CN101787010B - Method for extracting oligo proanthocyanidin from grape seeds - Google Patents
Method for extracting oligo proanthocyanidin from grape seeds Download PDFInfo
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Abstract
The invention provides a method for extracting oligo proanthocyanidin from grape seeds, which comprises the following steps: placing materials in extraction tanks, wherein the extraction solvent is water or water-containing ethanol, the using amount is 3-10 times of the volume of material mass, the temperature is 45-100 DEG C, and the time is 20-60 min; leading the content of active ingredients in extraction liquid in all the tanks to be gradually reduced by sequentially extracting the tanks, carrying out liquid discharge on the extraction liquid with the highest content of the active ingredients in all the tanks, entering into the circulating step, then carrying out residue discharge and material addition on the extraction tank which completes a plurality of times of solvent extraction of materials, adding a new solvent during the last extraction of the materials, then transferring by spacing one unit, carrying out a plurality of times of extraction and discharging liquid. The method can ensure that the materials and the solvents of all the extraction units can always keep the greater concentration difference of the active ingredients, accelerate the extraction rate, improve the concentration of the active ingredients of the final solvent and be characterized by saving the solvents, saving energy and the like under the premise of ensuring the higher extraction rate.
Description
Technical field
The invention belongs to effective ingredients in plant and extract the field, relate to the method for extracting effective components pycnogenols from Semen Vitis viniferae, particularly a kind of single jar of traditional extraction is improved to the pot group type countercurrent extraction, from Semen Vitis viniferae, extract the method for pycnogenols.
Background technology
Pycnogenols is to pass through C by (+)-catechin, (-)-l-Epicatechol and (-)-L-Epicatechin gallate
4-C
8Key or C
4-C
6The polyphenol substance of the different polymerization degree that key is formed by connecting extensively is present in the plants such as grape, blueberry, cherry, plum and Cortex Pini, and wherein Semen Vitis viniferae is the important source of pycnogenols.Pycnogenols (GPC) has strong antioxidant action, and the absorption of human body degree is high, can remove intravital radical and active oxygen, and prevention is owing to the arteriosclerosis that major cause causes that is oxidized to of low-density lipoprotein in the blood of human body (LDL).Also have the compelling physiological function of other, as pressure reduction effect with to myocardial protective effect, radiation resistance, antimicrobial, promote cell-proliferation activity, mutation and anticancer etc.
At present, the extracting mode that pycnogenols is commonly used has conventional solvent-extraction process, supercritical extraction method and microwave-assisted extraction method.It is solvent that conventional solvent-extraction process adopts water or aqueous ethanol, has the high shortcoming of big, the follow-up concentration process power consumption of solvent-oil ratio.Carbon dioxide upercritical fluid extraction method (like CN 1107110C) has the characteristics of product noresidue, environmental nonpollution.Because pycnogenols has must polarity, when adopting carbon dioxide upercritical fluid extraction, generally need to add a large amount of entrainment agents.Simultaneously, (27 ± 2MPa), the equipment input cost is high for the complicated pressure that also need be certain of this method equipment.It is short that microwave-assisted extraction method (like CN1102589C) has extraction time, the characteristics that thermo-efficiency is high, but have higher danger during microwave leakage, security is relatively poor.
Summary of the invention
The objective of the invention is to the deficiency to pycnogenols traditional extraction technique in the Semen Vitis viniferae, a kind of method of from Semen Vitis viniferae, extracting pycnogenols is provided, is a kind of dynamic jar of technological method of extracting pycnogenols of group countercurrent extraction that adopt.
The present invention realizes through following technical scheme:
(1) makes concentration gradient: put into extractor with the whole grain of material Semen Vitis viniferae or after pulverizing; To the extraction solvent of 3～10 times of amounts of first jar (A) adding material, be under 45～100 ℃ of conditions in temperature, extracted 20～60 minutes; After extracting end extracting solution is moved to next extractor; First jar (A) adds novel solvent all the time, and solvent shifts to next jar successively in all the other each extractors, and the effective constituent concentration of extracting solution in each jar is increased progressively successively;
(2) circulated in countercurrent is extracted: collect the highest extracting solution of effective constituent concentration in each jar; The extractor that the material that carries out three or four solvent extractions is belonged to carries out deslagging and adds new material; New material adds when the extraction solvent extracts for the last time, and novel solvent adds when material extracts for the last time, moves at a distance from an extractor afterwards; When the number of times that material is extracted when solvent is identical with the quantity of extractor; Merging is discharged and collected to solvent, survey total phenol content through sulfuric acid-Vanillin method survey procyanidin content and forint-Xiao Kafa, the extraction rate of transform is 60-95%.
