CN103860622B - A kind of method of extracting saponins compound from honeysuckle - Google Patents
A kind of method of extracting saponins compound from honeysuckle Download PDFInfo
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- CN103860622B CN103860622B CN201210556010.4A CN201210556010A CN103860622B CN 103860622 B CN103860622 B CN 103860622B CN 201210556010 A CN201210556010 A CN 201210556010A CN 103860622 B CN103860622 B CN 103860622B
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Abstract
The present invention relates to a kind of method of extracting saponins compound from honeysuckle, comprise pulverizing, ultraviolet irradiation, hydrolysis, concentrated, precipitating and drying and other steps. The present invention adopts ultraviolet ray irradiation and the deionized water hydrolysis of proper strength, avoids using multiple extraction agent and decolorizer. Saponins compound productive rate that the method prepares is high, energy consumption is low, pollution-free and operating procedure is simple, can be widely used in suitability for industrialized production.
Description
Technical field
The invention belongs to pharmaceutical technology field, be specifically related to a kind of method of extracting saponins compound from honeysuckle.
Background technology
Honeysuckle is the general designation of Chinese medicine and plant. Plant honeysuckle has another name called honeysuckle, is the perennial half evergreen winding wood of CaprifoliaceaeMatter liana. " honeysuckle " one come from Compendium of Material Medica, because FLOSLONICERAE is just opened as white, after transfer yellow to, thereforeThe honeysuckle of gaining the name. Medicinal material honeysuckle is Caprifoliaceae woodbine honeysuckle and congener dry flower or the first flower of opening of band. Gold and silverIn spending, containing volatile aromatic oil, saponins compound, chlorogenic acid, flavone compound etc., is one of traditional Chinese medicine material, alsoThe raw material of medicine-food two-purpose, have clearing heat and detoxicating, wind-heat dissipating, effect of hepatic cholagogic.
Saponin(e (Saponin) is that aglycon is a class glucosides of triterpene or spirostane compounds, is mainly distributed in that land is high plantsIn thing, be also present on a small quantity in the marine organisms such as starfish and sea cucumber. Many Chinese herbal medicines as ginseng, polygala root, balloonflower root, Radix Glycyrrhizae, knowThe main active ingredient of mother and honeysuckle etc. all contains saponin(e. Saponin(e has the BAs such as antibacterial or antipyretic, calm, anticancer.Triterpene saponin in honeysuckle is mainly hederagenin and two kinds of compositions of oleanolic acid. Therefore, how from honeysuckle, to haveEffect ground extracts the heat subject that saponins compound is pharmaceutical field research.
In prior art, there is the multiple preparation technology who extracts saponins compound from honeysuckle, its ultrasonic waves or organic molten that adopt moreAgent is extracted, and has that recovery rate is low, a defect such as energy consumption waste and doping chemical substance more. Chinese invention patent 2010105001623Disclose a kind of from honeysuckle the method for chlorogenic acid extracting and hederagenin, but the method has been used a large amount of chemical reagent,And extraction efficiency is not high. Prior art rarely has a kind of method of effectively extracting saponins compound from honeysuckle. ForOvercome the defect of prior art, we urgently need a kind of applicable honeysuckle saponins compound of research and development to extract and productive rate is high, energyConsume the method that is easy to suitability for industrialized production low, simple to operate.
Summary of the invention
In order to overcome the defect of honeysuckle saponins compound extracting method in prior art, the invention provides a kind of from honeysuckleThe method of middle extraction saponins compound, it is raw that the method saponins compound productive rate is high, energy consumption is low, step is simply easy to industrializationProduce.
Technical scheme of the present invention is implemented in the following way:
A method of extracting saponins compound from honeysuckle, it comprises the steps:
1) pulverize: 1kg honeysuckle is put in pulverizer and pulverized, be then laid into 1 square metre;
2) ultraviolet irradiation: ultraviolet ray is lower irradiates 10-15 minute, and uitraviolet intensity is 2000uW/cm2；
3) hydrolysis: using honeysuckle weight 8-10 deionized water doubly as solvent, maintain under 0.1 atmospheric pressure state 75 DEG CBe hydrolyzed 1 hour, collect filtrate;
4) concentrated: filtrate to be placed in vacuum decker, to be concentrated in vacuo to 1/3rd of filtrate volume;
5) precipitating: add the alcohol of amount of calculation, make the alcohol content in concentrate reach 75% (v/v), leave standstill green after 1 hourThe complete precipitating of ortho acid, filters and collects filtrate and precipitation;
6) dry: precipitation obtains chlorogenic acid through 80 DEG C of vacuum drying, filtrate adopts decompression rotary evaporation to remove ethanol, and low temperature drying obtainsTo saponins compound.
