CN102703204A - Method for extracting semen cannabis oil - Google Patents
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Abstract
The invention relates to a method for extracting semen cannabis oil, and belongs to a processing technology for extraction of vegetable oil and fat. The method comprises the following steps of: crushing semen cannabis, and pulping to obtain a mixed solution; adding protease into the mixed solution to perform enzymolysis; and after performing the enzymolysis, killing enzyme, and performing centrifugal separation to obtain the high-quality oil. According to the method, the semen cannabis oil is separated by using a bio-enzyme method, and the high-quality oil can be obtained by demulsifying the separated emulsified oil without refining. The semen cannabis oil is high in nutritive value and high in utilization value of semen cannabis protein and peptides. According to the method, the total oil extraction rate is 93.18 percent, and required equipment is simple and safe in operation; and the semen cannabis oil does not have solvent residues, and is low in albuminous degeneration and high in extraction rate.
Description
Technical field
The invention belongs to Vegetable oil lipoprotein and extract processing technology, relate in particular to a kind of process for extracting of Hemp Seed oil.
Background technology
At present, a Hemp Seed oil preparation process mechanical expression method.Milling process is the oil that pushes out by physics, also has other deliquescent thing also can come out, the sense organ of influence oil; Squeeze processing for a long time through later stage high temperature, oil, cake are of poor quality, the residual oil content in the dregs of beans high (5%～7%, butt); Protein denaturation is serious in the dregs of beans, can only be used as fertilizer, and nutrition circle is at present found after deliberation, and the bioactive peptide in the Hemp Seed has very high nutritive value and reaches functionally active widely, is easy to after the squeezing be destroyed, and this method causes the proteic waste of a large amount of quality plants.And contain very high unsaturated fatty acids in the Hemp Seed grease, after the high temperature squeezing, distribution of fatty acids is also had very big influence.
Aqueous enzymatic method is to adopt biological enzyme hydrolysis oil plant raw material, and it is gentle to carry deep-fried twisted dough sticks spare, and the performance of oilseed protein changes hardly, no matter is the direct processing and utilization of aqueous phase, still reclaims protein isolates and utilizes, and effect is all very good.Just there is the scholar to be applied to grease to biotechnology (enzyme) to seek the more process for extracting of science, health, safety abroad in the fifties in last century.To the nineties in last century; Aqueous enzymatic method is proposed the concern that oil tech causes Chinese scholars once more; Because the aqueous enzymatic method technology not only can overcome conventional oil-producing technique in many-sided drawbacks such as economy, environment, safety, and in stripping oil, can effectively reclaim other nutritive substances in the oil plant.The research of aqueous enzymatic extraction progressively becomes the focus of current domestic and international foodstuffs industry, nearly 20 kinds of oil plants is tested so far, and the enzyme that research relates to has nearly ten kinds.Experiment shows; Aqueous enzymatic method oil-producing technique to multiple oil plant all can improve oil yield; Improve the quality and the by product quality of oil, the aqueous enzymatic extraction technology is to utilize oil plant to obtain the Perfected process of grease and albumen simultaneously, but the greasy research of the fiery pockmarks of aqueous enzymatic extraction still belongs to blank at present.
Summary of the invention
Technical problem to be solved by this invention is exactly the deficiency to above-mentioned prior art, and a kind of process for extracting of Hemp Seed oil is provided, and reaches and does not destroy nutritive ingredient in the grease, improves the purpose of grease yield.
Technical problem to be solved by this invention realizes by the following technical programs:
A kind of process for extracting of Hemp Seed oil, the process for extracting step is following: mix with water after Hemp Seed is pulverized (1), obtains mixed solution; Amount of water is the 15-35% of weight of material; Mixed solution is put into hollander pull an oar, the making beating frequency is 20-40hz, and beating time is 10-30min; (2) add proteolytic enzyme in the mixed solution after making beating and carry out enzymolysis, enzyme concentration is the 5000-9000u/g substrate of weight of material, obtains enzymolysis solution, and hydrolysis temperature is 50-70 ℃, and enzymolysis time is 2.5-4.5h, and enzymolysis pH value is 7.5-9.5; (3) enzymolysis solution that step (2) the is obtained spinning of going out behind the enzyme is handled, and it is oily promptly get Hemp Seed, and centrifugal rotational speed is 6500r/min, and centrifugation time is 25min.
The preferred parameter of said method is: amount of water is 22% of a weight of material.
