CN102381975B - Extraction process for chlorogenic acid in parasenecio firmus - Google Patents
Extraction process for chlorogenic acid in parasenecio firmus Download PDFInfo
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- CN102381975B CN102381975B CN 201110394577 CN201110394577A CN102381975B CN 102381975 B CN102381975 B CN 102381975B CN 201110394577 CN201110394577 CN 201110394577 CN 201110394577 A CN201110394577 A CN 201110394577A CN 102381975 B CN102381975 B CN 102381975B
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- chlorogenic acid
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- 235000001368 chlorogenic acid Nutrition 0.000 title claims abstract description 42
- CWVRJTMFETXNAD-FWCWNIRPSA-N 3-O-Caffeoylquinic acid Natural products O[C@H]1[C@@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-FWCWNIRPSA-N 0.000 title claims abstract description 41
- PZIRUHCJZBGLDY-UHFFFAOYSA-N Caffeoylquinic acid Natural products CC(CCC(=O)C(C)C1C(=O)CC2C3CC(O)C4CC(O)CCC4(C)C3CCC12C)C(=O)O PZIRUHCJZBGLDY-UHFFFAOYSA-N 0.000 title claims abstract description 41
- CWVRJTMFETXNAD-KLZCAUPSSA-N Neochlorogenin-saeure Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O CWVRJTMFETXNAD-KLZCAUPSSA-N 0.000 title claims abstract description 41
- CWVRJTMFETXNAD-JUHZACGLSA-N chlorogenic acid Chemical compound O[C@@H]1[C@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-JUHZACGLSA-N 0.000 title claims abstract description 41
- 229940074393 chlorogenic acid Drugs 0.000 title claims abstract description 41
- FFQSDFBBSXGVKF-KHSQJDLVSA-N chlorogenic acid Natural products O[C@@H]1C[C@](O)(C[C@@H](CC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O FFQSDFBBSXGVKF-KHSQJDLVSA-N 0.000 title claims abstract description 41
- BMRSEYFENKXDIS-KLZCAUPSSA-N cis-3-O-p-coumaroylquinic acid Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)cc2)[C@@H]1O)C(=O)O BMRSEYFENKXDIS-KLZCAUPSSA-N 0.000 title claims abstract description 41
- 238000000605 extraction Methods 0.000 title claims abstract description 29
- 241001277226 Parasenecio firmus Species 0.000 title abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 40
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 57
- 229960004756 ethanol Drugs 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- 239000000284 extract Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 235000012054 meals Nutrition 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000000741 silica gel Substances 0.000 claims description 9
- 229910002027 silica gel Inorganic materials 0.000 claims description 9
- 238000010898 silica gel chromatography Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 238000010828 elution Methods 0.000 claims description 7
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 238000007598 dipping method Methods 0.000 claims description 2
- 239000000469 ethanolic extract Substances 0.000 claims description 2
- SRCZQMGIVIYBBJ-UHFFFAOYSA-N ethoxyethane;ethyl acetate Chemical compound CCOCC.CCOC(C)=O SRCZQMGIVIYBBJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000003208 petroleum Substances 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 238000002137 ultrasound extraction Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 5
- 239000000843 powder Substances 0.000 abstract description 4
- 206010028980 Neoplasm Diseases 0.000 abstract description 3
- 210000003169 central nervous system Anatomy 0.000 abstract description 3
- 150000003254 radicals Chemical class 0.000 abstract description 3
- 238000011160 research Methods 0.000 abstract description 2
- 241000894006 Bacteria Species 0.000 abstract 1
- 241000700605 Viruses Species 0.000 abstract 1
- 210000004369 blood Anatomy 0.000 abstract 1
- 239000008280 blood Substances 0.000 abstract 1
- 230000036772 blood pressure Effects 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 210000000232 gallbladder Anatomy 0.000 abstract 1
- 210000000265 leukocyte Anatomy 0.000 abstract 1
- 210000004185 liver Anatomy 0.000 abstract 1
- 229940126601 medicinal product Drugs 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 239000000126 substance Substances 0.000 description 6
- 239000003814 drug Substances 0.000 description 5
- 238000004809 thin layer chromatography Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 241000208688 Eucommia Species 0.000 description 3
- 238000004440 column chromatography Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 239000000796 flavoring agent Substances 0.000 description 3
- 235000019634 flavors Nutrition 0.000 description 3
- 230000001077 hypotensive effect Effects 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- OKKJLVBELUTLKV-MZCSYVLQSA-N Deuterated methanol Chemical compound [2H]OC([2H])([2H])[2H] OKKJLVBELUTLKV-MZCSYVLQSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 208000001953 Hypotension Diseases 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000000259 anti-tumor effect Effects 0.000 description 2
