CN101302156B - Process for extracting chlorogenic acid from Eupatorium adenophorum - Google Patents
Process for extracting chlorogenic acid from Eupatorium adenophorum Download PDFInfo
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- CN101302156B CN101302156B CN2007100989979A CN200710098997A CN101302156B CN 101302156 B CN101302156 B CN 101302156B CN 2007100989979 A CN2007100989979 A CN 2007100989979A CN 200710098997 A CN200710098997 A CN 200710098997A CN 101302156 B CN101302156 B CN 101302156B
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- chlorogenicacid
- hemp eupatorium
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Abstract
The invention relates to an extraction process for chlorogenic acid in Eupatorium adenophorum. The method is as follows: the Eupatorium adenophorum is taken as initial raw material, 20 to 60 percent alcohol solution is firstly used to extract, then a product is further purified through macroporous resin, and a chlorogenic acid extract with the content high up to 52.56 percent can be obtained. The method makes up for the limited resource when honeysuckle is take as raw material to extract the chlorogenic acid, can also obtain the chlorogenic acid with high yield when the Eupatorium adenophorum is changed from waste to treasure, has simple method and low cost, and is suitable for industrial production.
Description
Technical field
The present invention relates to the extraction process of chlorogenicacid in a kind of Hemp Eupatorium.
Background technology
Hemp Eupatorium (Eupatorium adenophorum Spreng) is a composite family Eupatorium per nnial herb; Originate in Mexico; Import the Yunnan Province of China south into from Burma and Vietnam before and after the 1950's, because of its growth and prolificacy extremely strong, in Yunnan Province and peripheral many areas spread.Because it is herded sideline production to agricultural and has brought serious harm the destruction of ecotope.
In view of Hemp Eupatorium has become one of the most serious exotic invasive species of China's harm, various places are when the Hemp Eupatorium that tightens control spreads measure, and the numerous and confused research that launches its comprehensive utilization is tried hard to change harmful to treasure.At document 1: the intercalation universe wins, Chen Qinghua, Yang Jie; Li Huamin, Cao's col journey, Wen Yongqi; He Lan. invasive species Hemp Eupatorium chemical ingredients and bioactivity research progress. Beijing Normal University's journal (natural science edition), 2006,42 (1): in 70; Reported contain in the Hemp Eupatorium chemical ingredients chlorogenicacid (Chlorogenic acid, CHA).Chlorogenicacid is claimed chlorogenic acid again; Have antibiotic significantly, antiviral, anti-oxidant, antimutagenic, antitumor and cholagogic, step-down, increase multiple physiologically actives such as white cell, stimulating central nervous system system, be used as additive at home and abroad and be widely used in food, function (health care) food, the beverage.
Now, domestic mainly is the raw material chlorogenic acid extracting with the Japanese Honeysuckle, like document 2: the Wang Tian system; Li Yongmei. the progress of Japanese Honeysuckle. West China pharmaceutical journal, 2000,15 (4): disclosed method in 292; But only contain 1% chlorogenicacid in this method extract, productive rate is low; The Japanese Honeysuckle resource is gathered in a large number, causes the waste of resource.
Summary of the invention
The object of the present invention is to provide the extraction process of chlorogenicacid in a kind of Hemp Eupatorium; This method is starting raw material with the Hemp Eupatorium; Not only can remedy the deficiency of resource-constrained when being the raw material chlorogenic acid extracting with the Japanese Honeysuckle; Can also change harmful to treasure in that the Hemp Eupatorium poisonous weeds are used by oneself, obtain the high productivity chlorogenicacid.
