CN101016287B - Method of extracting flavone from cabbage leaf - Google Patents
Method of extracting flavone from cabbage leaf Download PDFInfo
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- CN101016287B CN101016287B CN2007100174037A CN200710017403A CN101016287B CN 101016287 B CN101016287 B CN 101016287B CN 2007100174037 A CN2007100174037 A CN 2007100174037A CN 200710017403 A CN200710017403 A CN 200710017403A CN 101016287 B CN101016287 B CN 101016287B
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Abstract
The invention discloses an extracting method of flavone from cabbage leaf, which comprises the following steps: adopting cabbage leaf as raw material and 80% alcohol as extracting liquid; extracting twice at 50-60 deg.c with ultrasonic frequency at 60Hz; combining filtrate; filtering; removing impurity through ligarine; shortening the extracting time with high-flavone content under mild testing condition; improving the separation of flavone and theoretical tower floor number effectively.
Description
Technical field
The invention belongs to the extracting method of vegetable nutrient technology, be specifically related to a kind of method of from cabbage leaf, extracting flavones.
Background technology
Vitamin P complex is the aldehydes matter that occurring in nature exists, and also claims vitamin P, and normal and vitamins C companion deposits, and the platymiscium secondary metabolite is one of main active ingredient in the nature medicinal plant.Its physiological function mainly contains: antioxygenation, promote beta Cell of islet recovery, lowering blood glucose and serum cholesterol, improve sugar tolerance, to adrenolytic blood glucose increasing effect, suppress aldose reductase, regulate the animal lipid metabolism, improve the Endogenous Hormones relevant with growth, promote the nonspecific immunity function of mytolin deposition, acceleration growth of animal, enhancing body and humoral immune function, anti-bacteria and anti-virus.Flavonoid is mainly derived from vegetables, fruit in the meals.Chinese cabbage is one of main vegetables of China, and cultivated area reached 269.9 ten thousand hm in 2003
2, accounting for 15.75% of the vegetables total area, annual production 10,197 ten thousand t account for 19.24% (national agricultural statistics summary 2004) of vegetables ultimate production.Say in the ancient medical book " Mingyi Bielu " that Chinese cabbage energy tonneau stomach removes restlessness in the chest, relieving alcoholism.Qing Dynasty's supplementary Amplifications of the Compendium of Materia Medica record is said, cabbage juice, and sweet temperature is nontoxic, sharp stomach and intestine, except that uncomfortable in chest, sharp stool and urine, what is ended is coughed, and winter is good especially.Therefore be necessary the Chinese cabbage flavones is studied.
Flavonoid compound polarity is stronger, is soluble in polar solvent, as: buck, hot water, methyl alcohol, ethanol etc.In the plant extracting method comparative maturity of flavones mainly contain three kinds: extraction, water-bath heat reflow method, supersonic method.Shortcomings such as impurity is many, extraction time long because of extracting for preceding two kinds of methods, extracting solution deposits that easy corruption is rotten, follow-up filter operation difficulty, yield are lower, use seldom now.Ultrasonic auxiliary law is to utilize effects such as hyperacoustic vibration cavitation, mechanical disintegration, stirring, make the cavitation bubble collapse of plant tissue instantaneous generation in solvent, and make cell rupture in the tissue, be beneficial to solvent and be penetrated into vegetable cell inside, composition in the cell is entered in the solvent, acceleration interpenetrates, dissolves, to increase the dissolving of flavonoid compound in solvent.The advantage of ultrasonic extraction technology is to improve extraction ratio of effective constituents significantly, shortens extraction time, generally handles dozens of minutes and gets final product, and high-level efficiency is economized solvent.Also have at present microwave method, macroreticular resin absorbing method etc., it is former thereby temporarily be not extensive use of that though these methods have its unique distinction, because its use range is limited, equipment cost is higher, complex process, technology are still immature etc.
Summary of the invention
The object of the present invention is to provide a kind of method of from cabbage leaf, extracting flavones.
To achieve these goals, the present invention is achieved by following technical solution:
Extract the method for flavones in a kind of cabbage leaf, it is characterized in that this method is a raw material with the Chinese cabbage leaf, drying is pulverized, the ethanolic soln extraction, and filtration, removal of impurities, reclaim under reduced pressure, vacuum concentration obtain flavonoid extracts, specifically comprise the following steps:
Step 1 with the cabbage leaf 5min that completes, in 50 ℃～60 ℃ oven dry down, is carried out superfine grinding under 110 ℃, obtain 60 purpose Chinese cabbage leaf powder;
Step 2 places the supersound extraction device with Chinese cabbage leaf powder, as extracting solvent, under 50 ℃ temperature, is the ultrasonic wave of 60Hz with the frequency with the ethanolic soln of 80% massfraction, extracts 2 times, and the solid-liquid ratio of each extraction is 1: 20, merging filtrate;
Step 3 will obtain extracting solution after the filtrate filtration, extracts with 2-3 sherwood oil doubly, removes the oil-soluble impurities in the extracting solution;
Step 4, the extracting solution reclaim under reduced pressure after the removal of impurity can obtain flavonoid extracts behind the vacuum concentration.