Described making beating preferred parameter is: the making beating frequency is 30hz, and beating time is 20min.
Described enzymolysis preferred parameter is: 60 ℃ of hydrolysis temperatures, and enzymolysis time 3.7h, enzymolysis pH value is 8.0, enzyme concentration is the 7050u/g substrate of weight of material.
The inventive method is on the basis of Mechanical Crushing; Adopt the enzyme of ability degrading plant oil plant cell or have the enzyme of Degradation to act on oil plant complex bodys such as lipoprotein, LPS; Make grease be easy to from the oil plant solid, discharge; Utilize non-oil component (albumen and glucide) to the oil and the avidity difference of water, utilize profit proportion difference simultaneously and oil is separated with non-oil component.In the inventive method; Enzyme is except complex bodys such as the oil plant cell of degrading, decomposition lipoprotein, LPS; Can also destroy the lipoprotein membrane that is wrapped in oil droplets that oil plant forms in processes such as defibrination, reduce the stability of milk sap, thereby improve the free oil yield.The inventive method utilization is pulverized pre-treatment and is separated the Hemp Seed grease with the aqueous enzymatic method that enzyme combines; Devices needed is simple, operational safety, gained Hemp Seed oil no solvent residue; The oil in water emulsion that separation obtains need not refining and can obtain high-quality oil behind breakdown of emulsion, be of high nutritive value.Through checking and simultaneous test, total oily extraction yield can reach about 93.24% under enzymolysis process condition of the present invention.
Description of drawings
Fig. 1 overall process route
The kind of the different enzymes of Fig. 2 is to the influence of total oily extraction yield
Fig. 3 beating time is to the influence of total oily extraction yield
Fig. 4 influence of frequency of pulling an oar to total oily extraction yield
Fig. 5 quality of material mark is to the influence of total oily extraction yield
Fig. 6 enzyme concentration is to the influence of total oily extraction yield
Fig. 7 hydrolysis temperature is to the influence of total oily extraction yield
Fig. 8 enzymolysis time is to the influence of total oily extraction yield
Fig. 9 enzymolysis ph is to the influence of total oily extraction yield
Each enzymolysis parameter of Figure 10 is to the Dimension Reduction Analysis of total oily extraction yield
Mutual significantly the response surface analysis of each enzymolysis parameter of Figure 11 to total oily extraction yield
Specific embodiments
Further describe the present invention below in conjunction with specific embodiment:
A kind of process for extracting of Hemp Seed oil, the process for extracting step is following: mix with water after Hemp Seed is pulverized (1), obtains mixed solution; Amount of water is the 15-35% of weight of material; Mixed solution is put into hollander pull an oar, the making beating frequency is 20-40hz, and beating time is 10-30min; (2) add proteolytic enzyme in the mixed solution after making beating and carry out enzymolysis, enzyme concentration is the 5000-9000u/g substrate of weight of material, obtains enzymolysis solution, and hydrolysis temperature is 50-70 ℃, and enzymolysis time is 2.5-4.5h, and enzymolysis pH value is 7.5-9.5; (3) enzymolysis solution that step (2) the is obtained spinning of going out behind the enzyme is handled, and it is oily promptly get Hemp Seed, and centrifugal rotational speed is 6500r/min, and centrifugation time is 25min.
The preferred parameter of said method is: amount of water is 22% of a weight of material.
Described making beating preferred parameter is: the making beating frequency is 30hz, and beating time is 20min.
Described enzymolysis preferred parameter is: 60 ℃ of hydrolysis temperatures, and enzymolysis time 3.7h, enzymolysis pH value is 8.0, enzyme concentration is the 7050u/g substrate of weight of material.
The screening of embodiment 1 beating process condition optimum parameter
1 experimental technique
Technical process
Hemp Seed → clear up → pulverize → add water → making beating → adjusting pH value and the temperature → enzymolysis → enzyme that goes out → centrifugal → Hemp Seed oil
2 results and discussion
2.1 beating process list factor condition is to the influence of total oily extraction yield
2.1.1 beating time is to the influence of total oily extraction yield
At quality of material mark 25%, making beating frequency 30hz, enzymolysis time 3.5h, 60 ℃ of hydrolysis temperatures, enzymolysis pH are 8.5, and enzyme concentration 7000u/g under the centrifugal 30min condition of 4500r/min, investigates the influence of beating time to total oily extraction yield, and the result sees Fig. 3.Can find out that by Fig. 3 result beating time is significantly improved when the 15min, and when 20min, arrive mxm..Final beating time eigenwert is 20min.
