CN103351944A - Method for extracting grape seed oil by cold pressing - Google Patents
Method for extracting grape seed oil by cold pressing Download PDFInfo
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Abstract
The invention discloses a method for extracting grape seed oil by cold pressing, which can ensure the natural characteristic of the grape seed oil, is less in nutritional ingredient loss, and meanwhile can obtain higher oil extraction rate. The method comprises the step of adding compound enzyme enzymolysis process in the grape seed preprocessing step. The invention has the benefits that the technical scheme is that the cell walls of grape seeds are further destroyed by adopting an enzymolysis technology to facilitate oil flowing out, and then the grape seeds are cold-pressed to extract oil. The invention has the advantages that the natural characteristic of the grape seed oil can be ensured, the nutritional ingredient loss is less, and meanwhile, higher oil extraction rate can be obtained, so that the resources can be utilized more sufficiently. From the aspects of the production technology, the technological parameters and the product quality, as compared with the similar technology, the method adopting the technical scheme shows a good application effect and is high in product quality.
Description
Technical field
The present invention relates to the complete processing of raisin seed oil, be specifically related to a kind of method of cold press raisin seed oil.
Background technology
The waste (skin, seed, stalk) that the wine making process produces accounts for the 20%-30% of fresh fruit total amount, and wherein Semen Vitis viniferae accounts for the 7%-10% of fresh fruit gross weight, and the annual Semen Vitis viniferae waste that produces of China's wine industry is above 4.2 ten thousand tons.Northern Xinjiang Northern Slope of Tianshan Mountains and eastern boundary Turfan, Hami Prefecture abound with Wine Grape, and Wine Enterprises is more, and the reclamation area, Shihezi is 50,000 mu of Wine Grapes of achievement, just at have 40,000 mu in vegetative period, are planned for 2015 with cultivated area and expand 200,000 mu to.At present, Semen Vitis viniferae except small part as feed and the fertilizer, major part is simply discarded, and has not only caused the waste of resource, has also increased environmental stress.
Research is found, it is suitable with main oil crops soybean oleaginousness that the oleaginousness of Semen Vitis viniferae is about 14%-17%(), the semi-drying grease that belongs to unsaturated fatty acids, contain a large amount of unsaturated fatty acidss, content comprises palmitinic acid, stearic acid, oleic acid, linolic acid and micro-linolenic acid, lauric acid, tetradecanoic acid etc. up to more than 90%.Its main function composition is linolic acid, be essential fatty acid, content reaches more than 70%, all high than in general edible oil even the medicinal oil walnut oil Flos Carthami oil of content, it is one of important composition that consists of human body cell film and skin, for children's brain and neurodevelopment, and keep the grownup blood fat balance, reducing cholesterol, prevent thrombosis, the effects such as prevention of arterial sclerosis all play an important role.In addition, raisin seed oil also contains on a small quantity (≤1%) linolenic acid, linolenic acid is all essential fatty acid, must take in by diet, can be the EPA(timnodonic acid by liver metabolism), the DHA(docosahexenoic acid) and the DPA(clupanodonic acid) 3 kinds of polyunsaturated fatty acids, has the characteristic that easily enters brain cell by blood vessel, it is the brain-invigorating nutrition of high-quality, can promote neural system, brain and amphiblestroid growth, improve brain function and learning and memory, can play and improve memory, prevention senile dementia and allergy effect.Raisin seed oil contains multiple liposoluble vitamin (A, E, D, K, P) and various trace elements (Ca, Fe, Zn, Mn, Cu).In addition, raisin seed oil contains pycnogenols (OPC), to be that present occurring in nature is found anti-oxidant, anti-aging, acid base equilibrium is provided, remove the strongest material of free radical ability, and prevention of various diseases occurs, and particularly cardiovascular and cerebrovascular diseases is had good preventive effect.Raisin seed oil has the improvement effect and regulates the effects such as immunity of organisms, antianaphylaxis, anti-inflammatory microcirculation in human body, Patients with Cardiovascular/Cerebrovascular Diseases and renal disease patient there is auxiliary therapeutic action, also can stimulate circulation, fat is subdued gradually, play the effect of weight-reducing.Raisin seed oil nutritive value and medical functions all obtain domestic and international medical circle and nutritionist's abundant affirmation.
The major way that tradition is extracted raisin seed oil has solvent extraction method, supercritical CO
2Extraction process, mechanical expression method, aqueous enzymatic method.Although solvent extraction method extraction efficiency easy and simple to handle is higher, demonstrate industrial shortcoming, dissolvent residual can bring food safety hidden danger, high temperature extraction environmental disruption effective constituent; Supercritical CO
2The extraction process extraction efficiency is high, and extraction product is pollution-free, has kept the bioactive functions composition, but because material requested, apparatus expensive so that extraction cost is high, therefore mainly are conceived to small scale experiments, difficult realization large-scale commercial production.Aqueous enzymatic method prepares raisin seed oil can improve oil yield, but because the enzyme consumption is large, cost significantly increases; The mechanical expression method realizes that easily large-scale industrialization production is subject to brewery's favor because device simple, easy and simple to handle, however traditional milling process under 105 ℃ of high temperature, carry out, activeconstituents and thermally labile component are decomposed in the course of processing destroy.
