CN105481914A - Method for extracting tannin in grape seeds - Google Patents
Method for extracting tannin in grape seeds Download PDFInfo
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- C07H13/00—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids
- C07H13/02—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids by carboxylic acids
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Abstract
The invention discloses a method for extracting tannin in grape seeds. The extraction method includes the following steps that 1, degreased grape seed meal is subjected to smashing, sieving, extraction and suction filtration to obtain filtrate and filtration residues for standby application; 2, the filtrate obtained in step 1 is subjected to reduced-pressure concentration and vacuum drying to obtain a crude tannin product. According to the method, the conditions of a process for extracting the tannin in the grape seeds are optimized and researched by adopting an organic solvent extraction method, the influences of the material-liquid ratio, ethyl alcohol volume fraction, extraction time and extraction temperature on the extraction rate of the tannin in the grape seeds are investigated, and by the adoption of the analysis on the results of single factor experiments and response surface optimization experiments, the best extraction conditions of the tannin in the grape seeds are obtained as follows: the ethyl alcohol volume fraction is 51.70%, the extraction time is 3.08 hours, the extraction temperature is 61.87 DEG C, and the tannin extraction rate under the conditions is as high as 6.36%.
Description
Technical field
The present invention relates to the extracting method of tannin in a kind of Semen Vitis viniferae.
Background technology
Grape (grapes) is the defoliation liana of Vitaceae (Vitaceae) Vitis (Vitis).Fruit can be made into the products such as Sucus Vitis viniferae, raisin and grape wine, along with the turnout of grape product is increasing, waste such as Pericarpium Vitis viniferae, Semen Vitis viniferae, the grape dregs etc. produced in the course of processing is urgently fully utilized.
About research shows in grape waste containing the abundant material such as raisin seed oil, protein, tannin, trans-resveratrol, its protein content is high, amino acid classes is very complete, mineral substance enriches, all very important to the needs meeting human body, and these materials are also widely used in industries such as medicine, healthcare products, makeup, so how by these Semen Vitis viniferae wastes comprehensive development and utilization in addition, turn waste into wealth of far-reaching significance.If properly handled, not only can alleviate the pollution that brings to environment but also can create huge economic benefit, thus can reach the effect of doulbe-sides' victory.
Tannin is the water-soluble polyphenols class material be extensively present in many plants, it is a kind of extremely strong activity in vivo functional factor, much research shows, due to the polyphenol hydroxyl structure of himself, tannin has stronger resistance of oxidation and good pharmacologically active, has now been widely used in the fields such as food, healthcare products, leather production, printing and dyeing industry, medicine and makeup.But due to the complex structure of tannin, synthetic is more difficult, now both at home and abroad main from natural phant as extracted Turkey-galls, and because natural resource limited, the price that result in domestic and international market tannin is very expensive.In addition, the output of China's grape and cultivated area all occupy first place, the world, and grape is being squeezed the juice and in wine brewing process, a large amount of by products can be produced, as Semen Vitis viniferae, Pericarpium Vitis viniferae etc., tanning matter content and abundant in Semen Vitis viniferae, and some peculiar tannin also have effect of preventing cardiovascular disease.At present, from Semen Vitis viniferae, extract tannin at home there is very large potentiality to be exploited, but the domestic research to tannin extraction is less.Therefore probe into the Optimization Technology extracting tannin from Semen Vitis viniferae and have very important practical significance.
The application's application Responds Surface Methodology is optimized research to the extraction process of tannin in Semen Vitis viniferae, adopt polynary quadratic regression equation as the instrument of Function Estimation, level line and surface model is set up in conjunction with mathematics and statistics, make the extraction rate reached of tannin in Semen Vitis viniferae to the highest, the comprehensive development and utilization for Semen Vitis viniferae provides certain scientific basis.