The objective of the invention is to realize through following technical scheme:
The extraction process of chlorogenicacid comprises the steps: in the Hemp Eupatorium provided by the invention
1) young stem and leaf with Hemp Eupatorium is ground into powder;
2) with the Hemp Eupatorium young stem and leaf powder that obtains in the step 1), the adding volume ratio is 20-60% aqueous ethanolic solution, and with hydrochloric acid adjust pH to 2-6; At 50-80 ℃, will mix liquid and decoct 2-5 hours;
The Hemp Eupatorium young stem and leaf powder that is added and the weight ratio of aqueous ethanolic solution are 1:8-13;
3) decompress filter leaches filtrating 1; It is 20-60% aqueous ethanolic solution that filter residue is added volume ratio once more, and with hydrochloric acid adjust pH to 2-6; At 50-80 ℃, will mix liquid and reflux 2-5 hours;
4) decompress filter leaches filtrating 2; It is 20-60% aqueous ethanolic solution that filter residue is added volume ratio once more, and with hydrochloric acid adjust pH to 2-6; At 50-80 ℃, will mix liquid and reflux 2-5 hours;
5) decompress filter leaches filtrating 3; Merge three times filtrating, evaporation removes and desolvates, and gained medicinal extract is dried up with pneumatic pump, obtains the thick product of chlorogenicacid;
6) with the thick product of Amberlyst process purifying chlorogenicacid, the thick product of chlorogenicacid is dissolved in the ethanol, last appearance in macroporous resin, with deionized water as elutriant, twice on mistake post; Except that desolvating, drying obtains the chlorogenicacid extract with the water elution thing.
In the present technique scheme, the macroporous resin of said step 6) is NKA-9 type, NKA-II type or D101 type macroporous resin.
In the present technique scheme, the ratio of the deionized water of the thick product of chlorogenicacid, the ethanol that dissolves appearance and wash-out is 10g:100mL:400mL in the said step 6).
In the present technique scheme, control flow velocity 1-3mL/min when crossing post in the said step 6).
In the present technique scheme, in the said step 6), also can use the further wash-out of ethanol, obtain a spot of chlorogenicacid extract.
The present invention extracts with the ethanolic soln of 20-60% earlier, is further purified product through macroporous resin again, develops the optimal route that a cover is fit to chlorogenic acid extracting from Hemp Eupatorium.This method uses Hemp Eupatorium to be starting raw material, and it distributes wide in China, so abundant raw material.Method of the present invention can obtain content up to 52.56% chlorogenicacid extract, and high productivity obtains chlorogenicacid.Method provided by the invention is simple, and is with low cost, is suitable for suitability for industrialized production.
Embodiment
Embodiment 1,
Young stem and leaf with Hemp Eupatorium is ground into powder earlier, takes by weighing 100 gram Hemp Eupatorium young stem and leaf powder then, is loaded in the round-bottomed flask, adds the aqueous ethanolic solution of 800g20% (volume ratio), and with hydrochloric acid adjust pH to 6; At 80 ℃, will mix liquid and reflux 2 hours.
Use the B decompress filter, leach filtrating 1 and move in the eggplant type bottle; Filter residue is reinstalled in the round-bottomed flask, adds the aqueous ethanolic solution of 800g20% (volume ratio) once more, and with hydrochloric acid adjust pH to 6; At 80 ℃, will mix liquid and decoct 2 hours.
Use the B decompress filter once more, leach filtrating 2 and move in the eggplant type bottle; Filter residue is reinstalled in the round-bottomed flask, adds the aqueous ethanolic solution of 800g20% (volume ratio) once more, and with hydrochloric acid adjust pH to 6; At 80 ℃, will mix liquid and reflux 2 hours.
Decompress filter leaches filtrating 3, discards filter residue; Merge three times filtrating, evaporation removes and desolvates, and gained medicinal extract is transferred in the fine taper bottle of having weighed; Dry up with pneumatic pump, obtain the thick product 370.01g of chlorogenicacid, calculating the chlorogenicacid yield is 14.91%; Use HPLC to analyze, chlorogenic acid contents is 32.24% in medicinal extract.
Thick product with Amberlyst process purifying chlorogenicacid.At first, resin is carried out pre-treatment: with NKA-9 type macroporous resin with the deionized water swelling after flotation, soak 4h with the sodium hydroxide solution of 1mol/L then, deionized water is washed till neutrality, with the hydrochloric acid soln immersion 12h of 0.5mol/L, deionized water is washed till neutrality again; Use 70% alcohol immersion 24h at last, the continuous stirring is washed till no white casse phenomenon, only do not have the alcohol flavor with deionized water again; Deionized water soaks, and is for use.Then, pre-treatment is good macroporous resin is adorned post.At last, the thick product that takes by weighing the 10g chlorogenicacid is dissolved in the 100mL ethanol, last appearance; Use 400mL deionized water wash-out, control flow velocity 1-3mL/min crosses post twice, the water elution thing is removed desolvate, and drying obtains the chlorogenicacid extract, uses HPLC to analyze, and chlorogenic acid contents is 52.56% in this extract.