In view of to the demand of green food and growing with each passing day of environmental consciousness, the cold pressing oil technology take reduce industrial production to the pollution of product and environment as advantage, caused great concern in production characteristic healthy oils field.
Cold pressing oil belongs to physics liquefaction method, keep under the condition of homo(io)thermism by mechanical force material this technique of pressurizeing being had following characteristics: 1) avoided the impact of high temperature on material, can in expressing process, not produce the objectionable impuritiess such as trans fatty acid, grease polymer and make the sex change of nutrition of lipids material, keep the active substance in the pressed oil; 2) pressed oil that obtains satisfies directly edible condition, do not need further oil and fat refining, thereby avoided pressed oil in refining process, directly to contact with alkali lye, bleaching clay, phosphoric acid etc. and the high temperature during refining destroys the stability that grease may cause, kept to greatest extent the peculiar flavour of various fat-soluble nutritive ingredients in the grease such as VA and VE grease; When 3) having removed all kinds of industrial chemicals such as soda acid from and consume, avoided Chinese honey locust, soil to wash the various reaction waste such as waste water to the pollution of environment, so cold pressing process is a kind of oil-producing technique that has fewer environmental impacts, pollution-free at whole course of processing Green; 4) raisin seed oil that extracts with cold-press has natural pollution-free, is rich in fat-soluble nutritive ingredient and natural flavour mountaineous advantage, meets the organic pollution-free food theory of edible natural that present people praise highly.
But the cold pressing oil technology is only carried out strip plate to oil plant and is processed, and does not fry base processing, causes a large amount of cell walls of oil grain can not be destroyed, and the squeezing residual oil content of getting oil reaches about 20-35% usually.
Summary of the invention
Purpose of the present invention is exactly for above-mentioned defective of the prior art, and a kind of natural characteristic that both can guarantee raisin seed oil is provided, and nutrient loss is few, also can obtain the more method of the cold press raisin seed oil of high oil recovery simultaneously.
To achieve these goals, technical scheme provided by the invention is: a kind of method of cold press raisin seed oil is to add the complex enzyme zymohydrolysis process in the pre-treatment step of Semen Vitis viniferae.
Further, the method for above-mentioned a kind of cold press raisin seed oil, the enzymolysis process of described Semen Vitis viniferae will be for carrying out complex enzyme hydrolysis with cellulase, neutral protease and polygalacturonase through the Semen Vitis viniferae that rolls the embryo processing.
Further, the method for above-mentioned a kind of cold press raisin seed oil, the blending ratio of described complex enzyme hydrolysis process are cellulase: neutral protease: polygalacturonase is 1:1:0.5; The addition of described prozyme is 0.2% of Semen Vitis viniferae weight; Described hydrolysis temperature is 45 ℃; Described enzymolysis time is 8 hours.
A kind of method of cold press raisin seed oil, its whole process may further comprise the steps:
1) cleaning removal of impurities: by selection by winnowing and screening the Semen Vitis viniferae raw material is cleaned, foreign matter content is reduced to≤0.5%;
2) moisture is regulated: the Semen Vitis viniferae moisture content is adjusted to 8-10%, is beneficial to strip plate and processes;
3) strip plate: adopt two roller crushing rolls to roll sheet and process, the base sheet thickness after rolling is 0.6-1mm, chip index≤5%;
4) enzymolysis: adopt complex enzyme zymohydrolysis technique, the prozyme proportioning is cellulase: neutral protease: polygalacturonase is 1:1:0.5, and amount of water 20%, enzyme addition are 0.2%, and 45 ℃ of hydrolysis temperatures, enzymolysis time are 8h;
5) moisture and temperature regulation: again regulate moisture content and the temperature of Semen Vitis viniferae material base, to reach condition required for pressing, the pan feeding temperature is 55 ℃, pan feeding moisture content 4.0%;
6) squeezing: pressing bore temperature is 55 ℃, and gun pressure is 35MPa;
7) refining: depickling, excess alkali quantity are 20%, concentration of lye 10～30 degree Beaume; Decolouring, the adsorptive clay addition is take elaeometer as 2%, time 1.5h; Deodorization, vacuum tightness are residual voltage 550 handkerchiefs, and temperature is 240～260 ℃.
Beneficial effect of the present invention is: technical scheme provided by the invention is after to the Semen Vitis viniferae strip plate, adopt zymolysis technique that the cell walls of seed is further destroyed, be beneficial to the outflow of grease, carry out again cold press and get oil, its advantage is the natural characteristic that can guarantee raisin seed oil, nutrient loss is few, also can obtain higher oil yield simultaneously, and resource is utilized more fully.
