CN103351944B - 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 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 Semen Vitis viniferae waste that China's wine industry produces every year is more than 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 stone member is achievement 50,000 mu of Wine Grapes, have 40,000 mu just in vegetative period, are planned for 2015 and expand cultivated area to 200,000 mu.At present, Semen Vitis viniferae is except small part is as except feed and fertilizer, and major part is simply discarded, and not only causes the waste of resource, too increases environmental stress.
Research finds, it is suitable with main oil crops soybean oleaginousness that the oleaginousness of Semen Vitis viniferae is about 14%-17%(), belong to the semi-drying grease of unsaturated fatty acids, containing a large amount of unsaturated fatty acids, content, up to more than 90%, comprises palmitinic acid, stearic acid, oleic acid, linolic acid and micro-linolenic acid, lauric acid, tetradecanoic acid etc.Its main function composition is linolic acid, for essential fatty acid, content reaches more than 70%, all high than in general edible oil even medicinal oil walnut oil Flos Carthami oil of content, it is one of important composition forming human body cell film and skin, for children's brain and neurodevelopment, and the blood fat maintaining grownup balances, reduces cholesterol, prevents thrombosis, and the effect such as prevention of arterial sclerosis all plays an important role.In addition, raisin seed oil is also containing a small amount of (≤1%) linolenic acid, linolenic acid is all essential fatty acid, must be taken in by diet, be EPA(timnodonic acid by liver metabolism), DHA(docosahexenoic acid) and DPA(clupanodonic acid) 3 kinds of polyunsaturated fatty acids, be there is the characteristic easily being entered brain cell by blood vessel, it is the brain-invigorating nutrition of high-quality, neural system, brain and amphiblestroid growth can be promoted, improve brain function and learning and memory, Improving memory power can be played, 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), be current occurring in nature find anti-oxidant, anti-aging, acid base equilibrium, material that Scavenging ability is the strongest are provided, prevention of various diseases occurs, and particularly has good preventive effect to cardiovascular and cerebrovascular diseases.Raisin seed oil has improvement result to microcirculation in human body and regulates the effects such as immunity of organisms, antianaphylaxis, anti-inflammatory, auxiliary therapeutic action is had to Patients with Cardiovascular/Cerebrovascular Diseases and renal disease patient, also can stimulate circulation, fat is cut down gradually, play effect of weight-reducing.Raisin seed oil nutritive value and medical functions all obtain the abundant affirmation of domestic and international medical circle and nutritionist.
The major way that tradition extracts 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
2extraction process extraction efficiency is high, and extraction product is pollution-free, remains bioactive functions composition, but makes extraction cost high due to material requested, apparatus expensive, is therefore mainly conceived to small scale experiments, more difficultly realizes large-scale commercial production.Aqueous enzymatic method prepares raisin seed oil can improve oil yield, but due to enzyme consumption large, cost significantly increases; Mechanical expression method, due to device simple, easy and simple to handle, easily realizes industrialization scale operation and be subject to brewery's favor, but conventional press method is carried out under 105 DEG C of high temperature, easily makes activeconstituents and thermally labile component meet with decomposing in the course of processing destroying.
In view of to the demand of green food and growing with each passing day of environmental consciousness, cold pressing oil technology, to reduce the pollution of industrial production to product and environment for advantage, causes great concern in production special health grease field.
Cold pressing oil belongs to physics liquefaction method, on material this technique of pressurizeing, there is following characteristics by mechanical force under keeping the condition of homo(io)thermism: 1) avoid the impact of high temperature on material, the objectionable impurities such as trans fatty acid, grease polymer can not be produced make the sex change of nutrition of lipids material in expressing process, remain the active substance in pressed oil; 2) pressed oil obtained meets directly edible condition, do not need further oil and fat refining, thus avoid pressed oil directly contact with alkali lye, bleaching clay, phosphoric acid etc. in refining process and refining time high temperature the stability that grease may cause is destroyed, to remain in grease various fat-soluble nutrients composition to greatest extent as the peculiar flavour of VA and VE grease; 3) eliminate while all kinds of industrial chemicals such as soda acid consumes, avoid Chinese honey locust, soil washes the various reaction waste such as waste water to the pollution of environment, therefore cold pressing process is a kind of oil-producing technique had fewer environmental impacts, pollution-free at whole course of processing Green; 4) have natural pollution-free with the raisin seed oil that cold-press extracts, be rich in fat-soluble nutrients composition and natural flavour mountaineous advantage, meet the organic pollution-free food theory of edible natural that current people praise highly.
