CN111110713B - Extraction method of tussilago farfara polyphenol compounds - Google Patents
Extraction method of tussilago farfara polyphenol compounds Download PDFInfo
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- CN111110713B CN111110713B CN202010033245.XA CN202010033245A CN111110713B CN 111110713 B CN111110713 B CN 111110713B CN 202010033245 A CN202010033245 A CN 202010033245A CN 111110713 B CN111110713 B CN 111110713B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/28—Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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Abstract
The invention provides a method for extracting polyphenol compounds from coltsfoot flower, and relates to the field of preparation of effective ingredients of traditional Chinese medicines. The extraction method of the polyphenol compound comprises the following steps: (1) choline chloride and glycerol in a molar ratio of 1: 2, placing the mixture in a water bath at the temperature of 80 ℃ to synthesize an extraction solvent; (2) adding the extraction solvent into the common coltsfoot flower according to the mass ratio of 1:6, performing ultrasonic extraction for 40min, and centrifuging to obtain a supernatant; (3) eluting the supernatant with HP-20 macroporous resin to remove the extraction solvent, sequentially eluting with 0.1% formic acid water and 50% ethanol solution, collecting 50% ethanol eluate fraction, and concentrating to obtain polyphenol compounds in flos Farfarae. The invention has the advantages that: the extraction method can selectively extract and prepare the polyphenol compounds in one step, has simple steps and low cost, and avoids the problems of large pollution, strong volatility, flammability, explosiveness and the like of organic reagents.
Description
Technical Field
The invention relates to preparation of effective components of traditional Chinese medicines, in particular to a method for extracting polyphenol compounds from common coltsfoot flower by using a novel extraction solvent.
Technical Field
Tussilagofafara L. of Compositae family, has effects of moistening lung, descending qi, relieving cough and eliminating phlegm, and is mainly used for cough, asthma, anti-inflammatory, etc. clinically. The chemical components of flos Farfarae comprise flavonoids, sterols, phenolic acids, alkaloids, volatile oils, and sesquiterpenes. Wherein, the flavonoids and the phenolic acids belong to the polyphenol compounds, and the earlier research shows that the components have the functions of reducing phlegm and relieving cough (Journal of Pharmaceutical and biological Analysis,2013,75:158-164) and have the prospect of further developing new drugs.
The prior art method for preparing polyphenol compounds from coltsfoot flower needs to extract by organic solvent and then extract or separate by macroporous resin, but a large amount of organic reagents such as methanol, ethanol, ethyl acetate, n-butanol and the like are generally used in the extraction or extraction process, and the organic reagents have the problems of strong volatility, flammability, explosiveness and environmental pollution.
Disclosure of Invention
The invention aims to solve the problems, and provides a method for extracting polyphenol compounds in flos farfarae by using a novel extraction solvent; the method can avoid the problems of the existing method, such as heavy pollution of organic reagents, strong volatility, flammability, explosiveness and the like.
The invention provides a method for extracting coltsfoot flower polyphenol compounds, which comprises the following steps:
(1) choline chloride and glycerol are mixed in a molar ratio of 1: 2, placing the mixture in a water bath at the temperature of 75-85 ℃ to generate an extraction solvent;
(2) adding flos Farfarae into the above extraction solvent at a mass ratio of 1:6-10, ultrasonic extracting for 30-60min, centrifuging, and collecting supernatant;
(3) eluting the supernatant with HP-20 macroporous resin to remove the extraction solvent, sequentially eluting with 0.1% formic acid water and 50% ethanol solution, collecting 50% ethanol eluate fraction, and concentrating to obtain flos Farfarae polyphenol compounds.
The temperature of the water bath in the step (1) is preferably 80 ℃.
The mass ratio of the coltsfoot flower to the extraction solvent in the step (2) is preferably 1: 6.
The ultrasonic extraction time in the step (2) is preferably 40 min.
Compared with the prior art, the invention has the beneficial effects that: the novel extraction solvent (the extraction solvent generated by choline chloride and glycerol) provided by the invention is used for selectively extracting and preparing the polyphenol compounds from the coltsfoot flower in one step, the method has simple steps and low cost, and the problems of large pollution, strong volatility, flammability, explosiveness and the like caused by using a large amount of organic reagents are avoided.
Drawings
FIG. 1 is a chromatogram of flos Farfarae after extraction with choline chloride-glycerol extraction solvent
FIG. 2 is a chromatogram of flos Farfarae after extraction with 95% ethanol
FIG. 3 is a chromatogram of flos Farfarae extracted with 70% ethanol
Detailed Description
The present invention will be described in more detail and fully with reference to the following examples.