Summary of the invention
For Problems existing in background technology, the object of the present invention is to provide the extracting method of tannin in a kind of Semen Vitis viniferae, the application to be optimized the condition of tannin extraction process in Semen Vitis viniferae by organic solvent extraction and to probe into, investigate solid-liquid ratio, volume fraction of ethanol, extraction time and Extracting temperature are on the impact of tannin extraction yield in Semen Vitis viniferae, by the interpretation of result that experiment of single factor and response surface optimization are tested, show that in best Semen Vitis viniferae, tannin extraction conditions is: the volume fraction of ethanol is 51.70%, extraction time is 3.08h, Extracting temperature is 61.87, under this condition, the extraction yield of tannin is up to 6.36%.
The object of the invention is to be achieved through the following technical solutions:
An extracting method for tannin in Semen Vitis viniferae, described extracting method comprises the steps:
1) the defatted grape seed dregs of rice carried out pulverize, sieve, lixiviate, suction filtration obtains filtrate and filter residue is for subsequent use;
2) filtrate in step 1) is carried out concentrating under reduced pressure, vacuum-drying obtains tannin crude product.
Further, the pulverizing in described step 1), sieving is specially: get the appropriate defatted grape seed dregs of rice, pulverize with high-speed multifunctional pulverizer, then use 60 object sieve for subsequent use.
Further, the extracting solution of the lixiviate in described step 1) is ethanol, and the volume fraction of described ethanol is 30-70%, and the Semen Vitis viniferae dregs of rice after sieving and the solid-liquid ratio of described ethanol are: 1:40-1:80, and extraction time is 2-4h, and Extracting temperature is 40-80 DEG C.
Further, the extracting solution of the lixiviate in described step 1) is ethanol, and the volume fraction of described ethanol is 51.70%, and the Semen Vitis viniferae dregs of rice after sieving and the solid-liquid ratio of described ethanol are: 1:60, and extraction time is 3.08h, and Extracting temperature is 61.87 DEG C.
The present invention has following positive technique effect:
The application to be optimized the condition of tannin extraction process in Semen Vitis viniferae by organic solvent extraction and to probe into, investigate the impact on tannin extraction yield in Semen Vitis viniferae of solid-liquid ratio, volume fraction of ethanol, extraction time and Extracting temperature, by the interpretation of result that experiment of single factor and response surface optimization are tested, show that in best Semen Vitis viniferae, tannin extraction conditions is: the volume fraction of ethanol is 51.70%, extraction time is 3.08h, Extracting temperature is 61.87, and under this condition, the extraction yield of tannin is up to 6.36%.
Accompanying drawing explanation
Fig. 1 is that the volume fraction of extraction agent ethanol is on the impact of tannin extraction yield;
Fig. 2 is the impact of different feed liquid comparison tannin extraction yield;
Fig. 3 is the impact of different Extracting temperature on tannin extraction yield;
Fig. 4 is that different extraction time is on the impact of tannin extraction yield;
Fig. 5 be ethanol volume fraction and extraction time interaction on the impact (isogram) of tannin extraction yield;
Fig. 6 be ethanol volume fraction and extraction time interaction on the impact (response surface 3D schemes) of tannin extraction yield;
Fig. 7 is that the volume fraction of ethanol and Extracting temperature interaction are on the impact (isogram) of tannin extraction yield;
Fig. 8 is that the volume fraction of ethanol and Extracting temperature interaction are on the impact (3D surface chart) of tannin extraction yield;
Fig. 9 is that extraction time and Extracting temperature are on the impact (isogram) of tannin extraction yield;
Figure 10 is that extraction time and Extracting temperature are on the impact (3D surface chart) of tannin extraction yield.
Embodiment
Below, with reference to accompanying drawing, more fully illustrate the present invention, accompanying drawing acceptance of the bid shows exemplary embodiment of the present invention.But the present invention can be presented as multiple multi-form, and should not be construed as the exemplary embodiment being confined to describe here.But, these embodiments are provided, thus make the present invention comprehensively with complete, and scope of the present invention is fully conveyed to those of ordinary skill in the art.
This application provides the extracting method of tannin in a kind of Semen Vitis viniferae, this extracting method comprises the steps: 1) the defatted grape seed dregs of rice carried out pulverize, sieve, lixiviate, suction filtration obtains filtrate and filter residue is for subsequent use; 2) filtrate in step 1) is carried out concentrating under reduced pressure, vacuum-drying obtains tannin crude product.Wherein, pulverize, sieving is specially: get the appropriate defatted grape seed dregs of rice, pulverize with high-speed multifunctional pulverizer, then use 60 object sieve for subsequent use.
