smell exists to obtain concentrated solution, measuring relative density at 60 deg.C to 1.20, cooling the concentrated solution to 10 deg.C, filtering, adding 350ml chloroform into the filtrate, extracting, standing for 0.5h, removing chloroform extract, and oven drying at 80 deg.C or below to obtain flos Lonicerae extract with chlorogenic acid content of 30.42%, yield of 20.77% and water content of 2.0%.
Example 4 preparation of honeysuckle extract
The preparation method of the honeysuckle extract comprises the following steps:
1) 1Kg of honeysuckle is crushed, sieved by a 12mm sieve, added with 70 percent ethanol solution (V/W) which is 6 times of the weight of the medicinal materials, kept stand and soaked for 2 hours, extracted for 3 hours by reflux, and filtered to obtain filtrate;
2) Adding 70% ethanol solution (V/W) 5 times the weight of the medicinal materials into the filter residue, reflux-extracting for 2h, filtering, and collecting the filtrate;
3) Mixing the two filtrates, adding 0.5mol/L meglumine into the filtrate, adjusting pH to 6.5, standing for 12h, filtering, concentrating the filtrate, recovering ethanol until no ethanol smell is obtained, measuring relative density at 60 deg.C to 1.25, cooling the concentrated solution to 15 deg.C, filtering, adding 200ml chloroform into the filtrate, extracting, standing for 12h, removing chloroform extract, and oven drying at 80 deg.C or below to obtain flos Lonicerae extract with chlorogenic acid content of 29.43%, yield of 26.16% and water content of 2.7%.
Example 5 preparation of honeysuckle extract
The preparation method of the honeysuckle extract comprises the following steps:
1) 1Kg of honeysuckle is crushed, sieved by a 12mm sieve, added with 70 percent ethanol solution (V/W) which is 8 times of the weight of the medicinal materials, kept stand and soaked for 2 hours, extracted for 2 hours by reflux, and filtered to obtain filtrate;
2) Adding 70% (V/W) ethanol 6 times 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 3 mol/sodium hydroxide solution into the filtrate to adjust pH to 7.0, standing for 8h, filtering, concentrating the filtrate to recover ethanol until no ethanol smell is obtained to obtain concentrated solution, measuring relative density at 60 deg.C to 1.30, cooling the concentrated solution to 30 deg.C, filtering, adding 400ml chloroform into the filtrate to extract, standing for 8h, removing chloroform extract, and spray drying at 80 deg.C or below to obtain flos Lonicerae extract with chlorogenic acid content of 26.62%, yield of 27.33%, and water content of 3.86%.
Example 6 preparation of honeysuckle extract
The preparation method of the honeysuckle extract comprises the following steps:
1) 1Kg of honeysuckle is crushed, sieved by a 12mm sieve, added with 70 percent ethanol solution (V/W) which is 5 times of the weight of the medicinal materials, kept stand and soaked for 2 hours, extracted for 2 hours by reflux and filtered to obtain filtrate;
2) Adding 70% ethanol solution (V/W) 5 times 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 3 mol/sodium hydroxide solution into the filtrate to adjust pH to 7.0, standing for 4h, filtering, concentrating the filtrate to recover ethanol until no alcohol smell exists to obtain concentrated solution, measuring relative density at 60 deg.C to 1.35, cooling the concentrated solution to 30 deg.C, filtering, adding 150ml chloroform into the filtrate to extract, standing for 4h, removing chloroform extract, spray drying at 80 deg.C below to obtain golden yellow loose powder of flos Lonicerae extract with chlorogenic acid content of 29.56%, yield of 21.33%, and water content of 3.29%.
Example 7Preparation of flos Lonicerae extract
The preparation method of the honeysuckle extract comprises the following steps:
1) 1Kg of honeysuckle is crushed, sieved by a 12mm sieve, added with 70 percent ethanol solution (V/W) which is 8 times of the weight of the medicinal materials, kept stand and soaked for 8 hours, extracted for 2 hours by reflux, and filtered to obtain filtrate;
2) Adding 70% ethanol solution (V/W) 4 times 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, adjusting pH to 7.0, standing for 12h, filtering, concentrating the filtrate, recovering ethanol until no ethanol smell is obtained to obtain concentrated solution, measuring relative density at 60 deg.C to 1.40, cooling the concentrated solution to 4 deg.C, filtering, adding 100ml chloroform into the filtrate, extracting, standing for 2h, and spray drying the concentrated solution at a temperature below 80 deg.C to obtain flos Lonicerae extract with chlorogenic acid content of 31.91%, yield of 24%, and water content of 1.63%.