But cold pressing oil technology only carries out strip plate process to oil plant, do not carry out the processing of stir-fry base, the cell walls causing oil grain a large amount of can not be destroyed, and usually squeezes the residual oil content getting oil and reaches about 20-35%.
Summary of the invention
Object of the present invention is exactly for above-mentioned defect of the prior art, and provide a kind of natural characteristic that both can ensure raisin seed oil, nutrient loss is few, also can obtain the method for the cold press raisin seed oil of more 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 add 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 is that the Semen Vitis viniferae through rolling embryo process is carried out complex enzyme hydrolysis with cellulase, neutral protease and polygalacturonase.
Further, the method for above-mentioned a kind of cold press raisin seed oil, 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 DEG C; Described enzymolysis time is 8 hours.
A method for cold press raisin seed oil, its whole process, comprises the following steps:
1) removal of impurities is cleared up: by selection by winnowing and screening, Semen Vitis viniferae raw material is cleaned, foreign matter content is reduced to≤0.5%;
2) moisture regulates: Semen Vitis viniferae moisture content is adjusted to 8-10%, is beneficial to strip plate process;
3) strip plate: adopt two roller crushing roll to carry out rolling sheet process, the blank thickness after rolling is 0.6-1mm, chip index≤5%;
4) enzymolysis: adopt complex enzyme zymohydrolysis technique, enzyme ratio is cellulase: neutral protease: polygalacturonase is 1:1:0.5, amount of water 20%, and enzyme addition is 0.2%, hydrolysis temperature 45 DEG C, and enzymolysis time is 8h;
5) moisture and temperature regulate: the moisture content and the temperature that again regulate Semen Vitis viniferae material base, and to reach condition required for pressing, pan feeding temperature is 55 DEG C, pan feeding moisture content 4.0%;
6) squeeze: squeezing bore temperature is 55 DEG C, and gun pressure is 35MPa;
7) refining: depickling, excess alkali quantity is 20%, concentration of lye 10 ~ 30 degree Beaume; Decolouring, adsorptive clay addition with elaeometer for 2%, time 1.5h; Deodorization, vacuum tightness is residual voltage 550 handkerchief, and temperature is 240 ~ 260 DEG C.
Beneficial effect of the present invention is: technical scheme provided by the invention is after to Semen Vitis viniferae strip plate, the cell walls of zymolysis technique to seed is adopted to destroy further, be beneficial to the outflow of grease, carry out cold press again and get oil, its advantage is the natural characteristic that can ensure raisin seed oil, nutrient loss is few, also can obtain higher oil yield simultaneously, resource is utilized more fully.
From production technique, processing parameter and quality product three aspects, this technology is as follows with the concrete comparable situation of domestic and international similar technique:
(1) comparison of production technique
The zymolysis technique adopting multienzyme composite in this technology production technique carries out pre-treatment to Semen Vitis viniferae material base, then gets oil tech acquisition raisin seed oil by cold press.
1. enzymolysis process: at present, in domestic and international similar technique, cold press is got oil and is only adopted strip plate process, and this mode oil grain cell wall damage is not thorough, causes residual oil content too high.This technology is after carrying out strip plate process to Semen Vitis viniferae material, add cellulase, polygalacturonase and neutral protease complex enzyme hydrolysis technique, utilize the associating enzymolysis of multienzyme, greatly destroy seed cell wall, thus can residual oil content be reduced, improve Semen Vitis viniferae oil yield.
2. oily technique is got in cold press: by squeezing material temperature degree, squeezing material humidity, pressure bore temperature and the isoparametric control of gun pressure, optimize Semen Vitis viniferae cold press and get oily technique.