- 230000000840 anti-viral effect Effects 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
- 230000004071 biological effect Effects 0.000 description 2
- 230000002279 cholagogic effect Effects 0.000 description 2
- 210000003494 hepatocyte Anatomy 0.000 description 2
- 208000021822 hypotensive Diseases 0.000 description 2
- 230000001603 reducing effect Effects 0.000 description 2
- 230000004936 stimulating effect Effects 0.000 description 2
- 238000001644 13C nuclear magnetic resonance spectroscopy Methods 0.000 description 1
- 238000005160 1H NMR spectroscopy Methods 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229940123457 Free radical scavenger Drugs 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 241000133024 Syneilesis Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000003260 anti-sepsis Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 238000012742 biochemical analysis Methods 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 210000000748 cardiovascular system Anatomy 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 231100000957 no side effect Toxicity 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000452 restraining effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
Abstract
The invention belongs to the technical field of medicinal product researches, and particularly relates to an extraction process for chlorogenic acid in parasenecio firmus. Alcohol is added into coarse powder of parasenecio firmus for extraction, and after extracting solution is extracted, the extracted solution is separated and purified for obtaining the chlorogenic acid. The chlorogenic acid obtained in the invention mainly has the effects of resisting bacterium, resisting virus, increasing white blood cells, protecting liver and gallbladder, resisting tumour, lowering blood pressure, lowering blood fat, cleaning free radical and exciting the central nervous system and the like. The preparation method is simple, and the extraction ratio is 1.2 percent.
Description
Technical field
The invention belongs to the pharmaceutical prod studying technological domain, particularly the extraction process of chlorogenic acid in the Da Ye wild carraway.
Background technology
The Da Ye wild carraway
Parasenecio firmus(Komar.) Y. L. Chen has another name called the Da Ye Herba Syneilesis Aconitifoliae, and the plant for the composite family wild carraway belongs to produces ground such as Chinese Jilin Province Fusong, Changbai Mountain, Huijiang.Be born under the thick forest or border and opening, 800～1100 meters of height above sea level, NORTHERN KOREA also has.
Chlorogenic acid has biological activity widely, and bioactive research has been deep into a plurality of fields such as food, health care, medicine and daily-use chemical industry to modern science to chlorogenic acid.Chlorogenic acid is a kind of important biological material, have antibiotic, antiviral, increase effects such as white cell, hepatic cholagogic, antitumor, hypotensive, reducing blood-fat, removing free radical and stimulating central nervous system system; Modern pharmacology experimental results show that bark of eucommia chlorogenic acid has anticancer and presses down the effect of cancer, the Japan scholar has studied the variation originality restraining effect of bark of eucommia chlorogenic acid, find that this effect is relevant with different originality compositions of resistance such as chlorogenic acids, disclosed the significance of chlorogenic acid to tumor prevention; By a large amount of evidences, this biological activity of chlorogenic acid can produce provide protection to cardiovascular systems to chlorogenic acid as a kind of free-radical scavengers and antioxidant; Confirm that through clinical trial for many years bark of eucommia chlorogenic acid has tangible hypotensive effect, and curative effect is steady, nontoxic, have no side effect.Ministry of Health's " drug standard " includes 170 kinds of Chinese patent medicines with clearing heat and detoxicating, antisepsis and anti-inflammation, all contains chlorogenic acid and is main component.At present, in the production of medicines such as silver yellow preparation, 'Shuang Hualian ', with chlorogenic acid as one of important indicator of quality control.Polyphenols such as chlorogenic acid are called as " the 7th class nutrient substance ", are widely used in healthcare industry, characteristics such as that the health care medicine that has added chlorogenic acid has is clearing heat and detoxicating, beauty treatment skin moisten.Chlorogenic acid still is important chemical reagent in addition, all has widely to use in biochemical analysis and chemical industry.