From production technique, processing parameter and three aspects of quality product, present technique is as follows with the concrete comparable situation of domestic and international similar technology:
(1) comparison of production technique
Adopt the composite zymolysis technique of multienzyme that the Semen Vitis viniferae material base is carried out pre-treatment in the present technique production technique, get oil tech by cold press again and obtain raisin seed oil.
1. enzymolysis process: at present, in the domestic and international similar technology, cold press is got oil and is only adopted strip plate to process, and this mode oil grain cell walls destroys not thorough, causes residual oil content too high.Present technique is after carrying out the strip plate processing to the Semen Vitis viniferae material, increase cellulase, polygalacturonase and neutral protease complex enzyme hydrolysis technique, utilized the associating enzymolysis of multienzyme, greatly destroyed the seed cell wall, thereby can reduce residual oil content, improve the Semen Vitis viniferae oil yield.
2. oily technique is got in cold press: by to pressing the material temperature degree, press material humidity, pressing bore temperature and the isoparametric control of gun pressure, optimize the Semen Vitis viniferae cold press and get oily technique.
(2) comparison of processing parameter
Present technique mainly is the comparison that oily processing parameter is got in Semen Vitis viniferae pre-treatment and cold press with the parameter of domestic and international similar technology:
1. to get the preprocessing process of oil simple in traditional Semen Vitis viniferae cold press, be about to the removal of impurities of Semen Vitis viniferae selection by winnowing after, adopt two roller harders to carry out compressing tablet and process, compressing tablet thickness is generally 0.6-1.0mm; Present technique is on the basis that compressing tablet is processed, adopt the complex enzyme zymohydrolysis technology that material base is further processed, then carry out cold press and get oil, processing parameter is: amount of water 20%, the prozyme proportioning is cellulase: neutral protease: polygalacturonase=1:1:0.5,45 ℃ of hydrolysis temperatures, enzymolysis time 8h, enzyme addition 0.20%(is in the material base amount).
2. Semen Vitis viniferae cold pressing oil processing parameter: oily processing parameter is got in traditional Semen Vitis viniferae cold press, 50 ℃ of temperature of charge, and material moisture 4.5% presses 50 ℃ of bore temperatures, gun pressure 40MPa.Present technique is owing to there is enzymolysis pretreated auxiliary, and processing parameter is 55 ℃ of temperature of charge, and material moisture 4.0% presses 55 ℃ of bore temperatures, gun pressure 35MPa, and the oil yield of Semen Vitis viniferae reaches 92.37%.
(3) comparison of quality product
Adopt the cold press raisin seed oil of present technique preparation, its Oranoleptic indicator, physical and chemical index all are better than national raisin seed oil standard (GB/T 22478-2008), and quality product measured value and national Specification value are more as shown in table 1.
Table 1
| Project | Unit | International prescribed value | The product measured value |
| Color and luster | / | Light green or light yellow | Meet |
| Smell, flavour | / | Smell, mouthfeel are good | Normally |
| Transparency | / | Clarification, transparent | Meet |
| Acid number (KOH) | mg/g | ≤0.60 | 0.21 |
| Moisture and volatile matter content | % | ≤0.10 | 0.01 |
| Impurity | % | ≤0.05 | 0.03 |
| Peroxide value | mmol/kg | ≤5.0 | 1.3 |
| Saponified matter content | % | ≤0.005 | 0.004 |
Net result shows that present technique is applied to enzymolysis process in the preparation of cold press raisin seed oil, and effect is good, and quality product is high.
Description of drawings
Fig. 1 is that the proportioning of enzyme is on the impact of Semen Vitis viniferae oil yield.
Fig. 2 is that the addition of enzyme is on the impact of Semen Vitis viniferae oil yield.
Fig. 3 is that hydrolysis temperature is on the impact of Semen Vitis viniferae oil yield.
Fig. 4 is that enzymolysis time is on the impact of Semen Vitis viniferae oil yield.
Fig. 5 is that gun pressure is on the impact of Semen Vitis viniferae oil yield.
Fig. 6 is for pressing bore temperature to the impact of Semen Vitis viniferae oil yield.
Fig. 7 is that material temperature is on the impact of Semen Vitis viniferae oil yield.
Fig. 8 is that raw material moisture is on the impact of Semen Vitis viniferae oil yield.
Embodiment
Embodiment 1:
The enzyme pre-treatment on Semen Vitis viniferae cold press get the impact of oily technique:
1, materials and methods:
1.1 raw material and reagent:
Semen Vitis viniferae: the sky, Shihezi becomes grease company limited to provide.(vigor is 10 to polygalacturonase, 000U/g), (vigor is 10 to cellulase, 000U/g), (vigor is 50 to neutral protease, 000U/g), all is purchased from the extensive and profound in meaning bio tech ltd in Beijing.