Example 8Preparation of flos Lonicerae extract
The preparation method of the honeysuckle extract comprises the following steps:
1) 1Kg of honeysuckle is crushed, sieved by a 12mm sieve, added with 70 percent ethanol solution (V/W) which is 7 times of the weight of the medicinal materials, kept stand and soaked for 4 hours, extracted for 3 hours by reflux, and filtered to obtain filtrate;
2) Adding 70% ethanol solution (V/W) 5 times 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, adjusting pH to 7.0, standing for 12h, filtering, concentrating the filtrate, recovering ethanol until no ethanol smell is obtained, measuring relative density at 60 deg.C to obtain 1.05 concentrated solution, cooling to 20 deg.C, filtering, adding 280ml chloroform into the filtrate, extracting, standing for 4h, and oven drying the concentrated solution at a temperature below 80 deg.C to obtain flos Lonicerae extract with chlorogenic acid content of 28.14%, yield of 23%, and water content of 2.62%.
Example 9Preparation of honeysuckle extract
The preparation method of the honeysuckle extract comprises the following steps:
1) 1Kg of honeysuckle is crushed, sieved by a 12mm sieve, added with 70 percent acidified ethanol solution (pH is adjusted to 5 by 2mol/L acetic acid) (V/W) which is 7 times of the weight of the medicinal materials, kept stand and soaked for 4 hours, extracted for 3 hours by reflux, and filtered to obtain filtrate;
3) Adding 70% acidified ethanol solution (pH 5 adjusted by 2mol/L acetic acid) (V/W) 5 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, adjusting pH to 7.0, standing for 20h, filtering, concentrating the filtrate, recovering ethanol until no ethanol smell is obtained to obtain concentrated solution, measuring relative density at 60 deg.C to 1.20, cooling the concentrated solution to 15 deg.C, filtering, adding 500ml chloroform into the filtrate, extracting, standing for 8h, and oven drying the concentrated solution at a temperature below 80 deg.C to obtain flos Lonicerae extract with chlorogenic acid content of 29.71%, yield of 32%, and water content of 2.81%.
The dried paste of the honeysuckle extract prepared in the embodiments 1 to 9 is golden yellow loose powder after being crushed, has no moisture absorption and hardening phenomena after being placed in a natural environment, is clarified after being redissolved by water to obtain golden yellow clarified liquid, has no insoluble substance or floccule, and has high light transmittance.
Comparative example 1Preparation of honeysuckle extract
The preparation method of the honeysuckle extract comprises the following steps:
1) Pulverizing 100g of flos Lonicerae, sieving with 12mm sieve, adding 10 times of 70% (V/V) ethanol solution, soaking for 24h, and extracting under reflux at 60 deg.C for 3 times, each for 1h;
2) Mixing extractive solutions, concentrating under reduced pressure at 60 deg.C, and vacuum drying to obtain dry extract; the yield is 28.71 percent, and the content of chlorogenic acid is 11.47 percent.
The dried paste is crushed into brown yellow powder, black undissolved substances and a small amount of floccules exist in the solution after redissolution, and the powder is hardened after being placed at room temperature for one week.
The above description of the 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 without departing from the spirit of the present invention, which should fall within the scope of the appended claims.