(2) comparison of processing parameter
The parameter of this technology and domestic and international similar technique more mainly Semen Vitis viniferae pre-treatment and cold press gets the comparison of oily processing parameter:
1. traditional Semen Vitis viniferae cold press gets the preprocessing process of oil simply, and after the removal of impurities of Semen Vitis viniferae selection by winnowing, adopt two roller harder to carry out compressing tablet process, sheeting thickness is generally 0.6-1.0mm; This technology is on the basis of compressing tablet process, complex enzyme zymohydrolysis technology is adopted to be further processed material base, then carry out cold press and get oil, processing parameter is: amount of water 20%, enzyme ratio is cellulase: neutral protease: polygalacturonase=1:1:0.5, hydrolysis temperature 45 DEG C, enzymolysis time 8h, enzyme addition 0.20%(is with material base gauge).
2. Semen Vitis viniferae cold pressing oil processing parameter: oily processing parameter is got in traditional Semen Vitis viniferae cold press, temperature of charge 50 DEG C, material moisture 4.5%, squeezes bore temperature 50 DEG C, gun pressure 40MPa.This technology is owing to there being enzymolysis pretreated auxiliary, and processing parameter is temperature of charge 55 DEG C, material moisture 4.0%, and squeeze bore temperature 55 DEG C, gun pressure 35MPa, the oil yield of Semen Vitis viniferae reaches 92.37%.
(3) comparison of quality product
The cold press raisin seed oil adopting this technology to prepare, its Oranoleptic indicator, physical and chemical index are all better than national raisin seed oil standard (GB/T 22478-2008), and quality product measured value is more as shown in table 1 with national Specification value.
Table 1
| Project | Unit | International regulations value | 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 this technology and is applied to by enzymolysis process in the preparation of cold press raisin seed oil, and effect is good, and quality product is high.
Accompanying drawing explanation
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 the impact of hydrolysis temperature on Semen Vitis viniferae oil yield.
Fig. 4 is the impact of enzymolysis time on Semen Vitis viniferae oil yield.
Fig. 5 is the impact of gun pressure on Semen Vitis viniferae oil yield.
Fig. 6 squeezes bore temperature to the impact of Semen Vitis viniferae oil yield.
Fig. 7 is the impact of material temperature on Semen Vitis viniferae oil yield.
Fig. 8 is the impact of raw material moisture on Semen Vitis viniferae oil yield.
Embodiment
Embodiment 1:
Enzyme pre-treatment gets the impact of oily technique to Semen Vitis viniferae cold press:
1, materials and methods:
1.1 raw materials and reagent:
Semen Vitis viniferae: Shihezi Tian Cheng grease company limited provides.Polygalacturonase (vigor is 10,000U/g), cellulase (vigor is 10,000U/g), neutral protease (vigor is 50,000U/g), be all purchased from extensive and profound in meaning bio tech ltd, Beijing.
1.2 instrument and equipments:
PHS-2C type acidometer, Shanghai Precision Scientific Apparatus Co., Ltd; DGG-9053AD type Constant Temp. Oven, Shanghai is gloomy reliablely tests Instrument Ltd.; MLS-3020 type high pressure steaming cooking vessel, SANYO; LXJ-I-IB type whizzer, Town in Shanghai booth tech equipment factory; HH-4 type digital display thermostat water bath, Guo Hua Electrical Appliances Co., Ltd.2, experimental technique:
The pre-treatment of 2.1 Semen Vitis viniferaes:
Adopt selection by winnowing and vibratory screening apparatus Semen Vitis viniferae mesometamorphism, flat shell, individuality that epidermis is broken to be gone out, then soak the fruit juice mucus removing surface with clear water, put shady and cool ventilation place natural air drying, be placed into shady and cool lucifuge place after good seal and be in store for.
2.2 compressing tablets:
Adopt two roller flaking machine that the Semen Vitis viniferae after cleaning removal of impurities is carried out compressing tablet process, require that Semen Vitis viniferae blank thickness reaches 0.6-1.0mm.
2.3 soak:
By softening kettle, the moisture content of Semen Vitis viniferae blank is adjusted to 20%, temperature 40 DEG C.
