CN101797447B - Method for separating and purifying effective ingredients in natural product - Google Patents

Method for separating and purifying effective ingredients in natural product Download PDF

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Publication number
CN101797447B
CN101797447B CN2010101375251A CN201010137525A CN101797447B CN 101797447 B CN101797447 B CN 101797447B CN 2010101375251 A CN2010101375251 A CN 2010101375251A CN 201010137525 A CN201010137525 A CN 201010137525A CN 101797447 B CN101797447 B CN 101797447B
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China
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extraction
purification
natural
separation
active ingredient
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CN2010101375251A
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Chinese (zh)
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CN101797447A (en
Inventor
郭嘉
张虎极
罗晔
黄坤
池汝安
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武汉工程大学
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Abstract

The invention relates to a method for separating and purifying effective ingredients in a natural product. The method comprises the following steps: 1) extracting effective ingredients of the natural product; 2) removing impurities through membrane separation; and 3) purifying through adsorption. The beneficial effects of the invention are as follows: 1) the separation and purification technological processes are considered from an overall perspective, thus making up the defects of membrane separation in the aspect; 2) compared with the traditional 'water extraction and alcohol precipitation'method, the method of the invention uses water as solvent or adds a certain proportion of ethanol according to the characteristics of effective ingredients of the natural product; 3) compared with the ultra-low temperature freezing technology, the method does not adopt the ultra-low temperature state and is more convenient; and 4) compared with the supercritical or subcritical solvent extraction,continuous operation can be realized at room temperature without phase transition course, the technology is simple and is not harsh to devices, the extraction rate is higher, and the final product has high purity.