Effective effect that the present invention obtains:
The present invention once extracts saponins compound and chlorogenic acid from honeysuckle simultaneously, has improved the utilization rate of raw material, greatly fallsLow cost.
The present invention extracts the method for saponins compound from honeysuckle, and productive rate is higher than general conventional method;
The present invention adopts the ultraviolet ray of proper strength to irradiate, and honeysuckle cell membrane is thoroughly destroyed, the saponins of honeysuckleThe component such as compound and chlorogenic acid is discharged to greatest extent. Find by contrast test, ultraviolet ray can improve saponin(e greatlyThe dissolution rate of compounds and chlorogenic acid.
The present invention avoids using multiple extraction agent and decolorizer, has reduced industrial energy consumption, and makes saponins compound and greenThe content of the chemical reagent in ortho acid and desalination bleaching reagent reduces greatly, has reduced purification step, can directly apply to medicineIndustry.
Extraction step of the present invention is simple to operate, is applicable to suitability for industrialized production.
Detailed description of the invention
Below employing specific embodiment is made to further explanation to the present invention, but it is not as to initiative spirit of the present inventionRestriction.
Embodiment 1
A method of extracting saponins compound from honeysuckle, it comprises the steps:
1) pulverize: 1kg honeysuckle (Pingyi honeysuckle) is put in pulverizer and pulverized, be then laid into 1 square metre;
2) ultraviolet irradiation: ultraviolet ray is lower irradiates 10 minutes, and uitraviolet intensity is 2000uW/cm2；
3) hydrolysis: using the deionized water of 8 times of honeysuckle weight as solvent, maintain under 0.1 atmospheric pressure state 75 DEG C of waterSeparate 1 hour, collect filtrate;
4) concentrated: filtrate to be placed in vacuum decker, to be concentrated in vacuo to 1/3rd of filtrate volume;
5) precipitating: add the alcohol of amount of calculation, make the alcohol content in concentrate reach 75% (v/v), leave standstill green after 1 hourThe complete precipitating of ortho acid, filters and collects filtrate and precipitation;
6) dry: precipitation obtains chlorogenic acid through 80 DEG C of vacuum drying, filtrate adopts decompression rotary evaporation to remove ethanol, and low temperature drying obtainsTo saponins compound.
Weigh, obtain altogether saponins compound 8.9g, (concrete grammar can be referring to document to adopt conventional HPLC-ELSD method" Pharmaceutical Analysis magazine " 26 (6) Li Huijun in 2006 etc.) analyze the composition of saponins compound: hederagenin 5.9gWith oleanolic acid 1.8g, other materials 1.2g.
Weigh, obtain chlorogenic acid finished product 10.8g, the purity that HPLC detects chlorogenic acid is 97.1%, and concrete grammar is referring to 2000Year version the Pharmacopoeia of the People's Republic of China.
Embodiment 2
A method of extracting saponins compound from honeysuckle, it comprises the steps:
1) pulverize: 1kg honeysuckle is put in pulverizer and pulverized, be then laid into 1 square metre;
2) ultraviolet irradiation: ultraviolet ray is lower irradiates 15 minutes, and uitraviolet intensity is 2000uW/cm2；
3) hydrolysis: using the deionized water of 10 times of honeysuckle weight as solvent, maintain under 0.1 atmospheric pressure state 75 DEG C of waterSeparate 1 hour, collect filtrate;
4) concentrated: filtrate to be placed in vacuum decker, to be concentrated in vacuo to 1/3rd of filtrate volume;
5) precipitating: add the alcohol of amount of calculation, make the alcohol content in concentrate reach 75% (v/v), leave standstill green after 1 hourThe complete precipitating of ortho acid, filters and collects filtrate and precipitation;
6) dry: precipitation obtains chlorogenic acid through 80 DEG C of vacuum drying, filtrate adopts decompression rotary evaporation to remove ethanol, and low temperature drying obtainsTo saponins compound.
Weigh, obtain altogether saponins compound 8.7g, (concrete grammar can be referring to document to adopt conventional HPLC-ELSD method" Pharmaceutical Analysis magazine " 26 (6) Li Huijun in 2006 etc.) analyze the composition of saponins compound: hederagenin 5.8gWith oleanolic acid 1.8g, other materials 1.1g.