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 DEG C after for some time and carry out going out ferment treatment.Again to regulate material moisture and temperature to make it be applicable to squeezing liquefaction, with the oil yield of Semen Vitis viniferae for evaluation index, the factors such as the proportioning of enzyme, addition, hydrolysis temperature and enzymolysis time of investigating are on the impact of oil yield.
The mensuration (soxhlet extraction) of 2.5 Semen Vitis viniferae oil length:
With reference to country of the People's Republic of China (PRC) accurate (GB/T 5009.6-1985).
In 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 yields:
In formula: M
0the quality (g) of-Semen Vitis viniferae
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 set to 45 DEG C, enzymolysis time 6h, pH5.0, cellulase: neutral protease: the blending ratio of polygalacturonase is set to 1:1:1,2:1:1,3:1:1,1:2:1,1:3:1,1:1:0.5,1:1:1.5 respectively, enzymolysis is carried out to the Semen Vitis viniferae material base after compressing tablet conditioning, the addition of enzyme is that 0.2%(is in Semen Vitis viniferae quality), be adjusted to temperature 50 C after enzymolysis terminates, moisture content 5% carries out cold press and get oil (gun pressure 35MPa, squeeze bore temperature 50 DEG C), 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 set to 45 DEG C, enzymolysis time 6h, pH5.0, cellulase: neutral protease: the blending ratio of polygalacturonase is set to 1:1:1, enzymolysis is carried out to the Semen Vitis viniferae material base after compressing tablet conditioning, the addition of enzyme is set to 0.1% respectively, 0.15%, 0.2%, 0.25%, 0.3%(is in Semen Vitis viniferae quality), be adjusted to temperature 50 C after enzymolysis terminates, moisture content 5% carries out cold press and get oil (gun pressure 35MPa, squeeze bore temperature 50 DEG C), 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 set to 1:1:1, hydrolysis temperature is set to 35 DEG C, 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C respectively, enzymolysis is carried out to the Semen Vitis viniferae material base after compressing tablet conditioning, the addition of enzyme is that 0.2%(is in Semen Vitis viniferae quality), be adjusted to temperature 50 C after enzymolysis terminates, moisture content 5% carries out cold press and get oil (gun pressure 35MPa, squeeze bore temperature 50 DEG C), 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 set to 45 DEG C, pH5.0, cellulase: neutral protease: the blending ratio of polygalacturonase is set to 1:1:1, enzymolysis time is set to 4h, 5h, 6h, 7h, 8h, 9h respectively, and carry out enzymolysis to the Semen Vitis viniferae material base after compressing tablet conditioning, the addition of enzyme is that 0.2%(is in Semen Vitis viniferae quality), be adjusted to temperature 50 C after enzymolysis terminates, moisture content 5% carries out cold press and get oil (gun pressure 35MPa, squeeze bore temperature 50 DEG C), calculate oil yield, investigate hydrolysis temperature to the impact of Semen Vitis viniferae oil yield.
2.8 orthogonal tests:
According to single factor experiment result, select each factor to choose 3 levels, adopt L
9(3
4) orthogonal table carries out level of factor optimization Test, with Semen Vitis viniferae oil yield for evaluation index, determines the fuel-displaced optimal processing parameter of complex enzyme zymohydrolysis technical process to Semen Vitis viniferae cold press.
3 test results and analysis
The mensuration of 3.1 Semen Vitis viniferae oil length
According to GB/T 5009.6-1985, select sherwood oil (boiling range 30 DEG C ~ 60 DEG C) as extraction agent, adopt soxhlet extraction methods to measure the oil length of Semen Vitis viniferae, its concrete grammar is as follows:
1) prepare cellulose thimble: the filter paper of 8 × 15cm is converted into the test-tube model that diameter is about 2cm, form the cellulose thimble of bottom seal, for subsequent use.
2) sample preparation: accurately take the Semen Vitis viniferae sample of 5g and move in cellulose thimble.