But so far, as yet about chlorogenic acid The Chemical Constituents in the Da Ye wild carraway.
Summary of the invention
The object of the present invention is to provide the extraction process of chlorogenic acid in a kind of Da Ye wild carraway.
The technical solution used in the present invention is as follows:
The extraction process of chlorogenic acid in the Da Ye wild carraway adds ethanol with the meal of Da Ye wild carraway and extracts, and extracting solution extraction back extraction liquid separation and purification obtains chlorogenic acid.
It is as follows to add the process that ethanol extracts: the alcohol solution dipping that the dry meal of Da Ye wild carraway is incorporated as 8～10 times of quality of meal spends the night, supersound extraction 20-40min then, and extracting solution reclaims ethanol; Described ethanolic soln mass concentration is 70-90%.
Frequency is 80-100Hz during supersound extraction, and temperature is 25-30 ℃.
Further, repeat the process 3～5 times that meal adds ethanol ultrasonic extraction and reclaims ethanol in the extracting solution, united extraction liquid extracts.
Extracting solution adds that isopyknic water is mixed respectively to extract three times collection ethyl acetate layer component after evenly successively with sherwood oil, ethyl acetate and propyl carbinol during extraction.
To be dissolved in the dehydrated alcohol behind 50-70 ℃ of water bath method of ethyl acetate layer component, mix with isopyknic silica gel, pass through silica gel column chromatography after volatilizing solvent, adopt petroleum ether-ethyl acetate to carry out gradient elution, merge same composition and also carry out obtaining chlorogenic acid behind silica gel column chromatography, the purifying.
The ratio of sherwood oil and ethyl acetate is followed successively by 15:1,12:1,10:1,8:1,5:1,1:1,1:2,1:5 during gradient elution, collects same composition in the 10:1 elutriant.
Concrete, the preparation chlorogenic acid comprises following process:
Step 1): 80% alcohol immersion that the dry meal of Da Ye wild carraway (40 order) is added 8～10 times of amounts is spent the night, and ultrasonic (80Hz, 30 ℃) extract 30min, and extracting solution reclaims ethanol and is concentrated into nothing alcohol flavor, extracts so repeatedly 3～5 times, merges concentrated solution;
Step 2): with 1 the water of concentrated solution adding and concentrated solution equivalent respectively extracts three times with sherwood oil, ethyl acetate, propyl carbinol successively), obtains the ethyl acetate layer segment thus;
Step 3): with 2) is dissolved in the dehydrated alcohol behind 60 ℃ of water bath methods of ethyl acetate part in, mix with silica gel (100～200 order), volatilize solvent, by silica gel (200～300 order) column chromatography, eluting solvent is selected sherwood oil: the ethyl acetate (gradient elution of 15:1～1:5);
Step 4): with 3) gained 10:1 elutriant detects with TLC in, merges same composition, and concentrating under reduced pressure carries out silica gel column chromatography more repeatedly;
Step 5): with 4) similar flow point merges in, and concentrating under reduced pressure gets concentrated solution, separates out crystallization.
Step 6): with 5) crystal obtains chlorogenic acid monomer with recrystallizing methanol in.
The raw material of preparation chlorogenic acid of the present invention is the Da Ye wild carraway
Parasenecio firmus(Komar.) herb of Y. L. Chen.
The present invention has following advantage with respect to prior art:
Effects such as that the chlorogenic acid that the present invention obtains mainly has is antibiotic, antiviral, increase white cell, hepatic cholagogic, antitumor, hypotensive, reducing blood-fat, removing free radical and stimulating central nervous system system.The preparation method is simple, and extraction yield is 1.2%.