Weigh, obtain chlorogenic acid finished product 10.9g, the purity that HPLC detects chlorogenic acid is 96.7%, and concrete grammar is referring to 2000Year version the Pharmacopoeia of the People's Republic of China.
Embodiment 3
The impact of each factor on saponins compound and chlorogenic acid extraction efficiency
1, the impact of ultraviolet irradiation intensity and time, controls other conditions constant, only changes ultraviolet irradiation parameter, and every group is tried in triplicateTest, concrete outcome is referring to table 1
Table 1
Conclusion: find by analysis, ultraviolet irradiation can improve the output of saponins compound and chlorogenic acid greatly, but along with the timeGrowth, the purity of chlorogenic acid reduces greatly, may be because high light cause chlorogenic acid occur decompose reason, to saponinsThe impact of compound is little.
2, the impact of hydrolysis time on saponins compound and chlorogenic acid productive rate
Change the time of hydrolysis, control other conditions constant, in triplicate, concrete outcome is referring to table 2 in every group of test
Table 2
Conclusion: find by analysis, hydrolysis time is after one hour, and hydrolysis time increases to the output of saponins compound and chlorogenic acid alsoWithout larger change, but the purity of chlorogenic acid can decrease.
Be understandable that, the present invention can also make other restriction, and other of making on the basis of the embodiment of the present invention changeEnter still within protection scope of the present invention.
Claims (2)
1. a method of extracting saponins compound from honeysuckle, is characterized in that, described method comprises the steps: 1) pulverize,2) ultraviolet irradiation, 3) hydrolysis, 4) concentrated, 5) precipitating, 6) dry, specific as follows:
1) pulverize: 1kg honeysuckle is put in pulverizer and pulverized, be then laid into 1 square metre;
2) ultraviolet irradiation: ultraviolet ray is lower irradiates 10-15 minute, and uitraviolet intensity is 2000 μ W/cm2；
3) hydrolysis: using honeysuckle weight 8-10 deionized water doubly as solvent, maintain under 0.1 atmospheric pressure state 75 DEG C of hydrolysis1 hour, collect filtrate;
4) concentrated: filtrate to be placed in vacuum decker, to be concentrated in vacuo to 1/3rd of filtrate volume;
5) precipitating: add the alcohol of amount of calculation, make the alcohol content in concentrate reach volume fraction 75%, leave standstill green former after 1 hourAcid is precipitating completely, filters and collects filtrate and precipitation;
6) dry: precipitation obtains chlorogenic acid through 80 DEG C of vacuum drying, filtrate adopts decompression rotary evaporation to remove ethanol, and low temperature drying obtainsSaponins compound.
2. the method for claim 1, is characterized in that, described step 2) middle-ultraviolet lamp irradiation time is 10 minutes or 15 pointsClock.
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| CN201210556010.4A CN103860622B (en) | 2012-12-07 | 2012-12-07 | A kind of method of extracting saponins compound from honeysuckle |
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| CN201210556010.4A CN103860622B (en) | 2012-12-07 | 2012-12-07 | A kind of method of extracting saponins compound from honeysuckle |
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| CN103860622A CN103860622A (en) | 2014-06-18 |
| CN103860622B true CN103860622B (en) | 2016-05-25 |
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| CN109260347A (en) * | 2018-10-25 | 2019-01-25 | 岭南师范学院 | A kind of rhizoma cyperi saponins compound separating and extracting process |
| CN111937621A (en) * | 2020-09-10 | 2020-11-17 | 福州市长乐区白英设计有限公司 | Quinoa culture room and method for removing saponin |
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| CN101406509B (en) * | 2008-11-28 | 2011-08-31 | 江苏省中国科学院植物研究所 | Lonicera confusa extract and preparation method and application thereof |
| CN102443619A (en) * | 2010-10-09 | 2012-05-09 | 苏州宝泽堂医药科技有限公司 | Method for extracting chlorogenic acid and hederagenin from honeysuckle flower |
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Effective date of registration: 20180420 Address after: 273307 north of Yinhua Road, warm water park, Pingyi Economic Development Zone, Linyi, Shandong, west of Fengshan East Road Patentee after: Shandong HP Biotechnology Co., Ltd. Address before: 273307 Shandong, Shandong, Linyi, Pingyi County, Shandong Town, Australia Pharmaceutical Technology Co., Ltd. Patentee before: Lian Jifang |
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