1.2 instrument and equipment:
PHS-2C type acidometer, Shanghai Precision Scientific Apparatus Co., Ltd; DGG-9053AD type Constant Temp. Oven, the gloomy reliable Instr Ltd. that tests in Shanghai; MLS-3020 type high pressure steaming cooking vessel, SANYO; LXJ-I-IB type whizzer, Town in Shanghai booth science and technology instrument plant; HH-4 type digital display thermostat water bath, state China Electrical Appliances Co., Ltd.2, experimental technique:
2.1 the pre-treatment of Semen Vitis viniferae:
Adopt selection by winnowing and vibratory screening apparatus that Semen Vitis viniferae mesometamorphism, flat shell, individuality that epidermis is broken are gone out, soak the fruit juice mucus of removing the surface with clear water again, put shady and cool ventilation place natural air drying, be placed into shady and cool lucifuge place behind the good seal and be in store for.
2.2 compressing tablet:
The Semen Vitis viniferae that the two roller flaking machines of employing will be cleared up after the removal of impurities carries out the compressing tablet processing, requires Semen Vitis viniferae base sheet thickness to reach 0.6-1.0mm.
2.3 wetting:
By softening kettle the moisture content of Semen Vitis viniferae base sheet is adjusted to 20%, 40 ℃ of temperature.
2.4 enzymolysis:
Material is regulated moisture and temperature, add a certain proportion of neutral protease, polygalacturonase and cellulase and carry out enzymolysis, be warming up to 85 ℃ of enzymes that go out after for some time and process.Make it be fit to the squeezing liquefaction again to regulate material moisture and temperature, take the oil yield of Semen Vitis viniferae as evaluation index, investigate the factors such as proportioning, addition, hydrolysis temperature and enzymolysis time of enzyme to the impact of oil yield.
2.5 the mensuration of Semen Vitis viniferae oil length (soxhlet extraction):
With reference to country of the People's Republic of China (PRC) accurate (GB/T 5009.6-1985).
In the formula: m
1-receiving bottle quality (g)
m
2-receiving bottle and fat mass (g)
M-Semen Vitis viniferae quality (g)
2.6 Semen Vitis viniferae oil yield:
In the formula: M
0The quality of-Semen Vitis viniferae (g)
M
1The oil quality (g) that-squeezing obtains
The oil length of a-Semen Vitis viniferae
2.7 experiment of single factor:
(1) proportioning of enzyme is on the impact of Semen Vitis viniferae oil yield:
Hydrolysis temperature is made as 45 ℃, enzymolysis time 6h, pH5.0, cellulase: neutral protease: the blending ratio of polygalacturonase is set to respectively 1:1:1,2:1:1,3:1:1,1:2:1,1:3:1,1:1:0.5,1:1:1.5, Semen Vitis viniferae material base after the compressing tablet conditioning is carried out enzymolysis, the addition of enzyme is that 0.2%(is in the Semen Vitis viniferae quality), enzymolysis is adjusted to temperature 50 C after finishing, moisture content 5% is carried out cold press and got oil (gun pressure 35MPa, press 50 ℃ of bore temperatures), calculate oil yield, investigate the proportioning of enzyme to the impact of Semen Vitis viniferae oil yield.
(2) addition of enzyme is on the impact of Semen Vitis viniferae oil yield:
Hydrolysis temperature is made as 45 ℃, enzymolysis time 6h, pH5.0, cellulase: neutral protease: the blending ratio of polygalacturonase is made as 1:1:1, Semen Vitis viniferae material base after the compressing tablet conditioning is carried out enzymolysis, the addition of enzyme is made as respectively 0.1%, 0.15%, 0.2%, 0.25%, 0.3%(is in the Semen Vitis viniferae quality), enzymolysis is adjusted to temperature 50 C after finishing, moisture content 5% is carried out cold press and got oil (gun pressure 35MPa, press 50 ℃ of bore temperatures), calculate oil yield, investigate hydrolysis temperature to the impact of Semen Vitis viniferae oil yield.
(3) hydrolysis temperature is on the impact of Semen Vitis viniferae oil yield:
Enzymolysis time 6h, pH5.0, cellulase: neutral protease: the blending ratio of polygalacturonase is made as 1:1:1, hydrolysis temperature is made as respectively 35 ℃, 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃, Semen Vitis viniferae material base after the compressing tablet conditioning is carried out enzymolysis, the addition of enzyme is that 0.2%(is in the Semen Vitis viniferae quality), enzymolysis is adjusted to temperature 50 C after finishing, moisture content 5% is carried out cold press and got oil (gun pressure 35MPa, press 50 ℃ of bore temperatures), calculate oil yield, investigate hydrolysis temperature to the impact of Semen Vitis viniferae oil yield.