3) lixiviate: cellulose thimble is put into apparatus,Soxhlet's, connects the fatty receiving bottle being dried to constant weight, adds sherwood oil by prolong upper end, dosage is 2/3 volume of receiving bottle, in water-bath, (70 DEG C) heating, makes the continuous refluxing extraction of sherwood oil, and extraction time is 6 little till extracting is complete.
4) weigh: take off receiving bottle, reclaim sherwood oil, when in bottle to be received, sherwood oil remains 1-2ml, evaporate to dryness in water-bath; Again 100 DEG C-105 DEG C dry half an hour, after taking out cooling, be weighed into constant weight.
The oil length of the Semen Vitis viniferae recorded is as shown in table 2:
Table 2
3.2 enzymolysis pre-treatment are 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 decolouring spent bleaching clay, when the neutral protease proportional amount in prozyme is lower, the oil yield of Semen Vitis viniferae is higher, and the larger oil yield of the ratio along with neutral protease is lower; When proportions reaches maximum value for during 1:1:0.5; In addition, the ratio that polygalacturonase accounts for prozyme presents same trend, and the enzymolysis of fibres visible element enzyme to oil grain cell walls plays a part very important.Therefore 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, along with the increase of the addition of enzyme, Semen Vitis viniferae oil yield is rapid ascendant trend, illustrate that prozyme is extremely conducive to fuel-displaced 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, considering that the cost of enzyme is high, for reducing production cost, selecting the enzyme addition of 0.2% 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 Semen Vitis viniferae oil yield, reaches peak value when temperature is at 50 DEG C, and reduce temperature and raise and all reduce oil yield, the optimum temperuture of this and enzyme has close relationship, and this enzymatic hydrolysis system is the synergy of multiple enzyme 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 in the trend risen gradually, particularly in 4-6h performance obviously, but enzymolysis time is less more than the amplification of oil yield after 7h, considers the factor such as production cycle, energy consumption, select preferably enzymolysis time to be 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 3 factor 3 horizontal quadratures test, level of factor in table 3, L
9(3
4) orthogonal experiments is in table 4.
Table 3
Table 4
From orthogonal experiments, the impact of each factor on Semen Vitis viniferae oil yield is followed successively by: B > C > A, i.e. hydrolysis temperature > enzymolysis time > enzyme addition, more excellent level of factor is combined as A
2b
2c
3, namely enzyme addition is 0.2%, hydrolysis temperature 45 DEG C, and enzymolysis time is 8h, and oil yield is 91.87%.
4. the Quality Detection of raisin seed oil
According to " raisin seed oil " national standard (GB/T 22478-2008) Quality Detection to 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 to carry out enzymolysis pre-treatment to Semen Vitis viniferae material base, Semen Vitis viniferae oil yield can be increased.Result shows: under this test and Selection condition, and affect in 3 principal elements of Semen Vitis viniferae oil yield, hydrolysis temperature has the greatest impact to oil recovery rate, reaches pole conspicuous level, and enzymolysis time and enzyme addition affect not remarkable.Ferment treatment top condition is: enzyme addition is 0.2%, hydrolysis temperature 45 DEG C, and enzymolysis time is 8h, and 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:
Semen Vitis viniferae raw material is provided by Shihezi Tian Cheng grease company limited.Experimental instrument and equipment is in table 5.
Table 5
2, experimental technique:
The pre-treatment of 2.1 Semen Vitis viniferaes
Adopt selection by winnowing and vibratory screening apparatus Semen Vitis viniferae mesometamorphism, flat shell, individuality that epidermis is broken to be gone out, then soak the fruit juice mucus removing surface with clear water, put shady and cool ventilation place natural air drying, be placed into shady and cool lucifuge place after good seal and be in store for.
2.2 compressing tablet
Adopt two roller flaking machine that the Semen Vitis viniferae after cleaning removal of impurities is carried out compressing tablet process, require that Semen Vitis viniferae blank thickness reaches 0.6-1.0mm.
2.3 wetting
By softening kettle, the moisture content of Semen Vitis viniferae blank is adjusted to 20%, temperature 40 DEG C.