The thing Semen Vitis viniferae is crushed to below 10 orders.Extract solvent and select water or aqueous ethanol for use, selecting water for use is that the extractor number is four jars (A, B, C, D) when extracting solvent, and promptly Semen Vitis viniferae need advance four extractions, and extracting temperature is 70～100 ℃; Selecting aqueous ethanol for use is that the extractor number is three jars (A, B, C) when extracting solvent, and promptly Semen Vitis viniferae need advance three extractions, and alcohol concn is 35-75% (volume percent), and extracting temperature is 45～75 ℃.The material equivalent of putting in each step, ethanol isoconcentration equal-volume, it is also all identical to extract temperature and time.
The present invention has guaranteed to keep bigger effective constituent concentration difference between Semen Vitis viniferae and the solvent in each extractor, increases and extracts impellent, accelerates extraction efficiency, improves final solvent effective constituent concentration; Solvent in each extractor is participated in the extraction to material in all jars, through circulation, greatly reduces the absolute dosage of solvent, reduces the energy consumption of follow-up solvent recuperation.Compare with traditional thermal backflow extracting technology, this method has been kept higher extraction yield, and the solvent-oil ratio of unit material has reduced 44～75%, and extraction time has saved 25～33%.Therefore, use this method to extract that pycnogenols can not only guarantee higher extraction efficiency in Semen Vitis viniferae, and save greatly and extract solvent, reduce the spissated energy consumption of subsequent evaporation, be worth in industrial production, applying.
The present invention changes single jar of extraction of Semen Vitis viniferae into the pot group type countercurrent extraction; Repeatedly apply mechanically and move at each extractor through extracting solvent; Remain bigger concentration difference between material and extraction solvent, increase the velocity of diffusion of effective constituent in extracting solvent greatly, thereby accelerate extraction rate.Present method pycnogenols extraction yield is high, extraction time is short, it is few to extract solvent-oil ratio, and the energy consumption concentrated, treating process in later stage reduces greatly.The present invention makes water or alcohol-water for extracting solvent, can use existing organic solvent extractionprocess or Amberlyst process that pycnogenols is carried out follow-up refining purifying.Dynamically the application of jar group countercurrent extraction method is tending towards extensively, as from giant knotweed, extracting Schuttgelb, from Radix Glycyrrhizae, extracts Potenlini, chlorogenic acid extracting etc. from Japanese Honeysuckle.
Description of drawings
Fig. 1 is a three-effect counter flow extraction process schema.
Fig. 2 is a four-effect countercurrent extraction extraction process schema.
The practical implementation method
The present invention combines embodiment and accompanying drawing to be further described.
Embodiment one
Extraction using alcohol takes by weighing a certain amount of 10～40 order Semen Vitis viniferaes that are crushed to and puts into the A jar and add 6～10 times of amount 35～75% ethanol, and extracting temperature is 45～75 ℃, and extraction time is 30～60min.Operate (referring to Fig. 1) according to the following steps; (left side 1-5 is corresponding with the following step 1-5 among the figure); The material equivalent of putting in each step, ethanol isoconcentration equal-volume, it is also all identical to extract temperature and time; Survey procyanidin content and forint-Xiao Kafa survey total phenol content (down together) through sulfuric acid-Vanillin method, the extraction rate of transform is 60-95%.(left side 1-5 is corresponding with the following step 1-5 respectively among Fig. 1)
Step 1, in A, B, C jar, drop into a certain amount of Semen Vitis viniferae; The A jar adds novel solvent, under the temperature of setting, extracts, and extraction is got to the B jar to extracting solution after accomplishing;
Add novel solvent in step 2, the A jar, under the temperature of setting, extract simultaneously with the B jar; Extract and accomplish, the extracting solution of B jar is got to the C jar, and the extracting solution of A jar is got to the B jar;
Add novel solvent in step 3, the A jar, A, B, C extract under the temperature of setting simultaneously; Extract and accomplish, collect the extracting solution of C jar, the extracting solution of A jar is got to the C jar, the A jar is carried out deslagging and adds new material, the extracting solution of B jar is got to the A jar;
Add novel solvent in step 4, the B jar, A, B, C extract under the temperature of setting simultaneously; Extract and accomplish, collect the extracting solution of A jar, the extracting solution of B jar is got to the A jar, the B jar is carried out deslagging and adds new material, the extracting solution of C jar is got to the B jar;
Add novel solvent in step 5, the C jar, A, B, C extract under the temperature of setting simultaneously; Extract and accomplish, collect the extracting solution of B jar, the extracting solution of C jar is got to the B jar, the C jar is carried out deslagging and adds new material, the extracting solution of A jar is got to the C jar;
Step afterwards gets final product from step 3 beginning cyclical operation.