(4) enzymolysis time is on the impact of Semen Vitis viniferae oil yield:
Hydrolysis temperature is made as 45 ℃, pH5.0, cellulase: neutral protease: the blending ratio of polygalacturonase is made as 1:1:1, enzymolysis time is made as respectively 4h, 5h, 6h, 7h, 8h, 9h, and the Semen Vitis viniferae material base after the compressing tablet conditioning is carried out enzymolysis, and the addition of enzyme is that 0.2%(is in the Semen Vitis viniferae quality), enzymolysis is adjusted to temperature 50 C after finishing, moisture content 5% is carried out cold press and got oil (gun pressure 35MPa, press 50 ℃ of bore temperatures), calculate oil yield, investigate hydrolysis temperature to the impact of Semen Vitis viniferae oil yield.
2.8 orthogonal test:
According to the single factor experiment result, select each factor to choose 3 levels, adopt L
9(3
4) orthogonal table carries out the level of factor optimization Test, take the Semen Vitis viniferae oil yield as evaluation index, determines that the complex enzyme zymohydrolysis technical process is to the fuel-displaced optimal processing parameter of Semen Vitis viniferae cold press.
3 test results and analysis
3.1 the mensuration of Semen Vitis viniferae oil length
According to GB/T 5009.6-1985, select sherwood oil (30 ℃～60 ℃ of boiling ranges) as extraction agent, adopt the Soxhlet extraction process to measure the oil length of Semen Vitis viniferae, its concrete grammar is as follows:
1) preparation cellulose thimble: the filter paper of 8 * 15cm is converted into the test-tube model of diameter 2cm, forms the cellulose thimble of bottom seal, for subsequent use.
2) sample preparation: accurately take by weighing the Semen Vitis viniferae sample of 5g and move in the cellulose thimble.
3) lixiviate: cellulose thimble is put into apparatus,Soxhlet's, connect the fatty receiving bottle that has been dried to constant weight, add sherwood oil by the prolong upper end, dosage is 2/3 volume of receiving bottle, in water-bath (70 ℃) heating, make the continuous refluxing extraction of sherwood oil, extraction time be 6 hours complete to extracting till.
4) weigh: take off receiving bottle, reclaim sherwood oil, when treating that sherwood oil remains 1-2ml in the receiving bottle, evaporate to dryness in water-bath; 100 ℃-105 ℃ dry half an hour, be weighed into constant weight after the taking-up cooling again.
The oil length of the Semen Vitis viniferae that records is as shown in table 2:
Table 2
3.2 the enzymolysis pre-treatment is on the impact of Semen Vitis viniferae oil yield
3.2.1 single factor experiment:
(1) proportioning of enzyme is on the impact of Semen Vitis viniferae oil yield
As shown in Figure 1, cellulase: neutral protease: the proportioning of polygalacturonase has larger impact to the rate of recovery of grease in the useless carclazyte that decolours, when the neutral protease ratio content in the prozyme was low, the oil yield of Semen Vitis viniferae was higher, along with the larger oil yield of ratio of neutral protease is lower; When being 1:1:0.5, three's ratio reaches maximum value; In addition, the ratio that polygalacturonase accounts for prozyme presents same trend, and visible cellulase plays a part very important to the enzymolysis of oil grain cell walls.So cellulase is selected in follow-up test: neutral protease: polygalacturonase=1:1:0.5 carries out.
(2) addition of enzyme is on the impact of Semen Vitis viniferae oil yield
As shown in Figure 2, increase along with the addition of enzyme, the Semen Vitis viniferae oil yield is rapid ascendant trend, it is fuel-displaced to illustrate that prozyme extremely is conducive to the enzymolysis of Semen Vitis viniferae material base, when the addition of enzyme reaches after 0.2%, along with the increase of enzyme addition, oil yield amplification is mild, the cost of considering enzyme is high, and for reducing production costs, the enzyme addition of selection 0.2% is better.
(3) hydrolysis temperature is on the impact of Semen Vitis viniferae oil yield
As shown in Figure 3, hydrolysis temperature has larger impact to the Semen Vitis viniferae oil yield, when temperature reaches peak value during at 50 ℃, reduces temperature and raises and all reduce oil yield, and the optimum temperuture of this and enzyme has close relationship, and this enzymatic hydrolysis system is the synergy of plurality of enzymes in addition.
(4) enzymolysis time is on the impact of Semen Vitis viniferae oil yield
As shown in Figure 4, along with the prolongation of enzymolysis time, Semen Vitis viniferae oil yield rate is the trend that rises gradually, particularly in the 4-6h performance obviously, but enzymolysis time is less above the amplification of oil yield behind the 7h, considers the factors such as production cycle, energy consumption, and selecting better enzymolysis time is 7h.
3.2.2 orthogonal test
On the basis of single factor experiment, consider enzyme addition, hydrolysis temperature, enzymolysis time to the reciprocal effect of Semen Vitis viniferae oil yield, determine the pretreated optimal processing parameter of enzymolysis.Select the test of 3 factors, 3 horizontal quadratures, level of factor sees Table 3, L
9(3
4) orthogonal experiments sees Table 4.