Description

The method of active ingredient in a kind of separation and the purification natural products
Technical field
The invention belongs to technical field of chemical separation, concrete relate to a kind of adopt film to separate to separate with the charcoal absorption purification technique and the purification natural products in the method for active ingredient.
Background technology
Content of effective is often lower in the natural products, and composition is complicated, and the natural product chemistry composition is the important source of finding new drug or pharmaceutically active lead compound, also is widely used in industries such as agricultural, industry, daily-use chemical industry, food.Therefore, the new method of active ingredient separation and purification, new technology and technology also grow up thereupon in the natural products.Publication number is that CN1919221 discloses and adopts traditional " water extract-alcohol precipitation " method to extract active ingredient in the crape myrtle section plant asia belltree root leaf and fruit, and processes the regular dosage form on any pharmacy, but recovery rate is lower, and purification degrees is not high.Publication number is that CN1969890 discloses the employing superfreeze and the immersing in liquid nitrogen low-temperature grinding is extracted active component from fresh plant medicinal material, animal drug and marine product; Can improve recovery rate; But the techniques for ultra-low temperature of using are complicated, require very high to equipment dependability.Publication number is that CN101406487 and publication number are that CN101642632 discloses the overcritical and subcritical fluid extraction technology of employing respectively, and the equipment of use is various and complicated, and operational factor is restive, also leakage warning device need be installed.Publication number is that CN101274156 discloses and on extraction kettle, installed ultrasound-enhanced device (comprising ultrasonic generator and transducing head) additional, makes technology and equipment all more complicated.
Membrane separation technique is that an emerging separating substances is purified and concentration technique.In recent years, along with the development of membrane separation technique, the parts of traditional production technology is replaced by membrane separation technique.Compare with traditional isolation technics, membrane separation technique has following characteristics: 1. continued operation does not at normal temperatures have phase transition process; 2. need not add other reagent in the process, have energy-conservation in the large-scale production and advantage environmental protection; 3. need not heat the especially suitable advantages such as heat-sensitive substance that add thermal lability.Adsorption separation technology also is a kind of isolation technics commonly used, is to utilize the difference of solid absorbent to absorption affinity between the different adsorbates, thereby specific material is adsorbed the purpose that reaches separation.Use macroporous absorbent resin, active carbon and molecular sieve etc. in the industry always, be mainly used in the separation and purification of water soluble compound.
Because the complicated component in the natural product extraction liquid; Obtain target component and lean on single membrane separation technique or adsorption separation technology often not reach requirement, thereby, other isolation technics must not no longer be utilized; Like the precipitation method, salting out method, extraction, crystallization and recrystallization etc.; Complex process particularly adds organic solvent and is difficult to handle, and cost is high.Publication number is that CN 1490066 proposes active ingredient method in a kind of extraction natural products that makes up overcritical titanium dioxide fluid extraction technology and molecular distillation technique; But as previously mentioned; The equipment that supercritical fluid extraction uses; Operational factor is restive, and molecular distillation equipment cost of investment especially is high, restive.
Summary of the invention
Problem to be solved by this invention is the method that active ingredient in a kind of separation and the purification natural products is provided to above-mentioned prior art, adopts the active ingredient purity of this method gained high, and the adsorbent utilization rate is high, and technology is simple, with low cost.
The present invention by the problem of the above-mentioned proposition of solution the employing solution be: a kind of separate and the purification natural products in the method for active ingredient, it is characterized in that may further comprise the steps:
1) active ingredient of natural product extracts: natural products is pulverized, utilized water bath reflux method, it extracts temperature is 80-90 ℃, extraction time 1-2 hour, and extraction time 3-4 time; Or to utilize Microwave Extraction method, process conditions be power 500-1000W, extract 60-80 ℃ of temperature, extraction time 5-10 minute, extraction time 1-3 time; Or utilize ultrasonic extraction, and extraction time 1-1.5 hour, extraction time 3-4 time;
2) membrane separation for removing impurities: target component is analyzed, selected suitable single or multiple PSPP diffusion barrier to separate removal of impurities, obtain the extract after the separation and purification according to molecular weight size;
3) adsorption and purification: the target component in the extract after adopting solid absorbent to above-mentioned process membrane separating and purifying optionally adsorbs, desorb, obtains the active ingredient of natural product of separation and purification.
Press such scheme, described natural products is vegetable Chinese herbal medicine material Chinese anise, the root of kudzu vine, smilax, the leaf of bamboo, ginkgo leaf, Chinese gall, konjaku, barrenwort, the Radix Astragali, radix bupleuri, the root of large-flowered skullcap, gynostemma pentaphylla, the tuber of dwarf lilyturf, plate party, water shield, rheum officinale, pseudo-ginseng, sweet wormwood, Huai Shan or matrimony vine.
Pressing such scheme, after the described natural products of step 1) is pulverized, is that the ethanolic solution of 20-80% mixes with distilled water or mass concentration again.
Press such scheme, described solid absorbent is active carbon, macroporous absorbent resin or molecular sieve.
Beneficial effect of the present invention is: 1) though membrane separation technique or adsorption separation technology existing utilization in the purification of natural products separately; But the present invention gives full play to both advantages; Synthetically optimize technological parameter, consider two technical process from the integral body of separating and purify.The membrane separation technique that adopts at present is to utilize molecular size that the extract of natural products is separated; Active ingredient that molecular size is close and impurity are difficult to effectively separated; Adsorption technology has stronger selectivity to property material, has remedied film and has been separated in deficiency in this respect.Contain big molecular impurity such as a large amount of starch, polysaccharide, thermal source in the extract of natural products,, occur the adsorbent duct clogging that causes owing to macromolecular substances again often if directly use adsorption technology to separate; 2) with traditional " water extract-alcohol precipitation " method relatively, this method is solvent with water, or according to the characteristic of active ingredient of natural product, if necessary, can add the ethanol of proper proportion; 3) compare with the superfreeze technology, do not need the realization of ultralow temperature state, easier; 4) compare with overcritical or subcritical solvent extraction, continued operation does not at normal temperatures have phase transition process, and technology is succinct, the harsh requirement of unmatchful equipment, and the recovery rate that reaches is higher, and the purity of end product is high.