2.1.2 the making beating frequency is to the influence of total oily extraction yield
At quality of material mark 25%, beating time 20min, enzymolysis time 3.5h, 60 ℃ of hydrolysis temperatures, enzymolysis pH are 8.5, and enzyme concentration 7000u/g under the centrifugal 30min condition of 4500r/min, investigates the influence of making beating frequency to total oily extraction yield, and the result sees Fig. 4.Can see that by Fig. 4 result the making beating frequency at the 30hz place, peak occurs.Final making beating frequecy characteristic value is 30hz.
2.1.3 the quality of material mark is to the influence of total oily extraction yield
At making beating frequency 30hz, beating time 20min, 60 ℃ of hydrolysis temperatures, enzymolysis time 3.5h, enzymolysis pH are 8.5, and enzyme concentration 7000u/g under the centrifugal 30min condition of 4500r/min, investigates the influence of quality of material mark to total oily extraction yield, and the result sees Fig. 5.Can find out that by Fig. 5 result the quality of material mark obviously increases greater than 15% total oily extraction yield, but work as the quality of material mark greater than 35%, total oily extraction yield is on a declining curve, so the quality of material mark is selected 15%-35% in the response surface test design below.
Test the screening experiment of 2 enzymolysis process condition optimum parameters
1 experimental technique
Technical process
Hemp Seed → clear up → pulverize → add water → making beating → adjusting pH value and the temperature → enzymolysis → enzyme that goes out → centrifugal → Hemp Seed oil
2 results and discussion
2.1 enzymolysis process list factor condition is to the influence of total oily extraction yield
2.1.1 the enzyme concentration of Sumizyme MP is to the influence of total oily extraction yield
At quality of material mark 25%, enzymolysis time 3.5h, 60 ℃ of hydrolysis temperatures, enzymolysis pH are 8.5, under the centrifugal 30min condition of 4500r/min, investigate the influence of enzyme concentration to total oily extraction yield, the result sees Fig. 6.By Fig. 6 result can find out when enzyme concentration during at 7000u/g total oily extraction yield increase significantly, so the enzyme concentration level is selected 5000-9000u/g in the response surface test design below.
2.1.2 hydrolysis temperature is to the influence of total oily extraction yield
At enzyme concentration 7000u/g, quality of material mark 25%, enzymolysis time 3.5h, enzymolysis pH are 8.5, under the centrifugal 30min condition of 4500r/min, investigate the influence of hydrolysis temperature to total oily extraction yield, the result sees Fig. 7.Can find out that by Fig. 7 result near hydrolysis temperature total oily extraction yield 60 ℃ has higher value to occur, because consider interaction, so hydrolysis temperature is chosen in 50-70 ℃ in the response surface test design below.
2.1.3 enzymolysis time is to the influence of total oily extraction yield
At enzyme concentration 7000u/g, quality of material mark 25%, 60 ℃ of hydrolysis temperatures, enzymolysis pH are 8.5, under the centrifugal 30min condition of 4500r/min, investigate the influence of enzymolysis time to total oily extraction yield, the result sees Fig. 8.Can find out that by Fig. 8 result enzymolysis time obviously increases greater than the total oily extraction yield of 2.5h, but work as enzymolysis time greater than 4.5h, total oily extraction yield does not have considerable change, so enzymolysis time is selected 25-4.5h in the response surface test design below.
2.1.4pH influence to total oily extraction yield
At enzyme concentration 7000u/g, 60 ℃ of hydrolysis temperatures, enzymolysis time 3.5h, quality of material mark 25% under the centrifugal 30min condition of 4500r/min, is investigated the influence of pH to total oily extraction yield, and the result sees Fig. 9.Can find out that by Fig. 9 result pH has higher value to occur near 8-9, so pH selects 7.5-9.5 in the response surface test design below.
2.2 the response surface optimum experimental reaction conditions of enzymolysis process
2.2.1 enzymolysis process is to the result that influences of total oil extracting rate
2.2.1.1 empirical factor level code table
On the basis of single factor research; Choosing enzyme concentration, hydrolysis temperature, enzymolysis time, material-water ratio and an enzymolysis pH5 factor is independent variable(s), is response value with total oily extraction yield, according to the center combination principle of design; The experiment of design response surface analysis, its level of factor coding schedule is seen table 2-1
Table 2-1 level code table
2.2.1.2 response surface EE and experimental result
This experimental applications response surface optimized method carries out process optimization.With x
1, x
2, x
3, x
4, x
5Being independent variable(s), is response value Y with total oily extraction yield
1Response surface experimental program and result see that table 2-2 experiment 1-26 is factorial experiment, and 27-36 is 10 center tests, in order to the estimating experiment error.