Table 3
Table 4
By orthogonal experiments as can be known, each factor is followed successively by the impact of Semen Vitis viniferae oil yield: B＞C＞A, i.e. and hydrolysis temperature＞enzymolysis time＞enzyme addition, more excellent level of factor is combined as A
2B
2C
3, namely the enzyme addition is 0.2%, and 45 ℃ of hydrolysis temperatures, enzymolysis time are 8h, and oil yield is 91.87%.
4. the Quality Detection of raisin seed oil
According to the Quality Detection of " raisin seed oil " national standard (GB/T 22478-2008) to the cold press raisin seed oil.Moisture and volatile matter content 0.01%, impurity 0.03%, saponified matter content 0.004%, acid number 0.21mg/g, peroxide value 1.3mmol/kg,, plumbous 0.02mg/kg, aflatoxin B1＜10ug/kg, copper 0.01mg/kg, iron 0.02mg/kg, Tiguvon and Rogor do not detect.
5. conclusion
Utilize prozyme that the Semen Vitis viniferae material base is carried out the enzymolysis pre-treatment, can increase the Semen Vitis viniferae oil yield.The result shows: under this test and Selection condition, affect in 3 principal elements of Semen Vitis viniferae oil yield, hydrolysis temperature has the greatest impact to the oil recovery rate, has reached utmost point conspicuous level, and enzymolysis time and the impact of enzyme addition are not remarkable.Enzyme is processed top condition: the enzyme addition is 0.2%, and 45 ℃ of hydrolysis temperatures, enzymolysis time are 8h, and the oil recovery rate can reach 91.87% with this understanding.
Embodiment 2:
The optimization of Semen Vitis viniferae cold pressing oil technique:
1, experiment material and method:
The Semen Vitis viniferae raw material becomes grease company limited to provide by the sky, Shihezi.Experimental instrument and equipment sees Table 5.
Table 5
2, experimental technique:
2.1 the pre-treatment of Semen Vitis viniferae
Adopt selection by winnowing and vibratory screening apparatus that Semen Vitis viniferae mesometamorphism, flat shell, individuality that epidermis is broken are gone out, soak the fruit juice mucus of removing the surface with clear water again, put shady and cool ventilation place natural air drying, be placed into shady and cool lucifuge place behind the good seal and be in store for.
2.2 compressing tablet
The Semen Vitis viniferae that the two roller flaking machines of employing will be cleared up after the removal of impurities carries out the compressing tablet processing, requires Semen Vitis viniferae base sheet thickness to reach 0.6-1.0mm.
2.3 wetting
By softening kettle the moisture content of Semen Vitis viniferae base sheet is adjusted to 20%, 40 ℃ of temperature.
2.4 enzymolysis
Material is regulated moisture and temperature, add a certain proportion of neutral protease, polygalacturonase and cellulase and carry out enzymolysis, be warming up to 85 ℃ of enzymes that go out after for some time and process.Make it be fit to the squeezing liquefaction again to regulate material moisture and temperature, take the oil yield of Semen Vitis viniferae as evaluation index, investigate the factors such as proportioning, addition, hydrolysis temperature and enzymolysis time of enzyme to the impact of oil yield.
2.5 the mensuration of Semen Vitis viniferae oil length (soxhlet extraction)
With reference to country of the People's Republic of China (PRC) accurate (GB/T 5009.6-1985).
In the formula: m
1-receiving bottle quality (g)
m
2-receiving bottle and fat mass (g)
M-Semen Vitis viniferae quality (g)
2.6 Semen Vitis viniferae oil yield
In the formula: M
0The quality of-Semen Vitis viniferae (g)
M
1The oil quality (g) that-squeezing obtains
The oil length of a-Semen Vitis viniferae
2.7 oil is got in the Semen Vitis viniferae cold press
Press gun pressure power and be made as respectively 30Mpa, 35Mpa, 40Mpa, 45Mpa, 50Mpa; Press bore temperature and be made as 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃; The pan feeding temperature is made as 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃; The raw material water content is made as 3.5%, 4.0%, 4.5%, 5.0%, 5.5%, determines optimum process condition by the contrast experiment.
3 results and analysis
3.1 the mensuration of Semen Vitis viniferae oil length:
According to GB/T 5009.6-1985, select sherwood oil (30 ℃～60 ℃ of boiling ranges) as extraction agent, adopt the Soxhlet extraction process to measure the oil length of Semen Vitis viniferae, its concrete grammar is as follows:
1) preparation cellulose thimble: the filter paper of 8 * 15cm is converted into the test-tube model of diameter 2cm, forms the cellulose thimble of bottom seal, for subsequent use.
2) sample preparation: accurately take by weighing the Semen Vitis viniferae sample of 5g and move in the cellulose thimble.