The specific embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to following enforcement.
Embodiment 1:
The 15g Star Anise Fruit is mixed with 750mL distilled water (or mass concentration 30% ethanolic solution), utilize water bath reflux method in the time of 80 ℃, to extract the active ingredient shikimic acid in the Chinese anise, 1 hour extraction time, extraction time 3 times, suction filtration gets extract.Utilize membrane separation technique to carry out removal of impurities then, selecting for use and holding back relative molecular weight is that 10000 milipore filter carries out, and holds back and removes thermal source, polysaccharide, aqueous soluble protein matter etc., and can filter shikimic acid (relative molecular weight is 162).To the extract after the above-mentioned separation and purification, utilize active carbon as solid absorbent again, absorption shikimic acid wherein.The charcoal absorption shikimic acid is an exothermic process, and its operating temperature is 30 ℃.Utilize 30% ethanolic solution to carry out desorb to adsorbing saturated active carbon again, desorption effect reached 82.21%, the renewable use of active carbon after desorption efficiency can reach behind 96.34%, three adsorption-desorption desorption effect and reaches 90.12%, six adsorption-desorption.
Embodiment 2:
With 15g root of kudzu vine powder and 600mL mass concentration is 20% ethanolic solution pre-soaking 30 minutes; Utilize the Microwave Extraction method that wherein Puerarin is extracted, the process conditions of Microwave Extraction are power 1000W, extract 60 ℃ of temperature, 10 minutes extraction times, extraction time 1 time.Utilize membrane separation technique to carry out removal of impurities then, selecting for use and holding back relative molecular weight is that 10000 milipore filter carries out purifying, holds back and removes thermal source, polysaccharide, aqueous soluble protein matter etc., and can filter Puerarin (relative molecular weight 416.38).The general flavone of can purifying in the ultrafiltration gained trapped fluid.Utilize macroporous absorbent resin AB-8 as solid absorbent again, the Puerarin in the absorption filtered solution.Macroporous absorbent resin AB-8 absorption Puerarin is an exothermic process, and the selection operation temperature is 30 ℃.Utilizing mass concentration again is that 70% ethanolic solution carries out desorb to adsorbing saturated active carbon, and desorption effect reached 73.2% after desorption efficiency can reach behind 90.1%, three adsorption-desorption desorption effect and reaches 83.9%, six adsorption-desorption.Can regenerate to macroporous absorbent resin, reuse.
Embodiment 3:
With 15g smilax powder and 450mL mass concentration is that 80% ethanolic solution mixes the general flavone that utilizes in the Microwave Extraction method extraction smilax.The extraction process condition is power 600W, 80 ℃ of temperature of extraction, 5 minutes extraction times, twice of extraction time.At first utilize membrane separation technique to carry out removal of impurities, selecting molecular cut off for use is that 50000 milipore filter carries out purifying, holds back and removes macro-molecular protein, polysaccharide etc., and can filter general flavone.Again filter liquor is carried out the membrane separating and purifying second time, choosing and holding back relative molecular weight is 6000 milipore filter, removes aqueous solution salt and metal ion etc.Utilize macroporous absorbent resin AB-8 as solid absorbent the trapped fluid that obtains, the general flavone in the absorption filtered solution.Utilizing mass concentration again is that 90% ethanolic solution carries out desorb to adsorbing saturated resin, and desorption efficiency can reach 90.1%.
Embodiment 4:
10g bamboo leaf is mixed with 500mL distilled water, utilize ultrasonic extraction to extract the active ingredient flavones in the leaf of bamboo, 1.5 hours extraction times, extraction time 4 times, suction filtration gets extract.Utilize membrane separation technique to carry out removal of impurities then, selecting for use and holding back relative molecular weight is that 10000 milipore filter carries out, and holds back and removes thermal source, polysaccharide, aqueous soluble protein matter etc., and can filter flavone compound.The selection operation temperature is 25 ℃, utilizes active carbon as solid absorbent, the flavone compound in the absorption filtered solution.Utilize 20% ethanolic solution to carry out desorb to adsorbing saturated active carbon again, desorption effect reached 89.60%, the renewable use of active carbon after desorption efficiency can reach behind 98.15%, three adsorption-desorption desorption effect and reaches 92.47%, five adsorption-desorption.
Embodiment 5:
With 20g barrenwort and 700mL mass concentration is that 60% ethanolic solution mixes the general flavone that utilizes in the Microwave Extraction method extraction barrenwort.The extraction process condition is power 500W, 75 ℃ of temperature of extraction, 8 minutes extraction times, extraction time three times.At first utilize membrane separation technique to carry out removal of impurities, selecting molecular cut off for use is that 10000 milipore filter carries out purifying, holds back and removes macro-molecular protein, polysaccharide etc., and can filter general flavone.Again filter liquor is carried out the membrane separating and purifying second time, choosing and holding back relative molecular weight is 6000 milipore filter, removes aqueous solution salt and metal ion etc.Utilize macroporous absorbent resin AB-8 as solid absorbent the trapped fluid that obtains, the general flavone in the absorption filtered solution.Utilize 80% ethanolic solution to carry out desorb, general flavone extraction rate reached 84.5% again to adsorbing saturated resin.
Embodiment 6:
The 15g ginkgo leaf is mixed with 600mL distilled water, utilize water bath reflux method in the time of 85 ℃, to extract the active ingredient general flavone in the ginkgo leaf, 2 hours extraction times, extraction time 4 times, suction filtration gets extract.Utilize membrane separation technique to carry out removal of impurities then, selecting for use and holding back relative molecular weight is that 10000 milipore filter carries out, and holds back and removes thermal source, polysaccharide, aqueous soluble protein matter etc., and can filter general flavone.Utilize mesoporous molecular sieve as solid absorbent again, the general flavone in the absorption filtered solution.Utilize 25% ethanolic solution to carry out desorb to adsorbing saturated molecular sieve again, desorption efficiency can reach 97.16%, general flavone extraction rate reached 75.8%.