Extracting solution after the above-mentioned removal of impurity carries out the concentrating under reduced pressure crystallization to extracting solution under 35 ℃, collect crystal, obtains cabbage flavones crude product.
The usefulness of extracting the method for flavones from Chinese cabbage provided by the invention is:
1) simple: should method is simple, the gentle and control easily of experiment condition.
2) save time: extraction time is short.
3) efficient: flavones content is higher in the extracting solution, and promptly yield is higher.
4) with low cost: owing to there is not adding other organic solvent except that ethanol in the reaction process, therefore can not introduce other impurity in leaching process, this has just simplified the step of separation and purification greatly, has reduced the cost of separation and purification; The equal reusable edible of ethanol that it is selected for use and sherwood oil.
5) environmental protection: the solvent that is used to extract can recycle, so leaching process does not have waste liquid to discharge, helps environment protection.
Embodiment
The method of from cabbage leaf, extracting flavones of the present invention, with the cabbage leaf 10min that under 120 ℃, completes, in 50 ℃～60 ℃ oven dry down, pulverize, Chinese cabbage leaf powder is placed the supersound extraction device, and the ethanol with 80% is extracting solution, and solid-liquid ratio is (g/mL) 1: 20, extract 50 ℃～60 ℃ of temperature, under 50 ℃ temperature,, extracted 1 hour with ultrasonic frequency 60Hz, extract altogether twice, each solid-liquid ratio that extracts is 1: 20, and merging filtrate will obtain extracting solution after the filtrate filtration, extract with 2-3 sherwood oil doubly, remove the oil-soluble impurities in the extracting solution; Extracting solution reclaim under reduced pressure after the removal of impurity obtains flavonoid extracts behind the vacuum concentration.
Do standard substance with rutin and make typical curve, measure content of total flavone in the extract with ultra-violet absorption spectrum.
The method of extracting flavones from cabbage leaf provided by the invention is used the mixed solvent of ethanol/water, under certain temperature and certain ultrasonic frequency the Chinese cabbage sample is extracted, can high efficiency acquisition flavones.
Method of the present invention is to carry out according to the similar principle that mixes.The essence of its process is the mass transfer process that chromocor compound shifts to solvent from the Chinese cabbage cell interior: at first, solvent molecule is delivered to the surface of Chinese cabbage solid particulate from the solvent main body.Then, the Chinese cabbage cell is because the ultrasonic wave effect is broken, and solvent is penetrated into vegetable cell inside.Next, the composition in the cell enters in the solvent rapidly owing to action of ultrasonic waves.At last, chromocor compound is dissolved in the solvent main body from the Chinese cabbage solid particulate.Wherein, chromocor compound solubleness size and be two principal elements that influence extraction yield in selected solvent to the complexity of solvent diffusion.And the velocity of diffusion of chromocor compound in selected solvent depends on factors such as extracting temperature, solid-liquid ratio, solid particulate size, ultrasonic frequency.
Chromocor compound is present in the vegetable cell usually, and the diffusional resistance that cytolemma produces makes that its lixiviate speed ratio is less.Carry out such as drying or the pre-treatment pulverizing to raw material, help breaking of plant cell membrane, solvent also enters the inner directly dissolving of vegetable cell flavones easily, thereby can improve extraction efficiency.
It below is the specific embodiment that the contriver provides.
Embodiment 1:
After the orange leaf-head Chinese cabbage that just enters the heading stage gathered, weigh, clean, blade is spread out the 5min that in baking oven, completes under 110 ℃, 50～60 ℃ of oven dry down, be crushed to 60 orders, accurately take by weighing pulverize after drying to the Chinese cabbage sample 0.1g of constant weight in triangular flask, be extraction agent with 20mL 80% ethanol, ultrasonic frequency is 60Hz, extract 1h, extract altogether twice.Merging filtrate filters, and is settled to 50mL with water, with 2 times petroleum ether degreasing, obtain flavone extractive, through spectrophotometry, getting flavones content is 0.653mg, under 35 ℃ extracting solution is carried out the concentrating under reduced pressure crystallization, collect crystal, this is a flavone gruff bring up substance, obtains the 0.671mg crystal altogether.