3) lixiviate: cellulose thimble is put into apparatus,Soxhlet's, connect the fatty receiving bottle that has been dried to constant weight, add sherwood oil by the prolong upper end, dosage is 2/3 volume of receiving bottle, in water-bath (70 ℃) heating, make the continuous refluxing extraction of sherwood oil, extraction time be 6 hours complete to extracting till.
4) weigh: take off receiving bottle, reclaim sherwood oil, when treating that sherwood oil remains 1-2ml in the receiving bottle, evaporate to dryness in water-bath; 100 ℃-105 ℃ dry half an hour, be weighed into constant weight after the taking-up cooling again.
The oil length of 3 replications such as embodiment table 2.
3.2 oily technique is got in the Semen Vitis viniferae cold press
3.2.1 experiment of single factor
(1) gun pressure is on the impact of Semen Vitis viniferae oil yield
Learning from Fig. 5, is that the oil yield of 35MPa is the highest pressing gun pressure power, reaches 91.32%, significant difference.When press for extracting juice gun pressure power promoted gradually, oil yield was downward trend, is 50MPa when pressing gun pressure power, and oil yield only has 84.5%, and well below the oil yield of 35MPa, difference is extremely remarkable.Reason is that hypertonia can strengthen the degree of compacting of raw material, thereby has strengthened the circulating resistance of grease.Therefore select 35MPa as optimum process condition.
(2) press bore temperature to the impact of Semen Vitis viniferae oil yield
As shown in Figure 6, suitable temperature is conducive to keep pressing the essential plasticity-of material and reduce the grease viscosity during squeezing, yet the high temperature during squeezing also has side effects, rapid evaporation such as moisture destroys the normal plasticity of press for extracting juice material in squeezing, the oil cake color and luster is deepened even coking, the oxidation of grease, phosphatide and gossypol, the solubleness increase etc. in oil of the lipoid such as pigment, wax, for guaranteeing the quality of pressed oil, must the restriction pressing temperature.As can be seen from Figure 6, along with the rising of pressing bore temperature, oil yield also increases thereupon, and when press for extracting juice material temperature degree was 55 ℃, oil yield was the highest, significant difference.Surpass when being 55 ℃ when pressing bore temperature, oil yield descends to some extent, so select 55 ℃ as the optimum temps of pressing thoraxes.
(3) material temperature is on the impact of Semen Vitis viniferae oil yield
Set pressing bore temperature is 55 ℃, by the temperature that changes pan feeding material temperature is discussed the impact of cold press effect be the results are shown in Figure 7, and as can be seen from Figure 7, when the pan feeding temperature rose, oil yield rose gradually.The pan feeding temperature is 55 ℃ Semen Vitis viniferae, and oil yield is 91.39%, significant difference, and its grease color of producing is better in addition, and the physical and chemical index numerical value that records is also comparatively desirable.Material temperature is in the time of 55 ℃, and it is better to go out oil quality, carries out so subsequent experimental selects material temperature to be 55 ℃.
(4) moisture content of raw material is on the impact of Semen Vitis viniferae oil yield
Every group of 1000g of raw material, calculation formula: final amount of water X (g)=M (Z%-Y%)/(1-Z%).Wherein: M-group experimental raw total mass, Y%-raw material inherent moisture content, the moisture content that Z%-need to obtain.Drawing thus 4.5% moisture content should add 5g water on former basis, and 5.0% moisture content should add on former basis 10g water, 5.5% moisture content should add 16g water on former basis.At gun pressure 55MPa, under 55 ℃ of conditions of thorax temperature, experimental result is seen Fig. 8.
As shown in Figure 8, can judge when moisture content is 4.5%, the oil yield of Semen Vitis viniferae reaches maximum value, and every physical and chemical index is also comparatively desirable.
3.2.2 orthogonal test
On the basis of single factor experiment, consider gun pressure, press bore temperature and moisture content of raw material to the reciprocal effect of Semen Vitis viniferae oil yield, determine that the Semen Vitis viniferae cold press gets the optimal processing parameter of oil.Select the test of 3 factors, 3 horizontal quadratures, level of factor sees Table 6, L
9(3
4) orthogonal experiments sees Table 7.
Table 6
Table 7
By orthogonal experiments as can be known, each factor is followed successively by the impact of Semen Vitis viniferae oil yield: B〉A〉C, namely press bore temperature〉moisture content of raw material〉the gun pressure amount, optimum level of factor is combined as A
1B
2C
2, namely the raw material water content 4.0%, presses 55 ℃ of bore temperatures, and gun pressure 35MPa, oil yield are 92.37%.
4 cold press raisin seed oil physical and chemical indexs are analyzed, and are as shown in table 8.
Table 8
5. conclusion
Because have enzymolysis pretreated auxiliary, it is 55 ℃ of temperature of charge that oily processing parameter is got in the Semen Vitis viniferae cold press, material moisture 4.0% presses 55 ℃ of bore temperatures, gun pressure 35MPa, raisin seed oil extraction rate reached 92.37%.