Claims (3)

  1. One kind separate and the purification natural products in the method for active ingredient, it is characterized in that may further comprise the steps:
    1) active ingredient of natural product extracts: natural products is pulverized, and then, is that the ethanolic solution of 20-80% mixes with distilled water or mass concentration again, utilizes water bath reflux method, and its extraction temperature is 80-90 ℃, extraction time 1-2 hour, and extraction time 3-4 time; Or to utilize Microwave Extraction method, process conditions be power 500-1000W, extract 60-80 ℃ of temperature, extraction time 5-10 minute, extraction time 1-3 time; Or utilize ultrasonic extraction, and extraction time 1-1.5 hour, extraction time 3-4 time;
    2) membrane separation for removing impurities: target component is analyzed, selected suitable single or multiple PSPP diffusion barrier to separate removal of impurities, obtain the extract after the separation and purification according to molecular weight size;
    3) adsorption and purification: the target component in the extract after adopting solid absorbent to above-mentioned process membrane separating and purifying optionally adsorbs, desorb, obtains the active ingredient of natural product of separation and purification.
  2. 2. by the method for active ingredient in described separation of claim 1 and the purification natural products, it is characterized in that described natural products is vegetable Chinese herbal medicine material Chinese anise, the root of kudzu vine, smilax, the leaf of bamboo, ginkgo leaf, Chinese gall, konjaku, barrenwort, the Radix Astragali, radix bupleuri, the root of large-flowered skullcap, gynostemma pentaphylla, the tuber of dwarf lilyturf, plate party, water shield, rheum officinale, pseudo-ginseng, sweet wormwood, Huai Shan or matrimony vine.
  3. 3. by the method for active ingredient in claim 1 or 2 described separation and the purification natural products, it is characterized in that described solid absorbent is active carbon, macroporous absorbent resin or molecular sieve.
CN2010101375251A 2010-03-30 2010-03-30 Method for separating and purifying effective ingredients in natural product CN101797447B (en)

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Families Citing this family (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103304677B (en) * 2013-01-31 2015-11-25 重庆大学 A kind of method of separation and purification Rhizoma amorphophalli glucomannan
CN103145550A (en) * 2013-03-27 2013-06-12 张达燕 Method of extracting shikimic acid from star anise
CN103610209B (en) * 2013-11-13 2015-02-18 湖南科技大学 Natural plant preservative taking rape seed cakes and folium ginkgo as raw materials as well as preparation method and application thereof
CN103550402B (en) * 2013-11-21 2016-02-10 哈药集团中药二厂 A kind of preparation method of Fructus Lycii extract
CN104096381B (en) * 2014-07-09 2017-05-17 郑州大学 Method for extracting effective components of natural products through mixing of ethyl alcohol and sub-critical fluid
CN104274721A (en) * 2014-09-23 2015-01-14 苏州市天灵中药饮片有限公司 Preparation method of cold heat clearing granules
CN105105161A (en) * 2015-08-26 2015-12-02 浙江舟富食品有限公司 Braised beef product containing carrots and preparation method of braised beef
CN105660980A (en) * 2016-04-27 2016-06-15 黄旗兵 Method for making preserves by utilizing broccoli stems
CN106316830B (en) * 2016-07-22 2018-09-14 西南民族大学 A method of the separating-purifying shikimic acid from ginkgo fallen leaves
CN106749314B (en) * 2016-12-05 2017-12-08 江苏康缘尤赛金生物科技有限公司 A kind of extracting method of ginkgolides
CN108707142A (en) * 2018-06-21 2018-10-26 湖南双晟科技信息咨询有限公司 A kind of Retreatment method of pueraria starch processing slag and effluent
CN109594342A (en) * 2018-12-04 2019-04-09 山东如意科技集团有限公司 A kind of antibacterial rapid-curing cutback child clothing fabric and its production technology
CN111072646A (en) * 2019-12-27 2020-04-28 四川省玉鑫药业有限公司 Method for refining puerarin

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