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 DEG C after for some time and carry out going out ferment treatment.Again to regulate material moisture and temperature to make it be applicable to squeezing liquefaction, with the oil yield of Semen Vitis viniferae for evaluation index, the factors such as the proportioning of enzyme, addition, hydrolysis temperature and enzymolysis time of investigating are on the impact of oil yield.
The mensuration (soxhlet extraction) of 2.5 Semen Vitis viniferae oil length
With reference to country of the People's Republic of China (PRC) accurate (GB/T 5009.6-1985).
In 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 yields
In formula: M
0the quality (g) of-Semen Vitis viniferae
M
1the oil quality (g) that-squeezing obtains
The oil length of a-Semen Vitis viniferae
Oil is got in 2.7 Semen Vitis viniferae cold press
Squeeze gun pressure power and be set to 30Mpa, 35Mpa, 40Mpa, 45Mpa, 50Mpa respectively; Squeeze bore temperature and be set to 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C; Pan feeding temperature is set to 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C; Feed moisture content is set to 3.5%, 4.0%, 4.5%, 5.0%, 5.5%, determines optimum process condition by contrast experiment.
3 results and analysis
The mensuration of 3.1 Semen Vitis viniferae oil length:
According to GB/T 5009.6-1985, select sherwood oil (boiling range 30 DEG C ~ 60 DEG C) as extraction agent, adopt soxhlet extraction methods to measure the oil length of Semen Vitis viniferae, its concrete grammar is as follows:
1) prepare cellulose thimble: the filter paper of 8 × 15cm is converted into the test-tube model that diameter is about 2cm, form the cellulose thimble of bottom seal, for subsequent use.
2) sample preparation: accurately take the Semen Vitis viniferae sample of 5g and move in cellulose thimble.
3) lixiviate: cellulose thimble is put into apparatus,Soxhlet's, connects the fatty receiving bottle being dried to constant weight, adds sherwood oil by prolong upper end, dosage is 2/3 volume of receiving bottle, in water-bath, (70 DEG C) heating, makes the continuous refluxing extraction of sherwood oil, and extraction time is 6 little till extracting is complete.
4) weigh: take off receiving bottle, reclaim sherwood oil, when in bottle to be received, sherwood oil remains 1-2ml, evaporate to dryness in water-bath; Again 100 DEG C-105 DEG C dry half an hour, after taking out cooling, be weighed into constant weight.
The oil length of 3 replications is as embodiment table 2.
Oily technique is got in 3.2 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
Learn from Fig. 5, being that the oil yield of 35MPa is the highest squeezing gun pressure power, reaching 91.32%, significant difference.When squeezing gun pressure power and promoting gradually, oil yield is downward trend, and when squeezing gun pressure power is 50MPa, 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 compactness of raw material, thus increases the circulating resistance of grease.Therefore select 35MPa as optimum process condition.
(2) bore temperature is squeezed on the impact of Semen Vitis viniferae oil yield
As shown in Figure 6, temperature suitable during squeezing is conducive to keeping squeezing the required plasticity-of material and reducing grease viscosity, but high temperature during squeezing also has side effects, sharply evaporation as moisture destroys squeezes the normal plasticity of material in squeezing, oil cake color and luster deepens even coking, the oxidation of grease, phosphatide and gossypol, and the lipoid such as pigment, wax are solubleness increase etc. in oil, for guaranteeing the quality of pressed oil, pressing temperature must be limited.As can be seen from Figure 6, along with the rising of squeezing bore temperature, oil yield also increases thereupon, and when squeezing material temperature degree is 55 DEG C, oil yield is the highest, significant difference.When squeeze bore temperature exceed be 55 DEG C time, oil yield declines to some extent, thus select 55 DEG C as squeezing thorax optimum temps.
(3) material temperature is on the impact of Semen Vitis viniferae oil yield
It is 55 DEG C that bore temperature is squeezed in setting, and by the temperature changing pan feeding, the impact of material temperature on cold press effect is discussed and the results are shown in Figure 7, as can be seen from Figure 7, when pan feeding temperature rises, oil yield rises gradually.Pan feeding temperature is the Semen Vitis viniferae of 55 DEG C, and oil yield is 91.39%, significant difference, and its grease color produced is better in addition, and the physical and chemical index numerical value recorded is also ideal.Material temperature, 55 DEG C time, goes out oil quality better, therefore subsequent experimental is selected material temperature to be 55 DEG C to carry out.