Embodiment 2:
After orange leaf-head Chinese cabbage is gathered with the ripening stage, weigh, clean, blade is spread out the 5min that in baking oven, completes under 110 ℃, 50～60 ℃ of oven dry down, be crushed to 60 orders, accurately take by weighing pulverize after drying to the Chinese cabbage sample 0.2g of constant weight in triangular flask, be extraction agent with 40mL 80% ethanol, ultrasonic frequency is 60Hz, extract 1h, extract altogether twice.Merging filtrate filters, and is settled to 100mL with water, 2 times petroleum ether degreasing, obtain flavone extractive, through spectrophotometry, getting flavones content is 0.244mg, under 35 ℃ extracting solution is carried out the concentrating under reduced pressure crystallization, collect crystal, this is a flavone gruff bring up substance, obtains the 0.250mg crystal altogether.
Embodiment 3:
After common Chinese cabbage is gathered with the ripening stage, weigh, clean, blade is spread out the 5min that in baking oven, completes under 110 ℃, 50～60 ℃ of oven dry down, be crushed to 60 orders, accurately take by weighing pulverize after drying to the Chinese cabbage sample 0.5g of constant weight in triangular flask, be extraction agent with 100mL 80% ethanol, ultrasonic frequency is 60Hz, extract 1h, extract altogether twice.Merging filtrate, filter, under 35 ℃, extracting solution is evaporated to about 20mL,, obtains flavone extractive with the degreasing of 50mL petroleum ether extraction, through spectrophotometry, its flavones content is 0.087mg, under 35 ℃ concentrated solution is proceeded the concentrating under reduced pressure crystallization, collects crystal, this is a flavone gruff bring up substance, obtains the 0.089mg crystal altogether.
Claims (2)
1. a method of extracting flavones from cabbage leaf is characterized in that, specifically comprises the following steps:
Step 1 with the cabbage leaf 5min that completes, in 50 ℃～60 ℃ oven dry down, is carried out superfine grinding under 110 ℃, obtain 60 purpose Chinese cabbage leaf powder;
Step 2 places the supersound extraction device with Chinese cabbage leaf powder, as extracting solvent, under 50 ℃ temperature, is the ultrasonic wave of 60Hz with the frequency with the ethanolic soln of 80% massfraction, extracts 2 times, and the solid-liquid ratio of each extraction is 1: 20, merging filtrate;
Step 3 will obtain extracting solution after the filtrate filtration, extracts with 2-3 sherwood oil doubly, removes the oil-soluble impurities in the extracting solution;
Step 4, the extracting solution reclaim under reduced pressure after the removal of impurity can obtain flavonoid extracts behind the vacuum concentration.
2. the method for claim 1 is characterized in that, the extracting solution after the described removal of impurity carries out the concentrating under reduced pressure crystallization to extracting solution under 35 ℃, collects crystal, obtains cabbage flavones crude product.
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| CN2007100174037A CN101016287B (en) | 2007-02-12 | 2007-02-12 | Method of extracting flavone from cabbage leaf |
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| CN2007100174037A CN101016287B (en) | 2007-02-12 | 2007-02-12 | Method of extracting flavone from cabbage leaf |
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| CN101016287B true CN101016287B (en) | 2010-07-28 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102727584A (en) * | 2012-06-29 | 2012-10-17 | 厦门牡丹香化实业有限公司 | Method for extracting flavonoids from camphor tree leaves |
| CN104435021A (en) * | 2014-11-11 | 2015-03-25 | 青海康普生物科技股份有限公司 | Extraction method of sea buckthorn flavonoids |
| CN105362326B (en) * | 2015-09-18 | 2019-10-11 | 龙岩学院 | A kind of method and its application for extracting natural active matter from Chinese cabbage |
| CN108211417B (en) * | 2018-01-30 | 2020-01-03 | 河南省商业科学研究所有限责任公司 | Preparation method and application of extraction auxiliary substance for extracting flavone from plant |
| CN111440661B (en) * | 2020-04-21 | 2023-01-20 | 广州大学 | Banana-pineapple peel flavone natural antioxidant compound agent and preparation method and application thereof |
| CN114698733A (en) * | 2022-04-29 | 2022-07-05 | 华南农业大学 | Flavone extract of fagopyrum fulvestrant leaves and application of flavone extract in preparation of stylosanthes guianensis silage |
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| CN1172178C (en) * | 2001-02-16 | 2004-10-20 | 中国科学院长春应用化学研究所 | Method for testing quality of acanthopanax leaf |
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Patent Citations (3)
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| CN1172178C (en) * | 2001-02-16 | 2004-10-20 | 中国科学院长春应用化学研究所 | Method for testing quality of acanthopanax leaf |
| CN1857397A (en) * | 2006-04-05 | 2006-11-08 | 浙江大学 | Process of extracting flavonid from Haizhou elsholizia as copper polluted soil repairing plant |
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