Table 2-2 response surface experimental program and experimental result
2.2.1.3 response surface interpretation
Carry out data analysis through statistical analysis software SAS9.1; The quadratic response face of foundation regression model is following: Y=-209.295+0.014546*X1+10.61604*X2+34.9075*X3-1.338417*X 4-324775*X5-2.558E-6*X1*X1+0.002784*X1*X5-0.066721*X2*X2-0.56375*X2*X3-0067121*X4*X4+052575*X4*X5 (2-1) regression analysis and The results of analysis of variance are seen table 2-3; Table 2-4 is seen in the response surface optimizing; Dimension Reduction Analysis is seen Figure 10, and significant mutually alternately response surface analysis is seen Figure 11.
Table 2-3 returns and The results of analysis of variance
2-3 can know that the linear relationship between equation dependent variable and the independent variable(s) is obvious by table, and this regression models is (p＜0.0001) significantly, and it is not remarkable to lose the plan item, and this model R
2=92.52%, R
2 Adj=82.55%, explain that this model and experimental fit are good, linear relationship is remarkable between independent variable(s) and the response value, and the theory that can be used for this reaction is inferred.Can obtain the factor contributions rate by the F check is: x
1＞x
2＞x
4X
3＞x
5＞, i.e. enzyme concentration＞enzymolysis time＞solid-liquid ratio＞hydrolysis temperature＞pH.
Application responds face optimizing analytical procedure is analyzed regression model, seeks the optimal response result and sees table 2-4, can know that by table 2-4 working as enzyme concentration is 7050u/g; Temperature is 60 ℃, and enzymolysis time is 3.7h, quality of material mark 22%; PH is 8, and response surface has optimum value 93.62 ± 0.5%
Table 2-4 response surface optimizing result
Can know the Dimension Reduction Analysis of total oily extraction yield by each enzymolysis parameter of Figure 10, total oily extraction yield increase with the increase of enzyme concentration, but the trend that the later stage increases is not obvious, continues to increase enzyme concentration and can increase production cost.Total oily extraction yield improves with the increase of hydrolysis temperature, but under higher temperature, oil extracting rate descends to some extent, because Sumizyme MP has the most suitable temperature.Total oily extraction yield increases with the increase of enzymolysis time, total oily extraction yield receives the influence of hydrolysis temperature little in more excellent scope.Total oily extraction yield increases to increase afterwards earlier with the quality of material fractional and reduces, and the increasing value occurs 22%.Total oily extraction yield changes little with enzymolysis pH value, total oily extraction yield receives the influence of hydrolysis temperature little in more excellent scope.
Can find out by Figure 11 analytical results: enzyme concentration (x
1) and enzymolysis pH value (x
5), hydrolysis temperature (x
2) and enzymolysis time (x
3), hydrolysis temperature (x
2) and enzymolysis pH value (x
5) and solid-liquid ratio (x
4) and enzymolysis pH value (x
5) interaction to the influence of total oily extraction yield.
Though it is it is minimum to the factor contributions rate of total oily extraction yield at pH value pH in the 7.5-9.5 scope that hence one can see that, bigger to total oily extraction yield influence with the interaction of other factors.
3 confirmatory experiments
Under the top condition that the response surface analysis method is tried to achieve, i.e. enzyme concentration 7050u/g, 60 ℃ of temperature, enzymolysis time 3.7h quality of material mark 22%, pH8 carries out 3 parallel laboratory tests, the MV 93.24% of 3 parallel laboratory tests of total oily extraction yield.Experimental value and regression equation predictor that response value is described are identical good.
