CN102302586A - Extraction method of total iridoid glycoside from hedyotis diffusa willd - Google Patents
Extraction method of total iridoid glycoside from hedyotis diffusa willd Download PDFInfo
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- CN102302586A CN102302586A CN201110225557A CN201110225557A CN102302586A CN 102302586 A CN102302586 A CN 102302586A CN 201110225557 A CN201110225557 A CN 201110225557A CN 201110225557 A CN201110225557 A CN 201110225557A CN 102302586 A CN102302586 A CN 102302586A
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- hedyotidis diffusae
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Abstract
The invention provides an extraction method of total iridoid glycoside from hedyotis diffusa willd. The method is characterized in that: the hedyotis diffusa willd serving as a raw material is extracted with ethanol which serves as an entrainer by adopting a supercritical CO2 extraction method; the extract is extracted with ethanol solution and concentrated, and the concentrate passes through macroporous adsorption resin and is eluted with ethanol; and the eluate is subjected to membrane concentration and drying to obtain the total iridoid glycoside. The method has high efficiency, no use of harmful reagent and low degree of environmental pollution and can easily realize industrialization.
Description
Technical field
The invention belongs to technical field of Chinese medicines, relate to a kind of method of from Herba Hedyotidis Diffusae, extracting total iridoid glycoside.
Background technology
Herba Hedyotidis Diffusae (
Hedyotis diffusa(Willd) Roxb.) be Rubiaceae cerastium plant, all herbal medicine has multiple physiologically actives such as heat-clearing and toxic substances removing, blood circulation promoting and blood stasis dispelling, anti-inflammation and antitumor.Chemical constituent mainly comprises chemical compounds such as flavonoid, iridoid glycosides, anthraquinone class.Iridoid glycosides is one type of important chemical compound in the natural product; Also be one of main type chemical substance in the Herba Hedyotidis Diffusae, common iridoid mainly contains scandoside methyl ester, deacetyl asperulosidic acid methyl ester, asperuloside acid and asperuloside in the Herba Hedyotidis Diffusae.It has multiple biological activitys such as cell toxicant, antitumor, antioxidation.Iridoid belongs to the hemiacetal derivant of smelly ant dialdehyde, and the hemiacetal structural instability hydrolysis be prone to take place or variation such as rearrangement takes place in the acid medium again.Li Cunman etc. have studied the stability of iridoid glycosides compound in the Herba Hedyotidis Diffusae, and discovery iridoid glycoside compounds is deposited in the vial more stable in room temperature pure water medium, and should not surpass 6h 60 ℃ of standing times.
The enrichment method of iridoid glycoside compounds is mainly realized through the separation and purification of macroporous adsorbent resin; One Chinese patent application numbers 200810010309.3; A kind of Herba Hedyotidis Diffusae extract and method for separating and preparing thereof; With the Herba Hedyotidis Diffusae medical material is raw material, separates and steps such as process-scale chromatography separates through water extraction, precipitate with ethanol, membrance separation, non-polar macroporous resin, obtains extract.This method impurity is many, and bigger to the film damage, cost is high.One Chinese patent application numbers 200610028468.7, the monomeric extraction of iridoid, separation method in the Herba Hedyotidis Diffusae adopt the alcohol-water solution extracted twice; Macroporous resin column is separated, and water alcohol eluting is gone up Sephadex LH-20 after eluent concentrates and firmly once thought; The alcohol water elution concentrates crystallization; Obtain E-6-O-coumaric acyl Herba Paederiae time glycosides methyl ester, there are shortcomings such as poor reproducibility, length consuming time, automaticity are low in this method.
Through the document retrieval, still do not have at present and adopt supercritical fluid from Herba Hedyotidis Diffusae, to extract the method report of iridoid glycoside.
Summary of the invention
The objective of the invention is in order a kind of easy, low power consuming, environmental protection to be provided, effectively from Herba Hedyotidis Diffusae, to extract the method for total iridoid glycoside fast.
The objective of the invention is to realize through following technical scheme:
From Herba Hedyotidis Diffusae, extract the method for total iridoid glycoside, it is characterized in that comprising following processing step: (1) is ground into coarse powder with the Herba Hedyotidis Diffusae herb, add in the supercritical extraction jar, and be that entrainer extracts with ethanol, collect extract; (2) above-mentioned extract is put into Soxhlet extractor, add the alcoholic solution that 5-6 doubly measures, extract 3-6 hour repeatedly, extracting solution is concentrated into does not have the alcohol flavor; (3) above-mentioned concentrated solution is passed through macroporous adsorptive resins, use 0-10% ethanol and 30-80% ethanol elution successively, collect eluent, through membrance concentration, filtration, vacuum drying obtains total iridoid glycoside.
The said supercritical CO of step (1)
2Extraction conditions is: extracting pressure is 25-35MPa, and extraction temperature is 30-50 ℃, supercritical CO
2Flow is 20-35kg/h, and the extraction time is 1-6 hour, and parsing pressure is 4-11MPa, and resolution temperature is 45-60 ℃, and entrainer ethanol volume fraction is 70-95%.