The volume fraction of extraction agent ethanol is on the impact of tannin extraction yield:
Get 21 triangular flasks, be divided into 7 groups, often group 3 is parallel, adds the pretreated raw material of 1g wherein, to often organizing in triangular flask the ethanol 30mL adding 30%, 40%, 50%, 60%, 70%, 80%, 90% respectively, be put in lixiviate 3h in the thermostat water bath of 60 DEG C with after preservative film sealing.Use Büchner funnel vacuum filtration after taking out, filtrate is moved in centrifuge tube, the centrifugal 30min of 3000r/min.From each sample liquid, draw 1mL supernatant liquor, be placed in the 50mL volumetric flask filling 30mL distilled water, add 2.5mLF-D reagent, then add 5mL saturated sodium carbonate solution, be diluted with water to 50mL.Shake up and make it fully mix, and survey its light absorption value at 650nm place after 30min.
The impact of different feed liquid comparison tannin extraction yield
Get 21 triangular flasks, be divided into 7 groups, often group 3 is parallel, adds the pretreated raw material of 1g wherein, to often organizing in triangular flask ethanol 20mL, 30mL, 40mL, 50mL, 60mL, 70mL, 80mL of adding 50%, be put in lixiviate 3h in the thermostat water bath of 60 DEG C with after preservative film sealing.Use Büchner funnel vacuum filtration after taking out, filtrate is moved in centrifuge tube, the centrifugal 30min of 3000r/min.From each sample liquid, draw 2mL supernatant liquor, be placed in the 50mL volumetric flask filling 30mL distilled water, add 2.5mLF-D reagent, then add 5mL saturated sodium carbonate solution, be diluted with water to 50mL.Shake up and make it fully mix, and survey its light absorption value at 650nm place after 30min.
Different Extracting temperature is on the impact of tannin extraction yield
Get 21 triangular flasks, be divided into 7 groups, often group 3 is parallel, add the pretreated raw material of 1g wherein, to often organizing in triangular flask the ethanol 30mL adding 50% respectively, be put in lixiviate 3h in the thermostat water bath of 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C respectively with after preservative film sealing.Use Büchner funnel vacuum filtration after taking out, filtrate is moved in centrifuge tube, the centrifugal 30min of 3000r/min.Be draw 1mL supernatant liquor the sample liquid of 60 DEG C from Extracting temperature, remaining is often organized and all draws 2mL supernatant liquor, is placed in the 50mL volumetric flask filling 30mL distilled water, adds 2.5mLF-D reagent, then add 5mL saturated sodium carbonate solution, be diluted with water to 50mL.Shake up and make it fully mix, and survey its light absorption value at 650nm place after 30min.
Different extraction time is on the impact of tannin extraction yield
Get 15 triangular flasks, be divided into 5 groups, often group 3 is parallel, adds the pretreated raw material of 1g wherein, to often organizing in triangular flask the ethanol 30mL adding 50% respectively, with being put in difference lixiviate 1h, 2h, 3h, 4h, 5h in the thermostat water bath of 60 DEG C after preservative film sealing.Use Büchner funnel vacuum filtration after taking out, filtrate is moved in centrifuge tube, the centrifugal 30min of 3000r/min.From each sample liquid, draw 2mL supernatant liquor, be placed in the 50mL volumetric flask filling 30mL distilled water, add 2.5mLF-D reagent, then add 5mL saturated sodium carbonate solution, be diluted with water to 50mL.Shake up and make it fully mix, and survey its light absorption value at 650nm place after 30min.
According to Box-Behnken central. set and experimental design principles, the experimental result that comprehensive single factor test affects tannin extraction yield, choose 3 more excellent levels of solid-liquid ratio, extraction time and Extracting temperature 3 factors, single factor experiment basis adopt the Responds Surface Methodology of 3 factor 3 levels carry out experimental design, draw mathematical model, analyze the interaction between each factor, and the relation between each factor and response value.Empirical factor and level are in table 1.