Embodiment two
Water extraction takes by weighing a certain amount of whole grain Semen Vitis viniferae and puts into the A jar and add 3～6 times of water gagings, and extracting temperature is 70-100 ℃, and extraction time is 30-60min.Operate (referring to Fig. 2) according to the following steps, the material equivalent of putting in each step, the water equal-volume, it is all identical to extract temperature and time, and the extraction rate of transform is 60-85%.(left side 1-7 is corresponding with the following step 1-7 respectively among Fig. 2)
Step 1, in A, B, C, D jar, drop into a certain amount of Semen Vitis viniferae; The A jar adds novel solvent, under the temperature of setting, extracts, and extraction is got to the B jar to extracting solution after accomplishing;
Add novel solvent in step 2, the A jar, under the temperature of setting, extract simultaneously with the B jar; Extract and accomplish, the extracting solution of B jar is got to the C jar, and the extracting solution of A jar is got to the B jar;
Add novel solvent in step 3, the A jar, A, B, C extract under the temperature of setting simultaneously; Extract and accomplish, the extracting solution of C jar is got to the D jar, and the extracting solution of B jar is got to the C jar, and the extracting solution of A jar is got to the B jar;
Add novel solvent in step 4, the A jar, A, B, C, D extract under the temperature of setting simultaneously; Extract and accomplish, collect the extracting solution of D jar; The extracting solution of B jar is got to the D jar, and the extracting solution of A jar is got to interim container for storing liquid, and the A jar is carried out deslagging and the new material of valency, and the extracting solution of C jar is got to the A jar, and the extracting solution of interim container for storing liquid is got to the C jar;
Step 5, B jar add novel solvent, and A, B, C, D extract under the temperature of setting simultaneously; Extract and accomplish, collect the extracting solution of A jar; The extracting solution of C jar is got to the A jar, and the extracting solution of B jar is got to interim container for storing liquid, and the B jar is carried out deslagging and new material, and the extracting solution of D jar is got to the B jar, and the extracting solution of interim container for storing liquid is got to the D jar;
Step 6, C jar add novel solvent, and A, B, C, D extract under the temperature of setting simultaneously; Extract and accomplish, collect the extracting solution of B jar; The extracting solution of D jar is got to the B jar, and the extracting solution of C jar is got to interim container for storing liquid, and the C jar is carried out deslagging and Jia Xin material, and the extracting solution of A jar is got to the C jar, and the extracting solution of interim container for storing liquid is got to the A jar;
Step 7, D jar add novel solvent, and A, B, C, D extract under the temperature of setting simultaneously; Extract and accomplish, collect the extracting solution of C jar; The extracting solution of A jar is got to the C jar, and the extracting solution of D jar is got to interim container for storing liquid, and the D jar is carried out deslagging and Jia Xin material, and the extracting solution of B jar is got to the D jar, and the extracting solution of interim container for storing liquid is got to the B jar;
Step afterwards gets final product since 4 step cyclical operations.
Embodiment three
It is some part accurately to take by weighing 20 order Semen Vitis viniferaes, and every part of 20g, solid-liquid ratio are that (g: ml), extracting solvent was 35～75% ethanol, each 30 minutes extraction times in 1: 3～1: 10.The design orthogonal test, level of factor extracts from 1-5 by the operation steps of embodiment one referring to table 1.After extracting end, the extracting solution of combining step 3,4,5 is measured volume, the content of sampling analysis pycnogenols.The result is referring to table 2.Preferred specific embodiments is interpreted as only illustrating, but not limits scope of the present invention by any way.
Table 1 level of factor table
Table 2 orthogonal experiments
Embodiment four
Embodiment two is compared traditional water formulation condition with traditional water extraction technology: extract 100 ℃ of temperature, solid-liquid ratio (g: ml) 1: 6, extracted 4 times, each 1 hour; Experimental result is as shown in table 3:
The comparison of table 3 Different Extraction Method
Compare with traditional extraction technique, use during for solvent this method to extract the pycnogenols in Semen Vitis viniferae with water, extraction yield slightly improves, and extraction time reduces 33%, and the solvent-oil ratio of unit material reduces 75%.It is thus clear that the sharpest edges of using this method to extract the pycnogenols in the Semen Vitis viniferae are to guarantee under the prerequisite of higher extraction efficiency, not only shorten extraction time but also save the extraction solvent greatly, reduce the spissated energy consumption of subsequent evaporation.