Embodiment
Below with specific embodiment technical scheme of the present invention is described, but protection scope of the present invention is not limited thereto:
Embodiment 1
Step 1): with the dry meal 1000g(40 of Da Ye wild carraway order) 80% alcohol immersion that adds 8 times of amounts is spent the night, and ultrasonic (80Hz, 30 ℃) extract 30min, and extracting solution reclaims ethanol and is concentrated into nothing alcohol flavor, extracts so repeatedly 4 times, merges concentrated solution;
Step 2): with 1 the water of concentrated solution adding and concentrated solution equivalent respectively extracts three times with sherwood oil, ethyl acetate, propyl carbinol successively), obtains the ethyl acetate layer segment thus;
Step 3): with 2) is dissolved in the dehydrated alcohol behind 60 ℃ of water bath methods of ethyl acetate part in, mix with equal-volume silica gel (100～200 order), volatilize solvent, by silica gel (200～300) column chromatography, eluting solvent is selected sherwood oil: the ethyl acetate (gradient elution of 15:1～1:5), both ratios are followed successively by 15:1,12:1,10:1,8:1,5:1,1:1,1:2,1:5 during concrete wash-out, collect the 10:1 elutriant;
Step 4): with 3) gained 10:1 elutriant TLC detects in, merges same composition, is evaporated to small volume, carries out silica gel column chromatography more repeatedly;
Step 5): with 4) similar flow point merges in, and concentrating under reduced pressure gets concentrated solution, separates out crystallization.
Step 6): with 5) crystal obtains pale yellow powder 12.2g with recrystallizing methanol in.
The gained powder, 207～209 ℃ of mp.Slightly soluble in 25 ℃ of water, solubleness increases in the hot water.Be soluble in ethanol and acetone, be slightly soluble in ethyl acetate, be insoluble in lipotropy organic solvents such as chloroform, ether, benzene.Behind silica gel thin-layer chromatography, spot has fluorescence under the 254nm ultraviolet lamp, meets the iodine vapor displaing yellow, and the 10% ethanol solution of sulfuric acid back 105 ℃ of roasting plates of spraying show black, and its Rf value is consistent with the Rf value of chlorogenic acid standard substance.
1H-NMR（600MHz，DMSO-d
6）δ：7.43（1H，d，J=16.2Hz，H-β），7.06（1H，H-2'），6.96（1H，d，J=7.8Hz，H-6'），6.74（1H，d，J=7.8Hz，H-5'），6.21（1H，d，J=16.2Hz，H-α），5.16（1H，H-3），3.46（1H，d，J=7.8Hz，H-5），3.89（1H，H-4），1.79（4H，m，H-2，6）。
13C-NMR（150MHz，CD3OD）δ：175.1（C-7），166.7（C-8），147.7（C-4'），145.1（C-3'），144.9（C-β），125.9（C-1'），121.0（C-6'），114.6（C-2'），113.4（C-5'），113.3（C-α），74.2（C-1），71.6（C-4），70.1（C-3），69.4（C-5），36.9（C-2），36.3（C-6）。Physicochemical data and standard diagram basically identical with the chlorogenic acid standard substance.The gained compound is chlorogenic acid (chlorogcnic acid).
Embodiment 2
Step 1): with the dry meal 1000g(40 of Da Ye wild carraway order) 80% alcohol immersion that adds 10 times of amounts is spent the night, and ultrasonic (100Hz, 25 ℃) extract 30min, and extracting solution reclaims ethanol and is concentrated into nothing alcohol flavor, extracts so repeatedly 3 times, merges concentrated solution;
Step 2): with 1 the water of concentrated solution adding and concentrated solution equivalent respectively extracts three times with sherwood oil, ethyl acetate, propyl carbinol successively), obtains the ethyl acetate layer segment thus;
Step 3): with 2) is dissolved in the dehydrated alcohol behind 60 ℃ of water bath methods of ethyl acetate part in, mix with equal-volume silica gel (100～200 order), volatilize solvent, by silica gel (200～300) column chromatography, eluting solvent is selected sherwood oil: the ethyl acetate (gradient elution of 15:1～1:5), both ratios are followed successively by 15:1,12:1,10:1,8:1,5:1,1:1,1:2,1:5 during concrete wash-out, collect the 10:1 elutriant;
Step 4): with 3) gained 10:1 elutriant TLC detects in, merges same composition, is evaporated to small volume, carries out silica gel column chromatography more repeatedly;
Step 5): with 4) similar flow point merges in, and concentrating under reduced pressure gets concentrated solution, separates out crystallization.