Claims (4)
1. the process for extracting of Hemp Seed oil, its characteristic is following in the process for extracting step: (1) is pulverized the back with Hemp Seed and is mixed with water, obtain mixed solution; Amount of water is the 15-35% of weight of material; Mixed solution is put into hollander pull an oar, the making beating frequency is 20-40hz, and beating time is 10-30min; (2) add proteolytic enzyme in the mixed solution after making beating and carry out enzymolysis, enzyme concentration is the 5000-9000u/g substrate of weight of material, obtains enzymolysis solution, and hydrolysis temperature is 50-70 ℃, and enzymolysis time is 2.5-4.5h, and enzymolysis pH value is 7.5-9.5; (3) enzymolysis solution that step (2) the is obtained spinning of going out behind the enzyme is handled, and it is oily promptly get Hemp Seed, and centrifugal rotational speed is 6500r/min, and centrifugation time is 25min.
2. the process for extracting of a kind of Hemp Seed oil according to claim 1, it is characterized in that the preferred parameter of said method is: amount of water is 22% of a weight of material.
3. the process for extracting of a kind of Hemp Seed oil according to claim 1, it is characterized in that described making beating preferred parameter is: the making beating frequency is 30hz, and beating time is 20min.
4. the process for extracting of a kind of Hemp Seed oil according to claim 1 is characterized in that described enzymolysis preferred parameter is: 60 ℃ of hydrolysis temperatures, and enzymolysis time 3.7h, enzymolysis pH value is 8.0, enzyme concentration is the 7050u/g substrate of weight of material.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103385925A (en) * | 2013-07-18 | 2013-11-13 | 中国人民武装警察部队后勤学院 | Fructus cannabis enzymolysis fermentation liquor having fatigue resistance and its preparation method and use |
| CN104026260A (en) * | 2013-04-01 | 2014-09-10 | 洛阳春魁农业开发有限公司 | Peony seed blend oil containing hemp seed oil and preparation method thereof |
| CN104450156A (en) * | 2014-11-21 | 2015-03-25 | 国家粮食局科学研究院 | Method for extracting grease in fructus cannabis by using aqueous enzymatic method and fructus cannabis protein drink |
| CN106889298A (en) * | 2015-12-21 | 2017-06-27 | 北京华昱安然医药科技有限公司 | A kind of fructus cannabis polypeptide powder and preparation method thereof |
| WO2019100538A1 (en) * | 2017-11-22 | 2019-05-31 | 陈程 | Process for extracting fructus cannabis oil |
| CN110684073A (en) * | 2019-11-19 | 2020-01-14 | 东北农业大学 | Preparation method of low-THC organic fructus cannabis protein powder |
| FR3087091A1 (en) * | 2018-10-11 | 2020-04-17 | Ornatum Cosmetologie | PROCESS FOR THE ENZYMATIC FRACTIONATION OF HEMP SEEDS |
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| US20050147722A1 (en) * | 2003-03-12 | 2005-07-07 | Gao Wen Fan | Integrated process for separation of oil, protein, carbohydrates, shell and minor toxic components from seeds |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104026260A (en) * | 2013-04-01 | 2014-09-10 | 洛阳春魁农业开发有限公司 | Peony seed blend oil containing hemp seed oil and preparation method thereof |
| CN104026260B (en) * | 2013-04-01 | 2016-03-02 | 洛阳春魁农业开发有限公司 | A kind of peony seeds ready-mixed oil containing fructus cannabis oil and preparation method thereof |
| CN103385925A (en) * | 2013-07-18 | 2013-11-13 | 中国人民武装警察部队后勤学院 | Fructus cannabis enzymolysis fermentation liquor having fatigue resistance and its preparation method and use |
| CN104450156A (en) * | 2014-11-21 | 2015-03-25 | 国家粮食局科学研究院 | Method for extracting grease in fructus cannabis by using aqueous enzymatic method and fructus cannabis protein drink |
| CN104450156B (en) * | 2014-11-21 | 2017-07-11 | 国家粮食局科学研究院 | The method of grease and a kind of fructus cannabis matter beverage in a kind of aqueous enzymatic extraction fructus cannabis |
| CN106889298A (en) * | 2015-12-21 | 2017-06-27 | 北京华昱安然医药科技有限公司 | A kind of fructus cannabis polypeptide powder and preparation method thereof |
| WO2019100538A1 (en) * | 2017-11-22 | 2019-05-31 | 陈程 | Process for extracting fructus cannabis oil |
| FR3087091A1 (en) * | 2018-10-11 | 2020-04-17 | Ornatum Cosmetologie | PROCESS FOR THE ENZYMATIC FRACTIONATION OF HEMP SEEDS |
| CN110684073A (en) * | 2019-11-19 | 2020-01-14 | 东北农业大学 | Preparation method of low-THC organic fructus cannabis protein powder |
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