Table 1 tannin extraction process response surface empirical factor and level
As shown in Figure 1, be extraction agent with aqueous ethanolic solution, the tannin of different ratios to Semen Vitis viniferae arranging ethanol and water extracts, and compares the size of light absorption value.Typical curve according to drawing searches tannin concentration corresponding to measured light absorption value, calculates tannin content and extraction yield; As shown in Figure 1, the volume fraction of ethanol is the strongest to the dissolving power of tannin about 50% time, and when ratio raises or declines, extraction yield declines to some extent, and this is relevant with the physico-chemical property of ethanol with the complex construction of tannin.There is correlative study to show, add a little water higher than the extracted amount of straight alcohol solution to tannin, namely can promote the dissolving of combined tannin, the degraded of tannin in long-time heat preservation leaching process and rotten can be reduced again.
As shown in Figure 2, get the aqueous ethanolic solution that 1g raw material correspondence adds different volumes, the tannin of different solid-liquid ratios to Semen Vitis viniferae is set and extracts, calculate the tannin extraction yield of different feed liquid ratio.The tannin concentration that light absorption value measured by calculating according to the typical curve drawn is corresponding, and calculate tannin content and extraction yield; Can obviously be found out by Fig. 2, the extraction yield of tannin increases along with the increase of extraction agent volume, reaches maximum value when solid-liquid ratio is about 1:60, afterwards along with extraction agent volume increases the extraction yield change of tannin not quite, substantially tends towards stability.Because excessive solid-liquid ratio not only can cause the wasting of resources, but also give suction filtration, the follow-up work such as centrifugal, dry brings larger difficulty.So select 1:60 as the best solid-liquid ratio extracting tannin.
As shown in Figure 3, set according to the Suitable ranges that tannin extracts the comparison that 7 graded levels carry out tannin extraction yield in Semen Vitis viniferae, calculate the extraction yield of tannin under different Extracting temperature.The tannin concentration that light absorption value measured by calculating according to the typical curve drawn is corresponding, and calculate tannin content and extraction yield, can obviously be found out by Fig. 3, along with the increase of Extracting temperature, in Semen Vitis viniferae, tannin extraction yield also increases to some extent, when 60 DEG C, the extraction yield of tannin is the highest, and when temperature continues to increase, the extraction yield of tannin reduces gradually.This be due to temperature lower time, increasing of temperature can promote the dissolving of tannin in aqueous ethanolic solution, make extract tannin content increase gradually.But the chemical reactions such as tannin is easily degraded at an excessive temperature, condensation, oxidation, cause tannin extraction yield to decline.
As shown in Figure 4, the comparison of tannin extraction yield in Semen Vitis viniferae is carried out according to suitable time range set 5 levels of tannin extraction in related data, the light absorption value of sample liquid under more different extraction time, tannin concentration corresponding to measured light absorption value is searched again according to the typical curve drawn, calculate tannin content and extraction yield, can obviously be found out by Fig. 4, the extraction yield of tannin increases with the increase of extraction time, lixiviate 3 hours tannin extraction rate reached maximum value, the extraction yield lengthening extraction time tannin can decrease.According to pertinent data display, long extracting at constant temperature makes the extraction yield of tannin have a little decline, may be caused by tannin complexes sex change.
On the basis of experiment of single factor, application Design-Expert.8.05b software, adopt Box-BehnkenDesign founding mathematical models, to choose volume fraction of ethanol (X1), extraction time (X2), Extracting temperature (X3) three factors for investigating object, with the mean value of tannin extraction yield (Y) for response value, the response surface of Three factors-levels is adopted to carry out experimental design, by the test-results of Box-BehnkenDesign design gained in table 2.