Embodiment 2,
Young stem and leaf with Hemp Eupatorium is ground into powder earlier, takes by weighing 100 gram Hemp Eupatorium leaf powder then, is loaded in the round-bottomed flask, adds the aqueous ethanolic solution of 1300g40% (volume ratio), and with hydrochloric acid adjust pH to 4; At 50 ℃, will mix liquid and decoct 5 hours.
Use the B decompress filter, leach filtrating 1 and move in the eggplant type bottle; Filter residue is reinstalled in the round-bottomed flask, adds the aqueous ethanolic solution of 1300g40% (volume ratio) once more, and with hydrochloric acid adjust pH to 4; At 50 ℃, will mix liquid and decoct 5 hours.
Use the B decompress filter once more, leach filtrating 2 and move in the eggplant type bottle; Filter residue is reinstalled in the round-bottomed flask, adds the aqueous ethanolic solution of 1300g40% (volume ratio) once more, and with hydrochloric acid adjust pH to 4; At 50 ℃, will mix liquid and decoct 5 hours.
Decompress filter leaches filtrating 3, discards filter residue; Merge three times filtrating, evaporation removes and desolvates, and gained medicinal extract is transferred in the fine taper bottle of having weighed; Dry up with pneumatic pump, obtain the thick product 568.7g of chlorogenicacid, calculating the chlorogenicacid yield is 13.89%; Use HPLC to analyze, chlorogenic acid contents is 31.75% in medicinal extract.
Thick product with Amberlyst process purifying chlorogenicacid.At first, resin is carried out pre-treatment: with D101 type macroporous resin with the deionized water swelling after flotation, soak 4h with the sodium hydroxide solution of 1mol/L then, deionized water is washed till neutrality, with the hydrochloric acid soln immersion 12h of 0.5mol/L, deionized water is washed till neutrality again; Use 70% alcohol immersion 24h at last, the continuous stirring is washed till no white casse phenomenon, only do not have the alcohol flavor with deionized water again; Deionized water soaks, and is for use.Then, pre-treatment is good macroporous resin is adorned post.At last, the thick product that takes by weighing the 10g chlorogenicacid is dissolved in the 100mL ethanol, last appearance; Use 400mL deionized water wash-out, control flow velocity 1-3mL/min crosses post twice, the water elution thing is removed desolvate, and drying obtains the chlorogenicacid extract, uses HPLC to analyze, and chlorogenic acid contents is 50.08% in this extract.
Embodiment 3,
Leaf with Hemp Eupatorium is ground into powder earlier, takes by weighing 100 gram Hemp Eupatorium leaf powder then, is loaded in the round-bottomed flask, adds the aqueous ethanolic solution of 1000g60% (volume ratio), and with hydrochloric acid adjust pH to 2; At 60 ℃, will mix liquid and decoct 4 hours.
Use the B decompress filter, leach filtrating 1 and move in the eggplant type bottle; Filter residue is reinstalled in the round-bottomed flask, adds the aqueous ethanolic solution of 1000g60% (volume ratio) once more, and with hydrochloric acid adjust pH to 2; At 60 ℃, will mix liquid and decoct 4 hours.
Use the B decompress filter once more, leach filtrating 2 and move in the eggplant type bottle; Filter residue is reinstalled in the round-bottomed flask, adds the aqueous ethanolic solution of 1000g60% (volume ratio) once more, and with hydrochloric acid adjust pH to 2; At 60 ℃, will mix liquid and decoct 4 hours.
Decompress filter leaches filtrating 3, discards filter residue; Merge three times filtrating, evaporation removes and desolvates, and gained medicinal extract is transferred in the fine taper bottle of having weighed; Dry up with pneumatic pump, obtain the thick product 444.1g of chlorogenicacid, calculating the chlorogenicacid yield is 14.23%; Use HPLC to analyze, chlorogenic acid contents is 32.04% in medicinal extract.
