CN103860622A - Method for extracting saponin compounds from honeysuckle - Google Patents
Method for extracting saponin compounds from honeysuckle Download PDFInfo
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- CN103860622A CN103860622A CN201210556010.4A CN201210556010A CN103860622A CN 103860622 A CN103860622 A CN 103860622A CN 201210556010 A CN201210556010 A CN 201210556010A CN 103860622 A CN103860622 A CN 103860622A
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- flos lonicerae
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Abstract
The invention relates to a method for extracting saponin compounds from honeysuckle. The method comprises the steps of grinding, ultraviolet radiation, hydrolysis, concentration, precipitation, drying and the like. The method adopts ultraviolet with proper intensity for radiation and deionized water for hydrolysis and avoids using various extraction reagents and decoloring agents. The saponin compounds prepared by the method has high yield and the method has the advantages of low energy consumption, no pollution and simple operating steps and can be widely applied to industrial production.
Description
Technical field
The invention belongs to pharmaceutical technology field, be specifically related to a kind of method of extracting saponins compound from Flos Lonicerae.
Background technology
Flos Lonicerae is the general designation of Chinese crude drug and plant.Plant Flos Lonicerae has another name called Radix Ophiopogonis, is the perennial half evergreen winding bejuco of Caprifoliaceae." Flos Lonicerae " one come from Compendium of Material Medica, because Flos Lonicerae is just opened as white, after transfer yellow to, Flos Lonicerae hence obtains one's name.Medical material Flos Lonicerae is Caprifoliaceae woodbine Radix Ophiopogonis and congener dry flower or the first flower of opening of band.In Flos Lonicerae, containing volatile aromatic oil, saponins compound, chlorogenic acid, flavone compound etc., is one of Chinese medicine material, is also the raw material of medicine-food two-purpose, has heat-clearing and toxic substances removing, wind-heat dissipating, effect of hepatic cholagogic.
Saponin (Saponin) is that aglycon is a class glucosides of triterpene or spirostane compounds, is mainly distributed in the higher plant of land, is also present on a small quantity in the marine organisms such as Asterias amurensis Lutken and Stichopus japonicus.Many Chinese herbal medicine all contain saponin as the main effective ingredient of Radix Ginseng, Radix Polygalae, Radix Platycodonis, Radix Glycyrrhizae, the Rhizoma Anemarrhenae and Flos Lonicerae etc.Saponin has the biologic activity such as antibacterial or antipyretic, calm, anticancer.Triterpene saponin in Flos Lonicerae is mainly helexin and two kinds of compositions of oleanolic acid.Therefore, how from Flos Lonicerae, effectively to extract the heat subject that saponins compound is pharmaceutical field research.
In prior art, have the multiple preparation technology who extracts saponins compound from Flos Lonicerae, its ultrasound wave or organic solvent extraction of adopting, exist that extraction ratio is low, the defect such as energy consumption waste and doping chemical substance more more.Chinese invention patent 2010105001623 disclose a kind of from Flos Lonicerae the method for chlorogenic acid extracting and helexin, 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 Flos Lonicerae.In order to overcome the defect of prior art, we urgently need to research and develop, and a kind of applicable Flos Lonicerae saponins compound extracts and productive rate is high, energy consumption is low, the method that is easy to suitability for industrialized production simple to operate.
Summary of the invention
In order to overcome the defect of Flos Lonicerae saponins compound extracting method in prior art, the invention provides a kind of method of extracting saponins compound from Flos Lonicerae, the method saponins compound productive rate is high, energy consumption is low, step is simply easy to suitability for industrialized production.
Technical scheme of the present invention is implemented in the following way:
A method of extracting saponins compound from Flos Lonicerae, it comprises the steps:
1) pulverize: 1kg Flos Lonicerae is put in pulverizer and pulverized, be then laid into 1 square metre;
2) ultra-vioket radiation: irradiate 10-15 minute under ultraviolet, uitraviolet intensity is 2000uW/cm
2;
3) hydrolysis: using Flos Lonicerae weight 8-10 deionized water doubly as solvent, maintain under 0.1 atmospheric pressure state, 75 ℃ are 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 ethanol of amount of calculation, make the alcohol content in concentrated solution reach 75% (v/v), leave standstill the complete precipitating of chlorogenic acid after 1 hour, filter and collect filtrate and precipitation;
6) dry: precipitation obtains chlorogenic acid through 80 ℃ of vacuum dryings, filtrate adopts decompression rotary evaporation to remove ethanol, and cold drying obtains saponins compound.
Effective effect that the present invention obtains:
The present invention once extracts saponins compound and chlorogenic acid from Flos Lonicerae simultaneously, has improved the utilization rate of raw material, greatly reduces cost.
The present invention extracts the method for saponins compound from Flos Lonicerae, and productive rate is higher than general conventional method;
The present invention adopts the ultraviolet radiation of proper strength, and Flos Lonicerae cell wall is thoroughly destroyed, and the component such as saponins compound and chlorogenic acid of Flos Lonicerae is discharged to greatest extent.Find by contrast test, ultraviolet can improve the dissolution rate of saponins compound and chlorogenic acid greatly.
The present invention avoids using multiple extraction agent and depigmenting agent, has reduced industrial energy consumption, and chemical reagent in saponins compound and chlorogenic acid and the content of desalination bleaching reagent are reduced greatly, has reduced purification step, can directly apply to pharmaceuticals industry.