The experimental design of table 2 response surface optimization and response value
| Test number | X 1 | X 2 | X 3 | Y extraction yield/% |
| 1 | 40 | 3 | 70 | 4.3972 |
| 2 | 50 | 2 | 50 | 3.81812 |
| 3 | 60 | 4 | 60 | 4.52532 |
| 4 | 50 | 4 | 70 | 4.6471 |
| 5 | 60 | 3 | 50 | 4.19204 |
| 6 | 40 | 3 | 50 | 3.70035 |
| 7 | 50 | 3 | 60 | 6.3277 |
| 8 | 40 | 4 | 60 | 4.2249 |
| 9 | 50 | 3 | 60 | 6.24366 |
| 10 | 60 | 3 | 70 | 5.17134 |
| 11 | 50 | 3 | 60 | 5.94167 |
| 12 | 50 | 3 | 60 | 5.85613 |
| 13 | 60 | 2 | 60 | 4.395 |
| 14 | 50 | 4 | 50 | 4.02464 |
| 15 | 40 | 2 | 60 | 3.76136 |
| 16 | 50 | 3 | 60 | 6.14344 |
| 17 | 50 | 2 | 70 | 4.09485 |
After experimental result regression fit, obtain light absorption value to volume fraction of ethanol, extraction time and the polynary quadratic regression equation of extraction time:
Y=6.1+0.27X1+0.17X2+0.32X3-0.083X1X2+0.071X1X3+0.086X2X3-0.83X12-1.05X22-0.91X32
In formula: Y---tannin extraction yield
X1---volume fraction of ethanol
X2---extraction time
X3---extraction temperature
In order to check the reliability of regression equation, carry out variance analysis, analytical results is in table 3.
Table 3 analysis of variance table
| Source of variation | Sum of squares | Degree of freedom | All square | F value | P value |
| Regression model | 14.00 | 9 | 1.56 | 43.31 | <0.0001** |
| A | 0.60 | 1 | 0.60 | 16.84 | 0.0046** |
| B | 0.23 | 1 | 0.23 | 6.37 | 0.0396* |
| C | 0.83 | 1 | 0.83 | 23.08 | 0.0020** |
| AB | 0.028 | 1 | 0.028 | 0.77 | 0.4086 |
| AC | 0.020 | 1 | 0.020 | 0.56 | 0.4805 |
| BC | 0.030 | 1 | 0.030 | 0.83 | 0.3921 |
| A 2 | 2.89 | 1 | 2.89 | 80.42 | <0.0001 |
| B 2 | 4.62 | 1 | 4.62 | 128.58 | <0.0001 |
| C 2 | 3.48 | 1 | 3.48 | 96.81 | <0.0001 5 --> |
| Residual error | 0.25 | 7 | 0.036 | ||
| Lose and intend item | 0.093 | 3 | 0.031 | 0.78 | 0.5647 |
| Pure error | 0.16 | 4 | 0.040 | ||
| Total value | 14.25 | 16 |
Note: " * " is that significantly (p<0.05) " * * " is highly significant (p<0.01).
Lose as can be seen from Table 3 and intend item P=0.5647>0.05, show to lose plan not remarkable; The P<0.01 of regression model, shows model highly significant; The correction coefficient of determination (relation conefficient) R2Adj of model is 0.9597, illustrates that this model can reflect the change of 95.97% response value.Above 3 fitting degree all indicating this model are fine, and therefore this regression model can be used for analysis design mothod data and predicts optimum extraction condition more exactly.
Once the F value size of item reflects the influence degree situation of each factor to response value, and F value shows that more greatly the influence degree of this factor to response value is larger.As seen from Table 3, the influence degree order of each factor to tannin extraction yield is: extraction temperature > volume fraction of ethanol > extraction time.
As shown in Figure 5-10, response surface isogram and 3D figure can reflect the impact of each factor on tannin extraction yield intuitively, and the volume fraction of ethanol, interaction between extraction time and extraction temperature Three factors, optimal processing parameter can be found out more accurately.So on the basis of regression model the results of analysis of variance, utilize software Design-Expert8.05b to do extraction time, Extracting temperature, volume fraction of ethanol to the response surface of tannin extraction yield impact in Semen Vitis viniferae and isogram, result is as shown in Fig. 7 ~ Fig. 9.
Isogram in Fig. 5-10 and 3D surface chart reflect interaction between each factor intuitively on the impact of tannin extraction yield, namely when a factor is fixed wherein, two other factor interaction is on the impact of tannin extraction yield, and can find out optimal processing parameter.