Embodiment five
Embodiment one is compared alcohol heat reflux method processing condition with conventional alcohol heat reflux extraction method: extract 85 ℃ of temperature, alcohol concn 75%, solid-liquid ratio (g: ml) 1: 6, extract three times, each 40min.Experimental result is as shown in table 4:
The comparison of table 4 Different Extraction Method
Compare with the alcohol heat reflux extraction method of routine; 55% ethanol uses during for solvent this method to extract the pycnogenols in Semen Vitis viniferae; Though extraction yield slightly reduces; But amount of ethanol minimizing 26.7%, the solvent-oil ratio minimizing 44% of extracting 10 ℃ of temperature reductions, extraction time shortening 25%, unit material, so amount of ethanol is merely about 1/10 of routine.It is thus clear that the sharpest edges of using this method to extract the pycnogenols in the Semen Vitis viniferae are to guarantee under the prerequisite of higher extraction efficiency, not only reduce and extract temperature and reduce extraction time but also save amount of ethanol greatly, and reduce the spissated energy consumption of subsequent evaporation.
Claims (5)
1. a method of from Semen Vitis viniferae, extracting pycnogenols is characterized in that, realizes through following steps:
(1) makes concentration gradient: put into extractor with the whole grain of material Semen Vitis viniferae or after pulverizing; Select for use water or aqueous ethanol for extracting solvent; To extracting the extraction solvent that first extractor adds 3～10 times of amounts of weight of material, temperature is 45～100 ℃ earlier, and extraction time is 20～60 minutes; After extracting end extracting solution is moved to next extractor; First extractor adds novel solvent all the time, and solvent shifts to next jar successively in all the other each extractors, and the effective constituent concentration of extracting solution in each extractor is increased progressively successively;
(2) circulated in countercurrent is extracted: collect the highest extracting solution of effective constituent concentration in each extractor; The extractor that the material that carries out three or four solvent extractions is belonged to carries out deslagging and adds new material; New material adds when the extraction solvent extracts for the last time; Novel solvent adds when material extracts for the last time, moves at a distance from an extractor afterwards, when the number of times that material is extracted when solvent is identical with the quantity of extractor; Merging is discharged and collected to solvent, survey procyanidin content and survey total phenol content with forint-Xiao Kafa with sulfuric acid-Vanillin method.
2. a kind of method of from Semen Vitis viniferae, extracting pycnogenols according to claim 1 is characterized in that, when being that extractor group number is four jars when extracting solvent with water, extracting temperature is 70～100 ℃.
3. a kind of method of from Semen Vitis viniferae, extracting pycnogenols according to claim 1 is characterized in that, when being that alcohol concn is 35-75% when extracting solvent with the aqueous ethanol, extractor group number is three jars, and extracting temperature is 45～75 ℃.
4. a kind of method of from Semen Vitis viniferae, extracting pycnogenols according to claim 1 is characterized in that Semen Vitis viniferae is crushed to below 10 orders.
5. a kind of method of from Semen Vitis viniferae, extracting pycnogenols according to claim 1 is characterized in that, the material equivalent of putting in each step, and the concentration of said aqueous ethanol is identical with volume, and it is also all identical to extract temperature and time.
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| CN102807546A (en) * | 2012-08-06 | 2012-12-05 | 宁波杰顺生物科技有限公司 | Method for extracting anthocyanin in blackcurrant fruits |
| CN103223261B (en) * | 2013-04-22 | 2014-12-31 | 华南理工大学 | Apparatus and method for pulsed electric field-assisted countercurrent extraction of grape skin residue polyphenol |
| CN104496957A (en) * | 2014-12-01 | 2015-04-08 | 成都红柿子科技有限公司 | Method for extracting procyanidine from grape skins |
| CN105693678B (en) * | 2016-01-15 | 2018-09-14 | 甘肃寿鹿山药业有限公司 | The method of extracting proanthocyanidin from grape seeds |
| CN106858554A (en) * | 2017-01-05 | 2017-06-20 | 东北农业大学 | A kind of method that antioxidant is extracted in aqueous enzymatic method residue of grape seeds |
| CN108191805A (en) * | 2018-03-06 | 2018-06-22 | 云南华测检测认证有限公司 | A kind of method that natural procyanidins are extracted in the rose from polyphyll |
| CN113480514B (en) * | 2021-08-16 | 2022-07-22 | 内蒙古泓兴生物科技有限公司 | Method for extracting sesamin |
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| CN1193995C (en) * | 2003-05-30 | 2005-03-23 | 中国科学院新疆理化技术研究所 | Method of extracting oligo proanthocyanidin of grape seed |
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