(4) moisture content of raw material is on the impact of Semen Vitis viniferae oil yield
Raw material often organizes 1000g, 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, Z%-needs the moisture content obtained.Show that the moisture content of 4.5% should add 5g water on former basis thus, the moisture content of 5.0% should add on former basis 10g water, 5.5% moisture content should add 16g water on former basis.At gun pressure 55MPa, under thorax temperature 55 DEG C of conditions, experimental result is shown in Fig. 8.
As shown in Figure 8, can judge that the oil yield of Semen Vitis viniferae reaches maximum value when moisture content is 4.5%, every physical and chemical index is also ideal.
3.2.2 orthogonal test
On the basis of single factor experiment, consider gun pressure, squeezing bore temperature and moisture content of raw material to the reciprocal effect of Semen Vitis viniferae oil yield, determine that the optimal processing parameter of oil is got in Semen Vitis viniferae cold press.Select 3 factor 3 horizontal quadratures test, level of factor in table 6, L
9(3
4) orthogonal experiments is in table 7.
Table 6
Table 7
From orthogonal experiments, the impact of each factor on Semen Vitis viniferae oil yield is followed successively by: B>A>C, namely squeeze bore temperature > moisture content of raw material > gun pressure amount, optimum level of factor is combined as A
1b
2c
2, i.e. feed moisture content 4.0%, squeeze bore temperature 55 DEG C, gun pressure 35MPa, oil yield is 92.37%.
4 cold press raisin seed oil physical and chemical indexs are analyzed, as shown in table 8.
Table 8
5. conclusion
Owing to there being enzymolysis pretreated auxiliary, it is temperature of charge 55 DEG C that oily processing parameter is got in Semen Vitis viniferae cold press, material moisture 4.0%, squeezes bore temperature 55 DEG C, 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 carry out pilot scale research in Shihezi Tian Cheng grease company limited, produce raisin seed oil about 20 tons.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 product indices all reaches " raisin seed oil " national standard (GB/T22478-2008).
Technical process: Semen Vitis viniferae → cleaning, removal of impurities → moisture regulate → roll sheet → enzymolysis → moisture and temperature adjustment → squeezing → refining → filling → warehouse-in.
Key points for operation:
(1) removal of impurities is cleared up: by selection by winnowing and screening, Semen Vitis viniferae raw material is cleaned, require foreign matter content≤0.5%;
(2) moisture regulates: Semen Vitis viniferae moisture content is adjusted to 8-10%, is beneficial to strip plate process;
(3) strip plate: adopt two roller crushing roll to carry out rolling sheet process, require blank thickness 0.6-1mm, chip index≤5%;
(4) enzymolysis: adopt complex enzyme zymohydrolysis technique, enzyme ratio is cellulase: neutral protease: polygalacturonase=1:1:0.5, amount of water 20%, and enzyme addition is 0.2%, hydrolysis temperature 45 DEG C, and enzymolysis time is 8h;
(5) moisture and temperature regulate: the moisture content and the temperature that again regulate Semen Vitis viniferae material base, to reach condition required for pressing, require that pan feeding temperature is 55 DEG C, pan feeding moisture content 4.0%;
(6) squeeze: squeezing bore temperature is 55 DEG C, and gun pressure is 35MPa.
(7) refining: depickling, excess alkali quantity is 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 handkerchief), temperature (240 ~ 260 DEG C).