Step 6): with 5) crystal obtains pale yellow powder 11.8g with recrystallizing methanol in.
Above-described embodiment is the preferred embodiment of the present invention, but embodiments of the present invention are not restricted to the described embodiments, and the change that other any the present invention of not deviating from does all should be the substitute mode of equivalence, is included within protection scope of the present invention.
Claims (7)
1. the extraction process of chlorogenic acid in the Da Ye wild carraway is characterized in that, it is that the ethanol of 70-90% soaks and supersound extraction that the meal of Da Ye wild carraway is added mass concentration, and extracting solution extraction back extraction liquid obtains chlorogenic acid by silica gel column chromatography separating purification.
2. the extraction process of chlorogenic acid in the Da Ye wild carraway as claimed in claim 1, it is characterized in that, the process that adding ethanol extracts is as follows: the alcohol solution dipping that the dry meal of Da Ye wild carraway is added 8～10 times of quality of meal spends the night, supersound extraction 20-40min then, extracting solution reclaims ethanol.
3. the extraction process of chlorogenic acid in the Da Ye wild carraway as claimed in claim 2 is characterized in that frequency is 80-100Hz during supersound extraction, and temperature is 25-30 ℃.
4. the extraction process of chlorogenic acid in the Da Ye wild carraway as claimed in claim 2 is characterized in that, repeats the process 3～5 times that meal adds ethanol ultrasonic extraction and reclaims ethanol in the extracting solution, and united extraction liquid extracts.
5. as the extraction process of chlorogenic acid in the described Da Ye wild carraway of one of claim 1-4, it is characterized in that, extracting solution adds that isopyknic water is mixed respectively to extract three times collection ethyl acetate layer component after evenly successively with sherwood oil, ethyl acetate and propyl carbinol during extraction.
6. the extraction process of chlorogenic acid in the Da Ye wild carraway as claimed in claim 5, it is characterized in that, to be dissolved in the dehydrated alcohol behind 50-70 ℃ of water bath method of ethyl acetate layer component, mix with isopyknic silica gel, pass through silica gel column chromatography after volatilizing solvent, adopt petroleum ether-ethyl acetate to carry out gradient elution, the merging same composition also carries out obtaining chlorogenic acid behind silica gel column chromatography, the purifying.
7. the extraction process of chlorogenic acid in the Da Ye wild carraway as claimed in claim 6, it is characterized in that, the ratio of sherwood oil and ethyl acetate is followed successively by 15:1,12:1,10:1,8:1,5:1,1:1,1:2,1:5 during gradient elution, collects same composition in the 10:1 elutriant.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060020029A1 (en) * | 2004-07-02 | 2006-01-26 | Shimasaki Craig D | Pharmaceutical compositions from ethnobotanicals |
| CN101823964A (en) * | 2010-03-12 | 2010-09-08 | 山东大学威海分校 | Technology for preparing chlorogenic acid in viburnum sargentii koehne leaves |
| CN102000132A (en) * | 2010-11-22 | 2011-04-06 | 山东大学威海分校 | Preparation method of traditional Chinese medicine preparation and antioxidation application thereof |
-
2011
- 2011-12-02 CN CN 201110394577 patent/CN102381975B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060020029A1 (en) * | 2004-07-02 | 2006-01-26 | Shimasaki Craig D | Pharmaceutical compositions from ethnobotanicals |
| CN101823964A (en) * | 2010-03-12 | 2010-09-08 | 山东大学威海分校 | Technology for preparing chlorogenic acid in viburnum sargentii koehne leaves |
| CN102000132A (en) * | 2010-11-22 | 2011-04-06 | 山东大学威海分校 | Preparation method of traditional Chinese medicine preparation and antioxidation application thereof |
Non-Patent Citations (6)
| Title |
|---|
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| 不同植物中绿原酸的提取;董雄辎等;《安徽农业科学》;20091231;第37卷(第1期);第16-17页 * |
| 大叶蟹甲草不同萃取部位抗氧化活性研究;朱启光 等;《人参研究》;20110430(第4期);第20-23页 * |
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| 董雄辎等.不同植物中绿原酸的提取.《安徽农业科学》.2009,第37卷(第1期),第16-17页. |
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