The said Suo Shi extracting of step (2) uses the ethanol volume fraction to be 50-70%.
The said macroporous adsorbent resin of step (3) is selected from a kind of among XDA-1, ADS-7, NKA, the HPD450.
The said membrance concentration of step (3) is to pass through ultrafilter membrane earlier, and permeate adds NF membrane again and concentrates, and said ultrafilter membrane is the hollow fiber ultrafiltration film of molecular cut off 3000-8000, and the NF membrane molecular cut off is 200-300, optional polyether sulfone of material or politef.
The present invention compared with prior art, beneficial effect is: the present invention adopts supercritical fluid extraction, extraction yield is high, environmental pollution is few, automaticity is higher, but enlargement of scale production; The present invention adopts resin absorption and membrance separation to concentrate technological coupling, and medicinal liquid makes the composition of polluted membrane reduce greatly behind resin purification, is that effectively preprocess method is used in ultrafiltration; And ultrafiltration can be played further purified effect; Improve content of effective, remove the shed particles of resin, technology of the present invention does not need heating; Effective ingredient is played the certain protection effect, improved the stability of product.
The specific embodiment
Embodiment 1:
Get the Herba Hedyotidis Diffusae herb and be ground into coarse powder, get 2kg and drop in the supercritical extraction jar, add percent by volume and be 80% alcoholic solution as entrainer, addition is 0.10kg; At extracting pressure 27.6MPa, 40 ℃ of extraction temperature, CO
2Flow is extraction 2 hours under the condition of 22kg/h; It is 4MPa that pressure tank is resolved in control, and temperature is 45 ℃, collects extract; Extract is put into Soxhlet extractor, add the alcoholic solution of 5 times of amounts 60%, extract 3 hours repeatedly; Extracting solution is evaporated to does not have the alcohol flavor, concentrated solution is passed through the XDA-1 macroporous adsorptive resins, successively with deionized water and 50% ethanol elution; Collect 50% ethanol elution; Eluent is through the hollow poly (ether-sulfone) ultrafiltration membrane system of molecular cut off 3000, and filtered solution is 200 polyether sulfone filtering film again through molecular cut off, collects concentrated solution; Vacuum drying obtains total iridoid glucoside extract 2.1g, and cyclenes ether terpene component total content is 78% in the extract.
Embodiment 2:
Get the Herba Hedyotidis Diffusae herb and be ground into coarse powder, get 2kg and drop in the supercritical extraction jar, add percent by volume and be 80% alcoholic solution as entrainer, addition is 0.12kg; At extracting pressure 29.1MPa, 32 ℃ of extraction temperature, CO
2Flow is extraction 1 hour under the condition of 30kg/h; It is 6MPa that pressure tank is resolved in control, and temperature is 56 ℃, collects extract; Extract is put into Soxhlet extractor, add the alcoholic solution of 6 times of amounts 75%, extract 6 hours repeatedly; Extracting solution is evaporated to does not have the alcohol flavor, and concentrated solution through the HPD450 macroporous adsorptive resins, is used 10% ethanol and 70% ethanol elution successively; Collect 70% ethanol elution; Eluent is through the hollow politef ultrafiltration membrane system of molecular cut off 4000, and filtered solution is 200 politef NF membrane again through molecular cut off, collects concentrated solution; Vacuum drying obtains total iridoid glucoside extract 2.3g, and cyclenes ether terpene component total content is 76% in the extract.
Embodiment 3:
Get the Herba Hedyotidis Diffusae herb and be ground into coarse powder, get 2kg and drop in the supercritical extraction jar, add percent by volume and be 80% alcoholic solution as entrainer, addition is 0.15kg; At extracting pressure 25.5MPa, 44 ℃ of extraction temperature, CO
2Flow is extraction 3 hours under the condition of 35kg/h; It is 7MPa that pressure tank is resolved in control, and temperature is 58 ℃, collects extract; Extract is put into Soxhlet extractor, add the alcoholic solution of 5 times of amounts 70%, extract 5 hours repeatedly; Extracting solution is evaporated to does not have the alcohol flavor, and concentrated solution through the XDA-1 macroporous adsorptive resins, is used 10% ethanol and 40% ethanol elution successively; Collect 40% ethanol elution; Eluent is through the hollow poly (ether-sulfone) ultrafiltration membrane system of molecular cut off 8000, and filtered solution is 300 politef NF membrane again through molecular cut off, collects concentrated solution; Vacuum drying obtains total iridoid glucoside extract 2.5g, and cyclenes ether terpene component total content is 75% in the extract.