Last it is noted that the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (1)
1. the method for a cold press raisin seed oil, it is characterized in that, be add complex enzyme zymohydrolysis process in the pre-treatment step of Semen Vitis viniferae, the enzymolysis process of described Semen Vitis viniferae is that the Semen Vitis viniferae through rolling embryo process is carried out complex enzyme hydrolysis with cellulase, neutral protease and polygalacturonase; 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 DEG C; Described enzymolysis time is 8 hours; The method of cold press raisin seed oil is made up of following steps:
1) removal of impurities is cleared up: by selection by winnowing and screening, Semen Vitis viniferae raw material is cleaned, foreign matter content is reduced to≤0.5%;
2) moisture regulates: Semen Vitis viniferae moisture content is adjusted to 8-10%, is beneficial to strip plate process;
3) strip plate: adopt two roller crushing roll to carry out rolling sheet process, the blank thickness after rolling is 0.6-1mm, chip index≤5%;
4) enzymolysis: adopt complex enzyme zymohydrolysis technique, enzyme ratio is cellulase: neutral protease: polygalacturonase is 1:1:0.5, amount of water 20%, and enzyme addition is 0.2%, hydrolysis temperature 45 DEG C, and enzymolysis time is 8h;
5) moisture and temperature regulate: the moisture content and the temperature that again regulate Semen Vitis viniferae material base, and to reach condition required for pressing, pan feeding temperature is 55 DEG C, pan feeding moisture content 4.0%;
6) squeeze: squeezing bore temperature is 55 DEG C, and gun pressure is 35MPa;
7) refining: depickling, excess alkali quantity is 20%, concentration of lye 10 ~ 30 degree Beaume; Decolouring, adsorptive clay addition with elaeometer for 2%, time 1.5h; Deodorization, vacuum tightness is residual voltage 550 handkerchief, and temperature is 240 ~ 260 DEG C.
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| CN103695154B (en) * | 2013-12-13 | 2015-07-08 | 广西科技大学 | Grease squeezing pretreatment agent for full peanuts |
| CN103740460B (en) * | 2014-01-15 | 2015-06-10 | 甘肃农业大学 | Method for extracting and purifying grape seed oil from grape seeds |
| CN104255956B (en) * | 2014-09-16 | 2017-09-19 | 丽江永胜边屯食尚养生园有限公司 | A kind of preparation method of walnut oil |
| CN105219522A (en) * | 2015-10-09 | 2016-01-06 | 上海韬鸿化工科技有限公司 | The method of soybean oil is prepared in low temperature cold squeezing |
| CN105199834A (en) * | 2015-10-13 | 2015-12-30 | 东北农业大学 | Method for preparing wild rose seed oil by enzymolysis-cold pressing process |
| CN105462681A (en) * | 2015-12-23 | 2016-04-06 | 刘家容 | Extracting process regulating grease ratio of colza oil |
| CN105969510A (en) * | 2016-05-18 | 2016-09-28 | 蚌埠市九华油脂有限公司 | High-oil yield preparation method of grape seed oil |
| CN106433948A (en) * | 2016-08-30 | 2017-02-22 | 闫涛 | Method for extracting grape seed oil through wetting-method squeezing |
| CN106318614A (en) * | 2016-09-27 | 2017-01-11 | 乌鲁木齐上善元生物科技有限公司 | Method for preparing oil by cold pressing of grape seeds |
| CN106883927A (en) * | 2017-03-09 | 2017-06-23 | 管天球 | A kind of preparation method of grape-kernel oil |
| CN107043649B (en) * | 2017-04-05 | 2020-09-25 | 吉首大学 | Method for preparing camellia seed oil by near-solid enzymolysis combined with physical squeezing |
| CN108285827B (en) * | 2018-04-10 | 2021-10-08 | 无限极（中国）有限公司 | Grape seed oil and preparation method thereof |
| CN112920891A (en) * | 2021-03-05 | 2021-06-08 | 河北宁心机械设计有限公司 | Virgin peanut oil and production process thereof |
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| CN101779705A (en) * | 2010-02-22 | 2010-07-21 | 北京市科威华食品工程技术有限公司 | Production method of grape seed oil |
| CN102268325A (en) * | 2011-06-22 | 2011-12-07 | 西北农林科技大学 | Cold-pressing extraction method of grape seed oil |
| CN102422902A (en) * | 2011-10-27 | 2012-04-25 | 周天 | Sea-buckthorn seed-grape seed composite vegetable bended oil and preparation method thereof |
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| CN102268325A (en) * | 2011-06-22 | 2011-12-07 | 西北农林科技大学 | Cold-pressing extraction method of grape seed oil |
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