Isocontour shape can reflect non-interaction action and interactive power, oval represents that two because have interaction, and then in contrast, and isocontour density degree is relevant with interactive significance for circle.In addition, the obliquity of 3D figure surface chart also can determine both influence degrees to response value, and obliquity is higher, and namely the gradient is steeper, illustrates that interaction between them is more remarkable.3 isogram ovalizes of the application, and isocontour density degree is similar, 3D surface chart obliquity, close to consistent, shows that the interaction of each factor has impact to tannin extraction yield, but the mutual experiment of each group is more or less the same to the influence power of tannin extraction yield.
The optimization of optimum process condition and checking:
(1) optimization of optimum parameter
Solve according to the regression equation of response phase method computing gained and seek its maximum of points.
Y=6.1+0.27X1+0.17X2+0.32X3-0.083X1X2+0.071X1X3+0.086X2X3-0.83X12-1.05X22-0.91X32
As X1=0.185, X2=0.088, X3=0.203, Y value is maximum, and namely to obtain best processing condition be thus the volume fraction of ethanol is 51.70%, and extraction time is 3.08h, and Extracting temperature is 61.87 DEG C, and with this understanding, the extraction yield of tannin is up to 6.36%.
(2) checking of top condition
The optimum process condition drawn is adopted to carry out proof test.Using the mean value of three parallel tests as experimental result, the tannin extraction yield obtained is 6.35% differ 0.01% with theoretical value, and relative error is 0.16%, and practical measurement value conforms to substantially with theoretical expectation values, therefore the extraction conditions reliable in parameters adopting response phase method to obtain, has practical value.
In sum, herein by organic solvent extraction the condition of tannin extraction process in Semen Vitis viniferae is optimized and probes into, investigate the impact on tannin extraction yield in Semen Vitis viniferae of solid-liquid ratio, volume fraction of ethanol, extraction time and Extracting temperature, by the interpretation of result that experiment of single factor and response surface optimization are tested, show that in best Semen Vitis viniferae, tannin extraction conditions is: the volume fraction of ethanol is 51.70%, extraction time is 3.08h, Extracting temperature is 61.87, and under this condition, the extraction yield of tannin is up to 6.36%.
Described just in order to the present invention is described above, be construed as the present invention and be not limited to above embodiment, meet the various variants of inventive concept all within protection scope of the present invention.
Claims (4)
1. the extracting method of tannin in Semen Vitis viniferae, it is characterized in that, described extracting method comprises the steps:
1) the defatted grape seed dregs of rice carried out pulverize, sieve, lixiviate, suction filtration obtains filtrate and filter residue is for subsequent use;
2) filtrate in step 1) is carried out concentrating under reduced pressure, vacuum-drying obtains tannin crude product.
2. the extracting method of tannin in Semen Vitis viniferae according to claim 1, it is characterized in that, pulverizing in described step 1), sieving is specially: get the appropriate defatted grape seed dregs of rice, pulverize with high-speed multifunctional pulverizer, then use 60 object sieve for subsequent use.
3. the extracting method of tannin in Semen Vitis viniferae according to claim 1, it is characterized in that, the extracting solution of the lixiviate in described step 1) is ethanol, the volume fraction of described ethanol is 30-70%, the Semen Vitis viniferae dregs of rice after sieving and the solid-liquid ratio of described ethanol are: 1:40-1:80, extraction time is 2-4h, and Extracting temperature is 40-80 DEG C.
4. the extracting method of tannin in Semen Vitis viniferae according to claim 3, it is characterized in that, the extracting solution of the lixiviate in described step 1) is ethanol, the volume fraction of described ethanol is 51.70%, the Semen Vitis viniferae dregs of rice after sieving and the solid-liquid ratio of described ethanol are: 1:60, extraction time is 3.08h, and Extracting temperature is 61.87 DEG C.
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| CN114052248A (en) * | 2021-10-16 | 2022-02-18 | 湖南粟园酒庄有限责任公司 | Comprehensive processing system and equipment for rough processing of grape seed tannin raw materials |
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