Embodiment 4:
Get the Herba Hedyotidis Diffusae herb and be ground into coarse powder, get 2kg and drop in the supercritical extraction jar, add percent by volume and be 80% alcoholic solution as entrainer, addition is 0.18kg; At extracting pressure 32.8MPa, 47 ℃ of extraction temperature, CO
2Flow is extraction 6 hours under the condition of 20kg/h; It is 11MPa that pressure tank is resolved in control, and temperature is 49 ℃, collects extract; Extract is put into Soxhlet extractor, add the alcoholic solution of 5 times of amounts 90%, extract 4 hours repeatedly; Extracting solution is evaporated to does not have the alcohol flavor, concentrated solution is passed through the ADS-7 macroporous adsorptive resins, successively with deionized water and 80% ethanol elution; Collect 80% ethanol elution; Eluent is through the hollow politef ultrafiltration membrane system of molecular cut off 6000, and filtered solution is 300 polyether sulfone filtering film again through molecular cut off, collects concentrated solution; Vacuum drying obtains total iridoid glucoside extract 2.2g, and cyclenes ether terpene component total content is 73% in the extract.
Embodiment 5:
Get the Herba Hedyotidis Diffusae herb and be ground into coarse powder, get 2kg and drop in the supercritical extraction jar, add percent by volume and be 80% alcoholic solution as entrainer, addition is 0.14kg; At extracting pressure 34.4MPa, 50 ℃ of extraction temperature, CO
2Flow is extraction 5 hours under the condition of 28kg/h; It is 8MPa that pressure tank is resolved in control, and temperature is 60 ℃, collects extract; Extract is put into Soxhlet extractor, add the alcoholic solution of 6 times of amounts 95%, extract 5 hours repeatedly; Extracting solution is evaporated to does not have the alcohol flavor, and concentrated solution through the NKA macroporous adsorptive resins, is used 10% ethanol and 60% ethanol elution successively; Collect 60% ethanol elution; Eluent is through the hollow poly (ether-sulfone) ultrafiltration membrane system of molecular cut off 5000, and filtered solution is 200 politef NF membrane again through molecular cut off, collects concentrated solution; Vacuum drying obtains total iridoid glucoside extract 2.3g, and cyclenes ether terpene component total content is 74% in the extract.
Claims (5)
1. from Herba Hedyotidis Diffusae, extract the method for total iridoid glycoside, it is characterized in that comprising following processing step: (1) is ground into coarse powder with the Herba Hedyotidis Diffusae herb, add in the supercritical extraction jar, and be that entrainer extracts with ethanol, collect extract; (2) above-mentioned extract is put into Soxhlet extractor, add the alcoholic solution that 5-6 doubly measures, extract 3-6 hour repeatedly, extracting solution is concentrated into does not have the alcohol flavor; (3) above-mentioned concentrated solution is passed through macroporous adsorptive resins, use 0-10% ethanol and 30-80% ethanol elution successively, collect eluent, through membrance concentration, filtration, vacuum drying obtains total iridoid glycoside.
2. the method for from Herba Hedyotidis Diffusae, extracting total iridoid glycoside according to claim 1 is characterized in that the said supercritical CO of step (1)
2Extraction conditions is: extracting pressure is 25-35MPa, and extraction temperature is 30-50 ℃, supercritical CO
2Flow is 20-35kg/h, and the extraction time is 1-6 hour, and parsing pressure is 4-11MPa, and resolution temperature is 45-60 ℃, and entrainer ethanol volume fraction is 70-95%.
3. the method for from Herba Hedyotidis Diffusae, extracting total iridoid glycoside according to claim 1 is characterized in that the said Suo Shi extracting of step (2) uses the ethanol volume fraction to be 50-70%.
4. the method for from Herba Hedyotidis Diffusae, extracting total iridoid glycoside according to claim 1 is characterized in that, the said macroporous adsorbent resin of step (3) is selected from a kind of among XDA-1, ADS-7, NKA, the HPD450.
5. the method for from Herba Hedyotidis Diffusae, extracting total iridoid glycoside according to claim 1; It is characterized in that; The said membrance concentration of step (3) is to pass through ultrafilter membrane earlier, and permeate adds NF membrane again and concentrates, and said ultrafilter membrane is the hollow fiber ultrafiltration film of molecular cut off 3000-8000; The NF membrane molecular cut off is 200-300, optional polyether sulfone of material or politef.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112851621A (en) * | 2021-01-28 | 2021-05-28 | 汕头大学医学院 | Total iridoid extract of caulis et folium piperis, extraction and purification method and application thereof |
| CN115105441A (en) * | 2021-03-22 | 2022-09-27 | 香奈儿香水美妆品公司 | Swertiae extract and cosmetic composition comprising the same |
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2011
- 2011-08-08 CN CN201110225557A patent/CN102302586A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112851621A (en) * | 2021-01-28 | 2021-05-28 | 汕头大学医学院 | Total iridoid extract of caulis et folium piperis, extraction and purification method and application thereof |
| CN115105441A (en) * | 2021-03-22 | 2022-09-27 | 香奈儿香水美妆品公司 | Swertiae extract and cosmetic composition comprising the same |
| US11957781B2 (en) | 2021-03-22 | 2024-04-16 | Chanel Parfums Beaute | Swertia chirata extract and cosmetic compositions comprising same |
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Application publication date: 20120104 |