Embodiment 3:
Pilot scale research:
In October, 2012, adopt enzymolysis-cold pressing process to become grease company limited to carry out pilot scale research in the sky, Shihezi, produce about 20 tons of raisin seed oil.Product is oyster, clarification, transparent, smell good mouthfeel, moisture and volatile matter content 0.01%, impurity 0.03%, saponified matter content 0.004%, acid number 0.21mg/g, peroxide value 1.3mmol/kg,, plumbous 0.02mg/kg, aflatoxin B1＜10ug/kg, copper 0.01mg/kg, iron 0.02mg/kg, Tiguvon and Rogor do not detect, and the product indices all reaches " raisin seed oil " national standard (GB/T22478-2008).
Technical process: sheet → enzymolysis → moisture and temperature regulation → squeezing → refining → can → warehouse-in are regulated → rolled to Semen Vitis viniferae → cleaning, removal of impurities → moisture.
Key points for operation:
(1) cleaning removal of impurities: by selection by winnowing and screening the Semen Vitis viniferae raw material is cleaned, required foreign matter content≤0.5%;
(2) moisture is regulated: the Semen Vitis viniferae moisture content is adjusted to 8-10%, is beneficial to strip plate and processes;
(3) strip plate: adopt two roller crushing rolls to roll sheet and process, require base sheet thickness 0.6-1mm, chip index≤5%;
(4) enzymolysis: adopt complex enzyme zymohydrolysis technique, the prozyme proportioning is cellulase: neutral protease: polygalacturonase=1:1:0.5, and amount of water 20%, enzyme addition are 0.2%, 45 ℃ of hydrolysis temperatures, enzymolysis time are 8h;
(5) moisture and temperature regulation: again regulate moisture content and the temperature of Semen Vitis viniferae material base, to reach condition required for pressing, requiring the pan feeding temperature is 55 ℃, pan feeding moisture content 4.0%;
(6) squeezing: pressing bore temperature is 55 ℃, and gun pressure is 35MPa.
(7) refining: depickling, excess alkali quantity are 20%, concentration of lye 10～30 degree Beaume; Decolouring, adsorptive clay addition 2%(is with elaeometer), time 1.5h; Deodorization, vacuum tightness (residual voltage 550 handkerchiefs), temperature (240～260 ℃).
It should be noted that at last: the above only is the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment the present invention is had been described in detail, for a person skilled in the art, it still can be made amendment to the technical scheme that aforementioned each embodiment puts down in writing, and perhaps part technical characterictic wherein is equal to replacement.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (4)
1. the method for a cold press raisin seed oil is characterized in that, is to add the complex enzyme zymohydrolysis process in the pre-treatment step of Semen Vitis viniferae.
2. the method for a kind of cold press raisin seed oil according to claim 1 is characterized in that, the enzymolysis process of described Semen Vitis viniferae will be for carrying out complex enzyme hydrolysis with cellulase, neutral protease and polygalacturonase through the Semen Vitis viniferae that rolls the embryo processing.
3. the method for a kind of cold press raisin seed oil according to claim 1 is characterized in that, the blending ratio of described complex enzyme hydrolysis process is cellulase: neutral protease: polygalacturonase is 1:1:0.5; The addition of described prozyme is 0.2% of Semen Vitis viniferae weight; Described hydrolysis temperature is 45 ℃; Described enzymolysis time is 8 hours.
4. the method for a cold press raisin seed oil is characterized in that, may further comprise the steps:
1) cleaning removal of impurities: by selection by winnowing and screening the Semen Vitis viniferae raw material is cleaned, foreign matter content is reduced to≤0.5%;
2) moisture is regulated: the Semen Vitis viniferae moisture content is adjusted to 8-10%, is beneficial to strip plate and processes;
3) strip plate: adopt two roller crushing rolls to roll sheet and process, the base sheet thickness after rolling is 0.6-1mm, chip index≤5%;
4) enzymolysis: adopt complex enzyme zymohydrolysis technique, the prozyme proportioning is cellulase: neutral protease: polygalacturonase is 1:1:0.5, and amount of water 20%, enzyme addition are 0.2%, and 45 ℃ of hydrolysis temperatures, enzymolysis time are 8h;
5) moisture and temperature regulation: again regulate moisture content and the temperature of Semen Vitis viniferae material base, to reach condition required for pressing, the pan feeding temperature is 55 ℃, pan feeding moisture content 4.0%;
6) squeezing: pressing bore temperature is 55 ℃, and gun pressure is 35MPa;
7) refining: depickling, excess alkali quantity are 20%, concentration of lye 10～30 degree Beaume; Decolouring, the adsorptive clay addition is take elaeometer as 2%, time 1.5h; Deodorization, vacuum tightness are residual voltage 550 handkerchiefs, and temperature is 240～260 ℃.
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