The reagents and equipment used in the examples were as follows:
1 apparatus
Agilent 1260 high performance liquid chromatograph (Agilent corporation), G7111A quaternary pump, G7117C DAD detector, ultrasonic cleaner (KQ5200E, ultrasound instruments ltd, kunshan), Venusil MP C18 column (250mm × 4.6mm,5 μm), low speed centrifuge (kaihu science instruments ltd).
2 reagent
Choline chloride (purity not less than 98%, sahn chemical technology company), glycerol (purity not less than 99%, Tianjin Damao Co., Ltd.), acetonitrile (chromatographic purity, Fisher Co., Ltd.), phosphoric acid (chromatographic purity, Tianjin Damao Co., Ltd.), HP20 macroporous resin (Lonicera Japonica GmbH Co., Ltd.).
Example 1
1. Mixing 28g of choline chloride and 36.8g of glycerol (the molar ratio is 1: 2), and heating in a water bath at 80 ℃ until a uniform and transparent solution is generated, namely an extraction solvent;
2. weighing 10 g of flos farfarae, adding 60g of the above extraction solvent, performing ultrasonic extraction for 40min, centrifuging for 5min at 3500rmp, and taking supernatant;
3. soaking HP20 macroporous resin in 95% ethanol overnight, then carrying out column chromatography, wherein the column volume is 100mL, washing with distilled water until no alcohol smell exists, taking the obtained supernatant, sequentially eluting with 1000mL of 0.1% formic acid water and 1000mL of 50% ethanol, collecting 50% ethanol eluent, concentrating and drying to obtain the coltsfoot flower polyphenol compounds.
Comparative example 1 ultrasonic extraction of flos Farfarae with 95% ethanol
Weighing 10 g of flos farfarae, adding 60mL of 95% ethanol, carrying out ultrasonic extraction for 40min, centrifuging for 5min at 3500rmp, taking supernatant, filtering with a 0.45-micron filter membrane, and detecting by high performance liquid chromatography.
Comparative example 2 ultrasonic extraction of flos Farfarae with 70% ethanol
Weighing 10 g of flos farfarae, adding 60mL of 70% ethanol, carrying out ultrasonic extraction for 40min, centrifuging for 5min at 3500rmp, taking supernatant, filtering with a 0.45-micron filter membrane, and detecting by high performance liquid chromatography.
In comparative examples and comparative examples, flavonoids and phenolic acid compounds (figure 1) can be selectively extracted by using the choline chloride-glycerol extraction solvent provided by the invention, wherein the peak 1 is chlorogenic acid, the peak 2 is rutin, the peak 3 is hyperin, the peak 4 is isochlorogenic acid B, the peak 5 is isochlorogenic acid A, and the peak 6 is isochlorogenic acid C; whereas the traditional ethanol extraction is not selective (fig. 2, fig. 3).
Claims (4)
1. A method for extracting coltsfoot flower polyphenol compounds is characterized by comprising the following steps:
(1) choline chloride and glycerol in a molar ratio of 1: 2, placing the mixture in a water bath at the temperature of 75-85 ℃ to generate an extraction solvent;
(2) adding flos Farfarae into the above extraction solvent at a mass ratio of 1:6-10, ultrasonic extracting for 30-60min, centrifuging, and collecting supernatant;
(3) eluting the supernatant with HP-20 macroporous resin to remove the extraction solvent, sequentially eluting with 0.1% formic acid and 50% ethanol solution, collecting the 50% ethanol eluate, and concentrating to obtain flos Farfarae polyphenol compounds.
2. The method for extracting coltsfoot flower polyphenol compounds as claimed in claim 1, wherein the water bath temperature in the step (1) is 80 ℃.
3. The method for extracting coltsfoot flower polyphenol compounds as claimed in claim 1, wherein the mass ratio of coltsfoot flower to extraction solvent in the step (2) is 1: 6.
4. The method for extracting coltsfoot flower polyphenol compounds as claimed in claim 1, wherein the ultrasonic extraction time in the step (2) is 40 min.
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| CN106518590B (en) * | 2016-09-18 | 2018-11-23 | 曲阜师范大学 | The method that polyphenols in granatum is extracted using eutectic solvent |
| CN107184461A (en) * | 2017-05-23 | 2017-09-22 | 林燕 | A kind of extracting method of pawpaw polyphenol |
| CN108030809B (en) * | 2018-01-26 | 2020-12-25 | 山西大学 | Method for extracting anti-inflammatory and antioxidant components of fructus forsythiae |
| CN108948102B (en) * | 2018-08-27 | 2020-11-10 | 广州五羊日化有限公司 | Method for extracting tea polyphenol |
| CN110623991A (en) * | 2019-10-21 | 2019-12-31 | 华侨大学 | Method for extracting polyphenol compounds in artichoke by using ultrasonic-assisted eutectic solvent |
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