Thick product with Amberlyst process purifying chlorogenicacid.At first; Resin is carried out pre-treatment: with NKA-II type macroporous resin with the deionized water swelling after flotation, soak 4h with the sodium hydroxide solution of 1mol/L then, deionized water is washed till neutrality; Hydrochloric acid soln with 0.5mol/L soaks 12h again, and deionized water is washed till neutrality; Use 70% alcohol immersion 24h at last, the continuous stirring is washed till no white casse phenomenon, only do not have the alcohol flavor with deionized water again; Deionized water soaks, and is for use.Then, pre-treatment is good macroporous resin is adorned post.At last, the thick product that takes by weighing the 10g chlorogenicacid is dissolved in the 100mL ethanol, last appearance; Use 400mL deionized water wash-out, control flow velocity 1-3mL/min crosses post twice, the water elution thing is removed desolvate, and drying obtains the chlorogenicacid extract, uses HPLC to analyze, and chlorogenic acid contents is 51.07% in this extract.Also can use the further wash-out of ethanol, obtain a spot of chlorogenicacid extract.
Claims (5)
1. the extraction process of chlorogenicacid in the Hemp Eupatorium comprises the steps:
1) leaf with Hemp Eupatorium is ground into powder;
2) with the Hemp Eupatorium leaf powder that obtains in the step 1), the adding volume ratio is 20-60% aqueous ethanolic solution, and with hydrochloric acid adjust pH to 2-6; At 50-80 ℃, will mix liquid and decoct 2-5 hours;
The Hemp Eupatorium leaf powder that is added and the weight ratio of aqueous ethanolic solution are 1:8-13;
3) decompress filter leaches filtrating 1; It is 20-60% aqueous ethanolic solution that filter residue is added volume ratio once more, and with hydrochloric acid adjust pH to 2-6; At 50-80 ℃, will mix liquid and decoct 2-5 hours;
4) decompress filter leaches filtrating 2; It is 20-60% aqueous ethanolic solution that filter residue is added volume ratio once more, and with hydrochloric acid adjust pH to 2-6; At 50-80 ℃, will mix liquid and decoct 2-5 hours;
5) decompress filter leaches filtrating 3; Merge three times filtrating, evaporation removes and desolvates, and gained medicinal extract is dried up with pneumatic pump, obtains the thick product of chlorogenicacid;
6) with the thick product of Amberlyst process purifying chlorogenicacid, the thick product of chlorogenicacid is dissolved in the ethanol, last appearance in macroporous resin, with deionized water as elutriant, twice on mistake post; Except that desolvating, drying obtains the chlorogenicacid extract with the water elution thing.
2. the extraction process of chlorogenicacid in the Hemp Eupatorium as claimed in claim 1 is characterized in that: the macroporous resin of said step 6) is NKA-9 type, NKA-II type or D101 type macroporous resin.
3. the extraction process of chlorogenicacid in the Hemp Eupatorium as claimed in claim 1 is characterized in that: the ratio of the deionized water of the thick product of chlorogenicacid, the ethanol that dissolves appearance and wash-out is 10g:100mL:400mL in the said step 6).
4. the extraction process of chlorogenicacid in the Hemp Eupatorium as claimed in claim 1 is characterized in that: in the said step 6), and control flow velocity 1-3mL/min when crossing post.
5. the extraction process of chlorogenicacid in the Hemp Eupatorium as claimed in claim 1 is characterized in that: in the said step 6), use the further wash-out of ethanol, obtain a spot of chlorogenicacid extract.
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101838200B (en) * | 2009-03-20 | 2014-04-09 | 上海相宜本草化妆品股份有限公司 | Method for extracting and separating chlorogenic acid from honeysuckle |
| CN103274935B (en) * | 2013-05-20 | 2015-04-22 | 中国农业科学院植物保护研究所 | Method for extracting nepetin compounds from crofton weed |
| CN105367424B (en) * | 2015-12-24 | 2018-06-19 | 攀枝花市西宇生物科技有限公司 | The method that high-purity chlorogenic acid is prepared with Eupatorium adenophorum |
| CN110156604A (en) * | 2019-06-21 | 2019-08-23 | 普洱学院 | A kind of extracting method of yellow fruit eggplant Content of Chlorogenic Acid |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1740137A (en) * | 2005-09-10 | 2006-03-01 | 江南大学 | Chlorogenic acid extracting and purifying process from sunflower seed dregs |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1740137A (en) * | 2005-09-10 | 2006-03-01 | 江南大学 | Chlorogenic acid extracting and purifying process from sunflower seed dregs |
Non-Patent Citations (1)
| Title |
|---|
| 杨婕 闫乾胜.入侵物种紫茎泽兰化学成分及生物活性研究进展.《北京师范大学学报》.2006,第42卷(第1期),71-72. * |
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