Extraction step of the present invention is simple to operate, is applicable to suitability for industrialized production.
The specific embodiment
Below employing specific embodiment is made to further explanation to the present invention, but it is not as the restriction to initiative spirit of the present invention.
Embodiment 1
A method of extracting saponins compound from Flos Lonicerae, it comprises the steps:
1) pulverize: 1kg Flos Lonicerae (Pingyi Flos Lonicerae) is put in pulverizer and pulverized, be then laid into 1 square metre;
2) ultra-vioket radiation: irradiate under ultraviolet 10 minutes, uitraviolet intensity is 2000uW/cm
2;
3) hydrolysis: using the deionized water of 8 times of Flos Lonicerae weight as solvent, maintain under 0.1 atmospheric pressure state, 75 ℃ of hydrolysis 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 ethanol of amount of calculation, make the alcohol content in concentrated solution reach 75% (v/v), leave standstill the complete precipitating of chlorogenic acid after 1 hour, filter and collect filtrate and precipitation;
6) dry: precipitation obtains chlorogenic acid through 80 ℃ of vacuum dryings, filtrate adopts decompression rotary evaporation to remove ethanol, and cold drying obtains saponins compound.
Weigh, obtain altogether saponins compound 8.9g, adopt conventional HPLC-ELSD method (concrete grammar can referring to document " pharmaceutical analysis magazine " 26 (6) Li Huijun in 2006 etc.) to analyze the composition of saponins compound: helexin 5.9g and 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 was referring to the version Pharmacopoeia of the People's Republic of China in 2000.
Embodiment 2
A method of extracting saponins compound from Flos Lonicerae, it comprises the steps:
1) pulverize: 1kg Flos Lonicerae is put in pulverizer and pulverized, be then laid into 1 square metre;
2) ultra-vioket radiation: irradiate under ultraviolet 15 minutes, uitraviolet intensity is 2000uW/cm
2;
3) hydrolysis: using the deionized water of 10 times of Flos Lonicerae weight as solvent, maintain under 0.1 atmospheric pressure state, 75 ℃ of hydrolysis 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 ethanol of amount of calculation, make the alcohol content in concentrated solution reach 75% (v/v), leave standstill the complete precipitating of chlorogenic acid after 1 hour, filter and collect filtrate and precipitation;
6) dry: precipitation obtains chlorogenic acid through 80 ℃ of vacuum dryings, filtrate adopts decompression rotary evaporation to remove ethanol, and cold drying obtains saponins compound.
Weigh, obtain altogether saponins compound 8.7g, adopt conventional HPLC-ELSD method (concrete grammar can referring to document " pharmaceutical analysis magazine " 26 (6) Li Huijun in 2006 etc.) to analyze the composition of saponins compound: helexin 5.8g and 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 was referring to the version Pharmacopoeia of the People's Republic of China in 2000.
Embodiment 3
The impact of each factor on saponins compound and chlorogenic acid extraction efficiency
1, the impact of ultra-vioket radiation intensity and time, controls other conditions constant, only changes ultra-vioket radiation parameter, tests in triplicate for every group, and concrete outcome is referring to table 1
Table 1
Conclusion: find by analysis, ultraviolet radiation can improve the output of saponins compound and chlorogenic acid greatly, and still, along with the growth of time, the purity of chlorogenic acid reduces greatly, may be because high light causes chlorogenic acid that the reason of decomposing occurs, little on the impact of saponins compound.
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 growth there is no larger change to the output of saponins compound and chlorogenic acid, 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 improve still within protection scope of the present invention.
Claims (2)
1. a method of extracting saponins compound from Flos Lonicerae, is characterized in that, described method comprises the steps: 1) pulverize 2) ultra-vioket radiation, 3) hydrolysis, 4) concentrated, 5) precipitating, 6) dry.Specific as follows:
1) pulverize: 1kg Flos Lonicerae is put in pulverizer and pulverized, be then laid into 1 square metre;
2) ultra-vioket radiation: irradiate 10-15 minute under ultraviolet, uitraviolet intensity is 2000uW/cm
2;
3) hydrolysis: using Flos Lonicerae weight 8-10 deionized water doubly as solvent, maintain under 0.1 atmospheric pressure state, 75 ℃ are 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 ethanol of amount of calculation, make the alcohol content in concentrated solution reach 75% (v/v), leave standstill the complete precipitating of chlorogenic acid after 1 hour, filter and collect filtrate and precipitation;
6) dry: precipitation obtains chlorogenic acid through 80 ℃ of vacuum dryings, filtrate adopts decompression rotary evaporation to remove ethanol, and cold drying obtains saponins compound.
2. the method for claim 1, is characterized in that, described step 2) middle-ultraviolet lamp irradiation time preferably 10 minutes or 15 minutes.
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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 true CN103860622A (en) | 2014-06-18 |
| CN103860622B CN103860622B (en) | 2016-05-25 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101406509A (en) * | 2008-11-28 | 2009-04-15 | 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 |
-
2012
- 2012-12-07 CN CN201210556010.4A patent/CN103860622B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101406509A (en) * | 2008-11-28 | 2009-04-15 | 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| Publication number | Publication date |
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| CN103860622B (en) | 2016-05-25 |
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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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