Claims (19)

1. A preparation method of a honeysuckle extract with high chlorogenic acid content comprises the following steps:
1) Weighing the required amount of honeysuckle, adding 60-80% (V/V) ethanol solution, wherein the adding amount of the ethanol solution is 4-8 times (V/W) of the weight of the medicinal materials, soaking for 2-10h, heating and refluxing for 2-4 times, refluxing and extracting for 1.5-3 h each time, filtering, collecting ethanol extract, adjusting the pH of filtrate to 5.5-8.5, standing for 2-50h, filtering, concentrating the filtrate until no alcohol smell exists, and preparing concentrated solution with the relative density of 1.05-1.4, wherein the relative density is measured at 60 ℃, and the concentration is selected from any one or combination of reduced pressure concentration, film concentration and vacuum concentration;
2) Cooling the concentrated solution prepared in the step 1) to 4-35 ℃, filtering, adding chloroform with the weight of 0.05-0.5 time (V/W) of the medicinal material into the filtrate for extraction, standing for 0.5-12h, separating and removing the chloroform extract, and drying to obtain the product, wherein the drying is any one or the combination of reduced pressure drying, vacuum drying, spray drying and boiling drying.
2. The method according to claim 1, wherein the concentration of the ethanol solution is 65-75% (V/V).
3. The method according to claim 1, wherein the pH of the filtrate obtained in step 1) is adjusted to 6.5 to 7.5.
4. The preparation method according to claim 3, wherein the acid-base substance for adjusting pH of the filtrate is selected from any one of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, triethylamine, 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.
5. The method according to claim 4, wherein the concentration of the solution of the acid-base substance for adjusting the pH of the filtrate is 0.5 to 8mol/L.
6. The method according to claim 1, wherein the amount of chloroform used in step 2) is 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 (V/W) of the medicinal material.
7. The preparation method according to claim 1, wherein the dry extract obtained in step 2) is pulverized by any one or combination of jet milling, fluid milling, colloid milling, jet milling, co-milling and ball milling.
8. The preparation method of claim 1, wherein the chlorogenic acid content in the prepared honeysuckle extract is more than or equal to 26%.
9. The preparation method of claim 8, wherein the chlorogenic acid content in the prepared honeysuckle extract is more than or equal to 28%.
10. A preparation method of a honeysuckle extract with high chlorogenic acid content comprises the following steps:
1) Weighing required amount of honeysuckle, adding acidified ethanol solution with concentration of 60-80% (V/V), wherein the added amount of the acidified ethanol solution is 4-8 times (V/W) of the weight of the medicinal materials, soaking for 2-10h, heating and refluxing for 2-4 times, refluxing and extracting for 1.5-3 h each time, filtering, collecting acidified ethanol extract, adjusting pH of the filtrate to 5.5-8.5, standing for 5-40h, filtering, concentrating the filtrate until no alcohol smell exists, and preparing concentrated solution with relative density of 1.10-1.35, wherein the acidified ethanol solution has pH of 4-5, the relative density is measured at 60 ℃, and the concentration is selected from any one or combination of reduced pressure concentration, film concentration and vacuum concentration;
2) Cooling the concentrated solution prepared in the step 1) to 10-25 ℃, filtering, adding chloroform with the weight of 0.05-0.5 time (V/W) of the weight of the medicinal materials into the filtrate for extraction, standing for 2-10h, separating and removing the chloroform extract, and drying, wherein the drying is any one or the 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 65-75% (V/V).
12. The preparation method according to claim 10, wherein the acidic substance for adjusting the pH of the acidified ethanol solution is selected from any one of hydrochloric acid, sulfuric acid, nitric acid, hydrobromic acid, hydrofluoric 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 method according to claim 12, wherein the concentration of the acidic substance solution for adjusting the pH of the acidified aqueous ethanol solution is 1 to 5mol/L.
14. The method according to claim 10, wherein the pH of the filtrate obtained in step 1) is adjusted to 6.5 to 7.5.
15. The preparation 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, 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 preparation method according to claim 15, wherein the concentration of the acid-base substance solution for adjusting the pH of the filtrate is 1 to 5mol/L.
17. The method according to claim 10, wherein the amount of chloroform used in step 2) is 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 (V/W) of the medicinal material.
18. The preparation method according to claim 10, wherein the dry extract obtained in step 2) is pulverized by any one or combination of jet milling, fluid milling, colloid milling, jet milling, co-milling and ball milling.
19. The preparation method of claim 10, wherein the chlorogenic acid content of the prepared honeysuckle extract is not less than 28%.
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