CN107338107A - The extracting method of mongolian amygdalus seed grease - Google Patents
The extracting method of mongolian amygdalus seed grease Download PDFInfo
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- CN107338107A CN107338107A CN201710722578.1A CN201710722578A CN107338107A CN 107338107 A CN107338107 A CN 107338107A CN 201710722578 A CN201710722578 A CN 201710722578A CN 107338107 A CN107338107 A CN 107338107A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/025—Pretreatment by enzymes or microorganisms, living or dead
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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- Oil, Petroleum & Natural Gas (AREA)
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- Fats And Perfumes (AREA)
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Abstract
The invention discloses the extracting method of mongolian amygdalus seed grease, chooses Prunus Mongolica seeds, sloughs shell；The Prunus Mongolica seeds of crushing are inserted in the phosphate buffer solution that pH is 7.3~7.8 according to 1: 2.5 3.5 solid-liquid ratio；Add n-hexane, 1 1.5%w/w neutral proteinase enzyme preparations are sufficiently stirred；At 35 DEG C~40 DEG C, 1 3h of enzymolysis is stirred continuously, enzyme deactivation vigor is heated, is cooled to room temperature, added n-hexane by 1: 1.5 2.5 solid-liquid ratio, 40min~50min is extracted at a temperature of 75 90 DEG C；Separated again through grease, remove organic solvent and produce.Enzymolysis optimal conditions be neutral proteinase enzyme preparation addition be 1.25%, hydrolysis temperature is 40 DEG C, enzymolysis time 3h, enzymolysis pH value be 7.5.The extraction of biological enzyme formulation degradation and organic solvent is acted on fusion application by the present invention, is reduced production cost, is saved raw material active component, substantially reduce extraction time, improve grease extraction efficiency.
Description
Technical field
The present invention relates to vegetable oil extractive technique field, the specifically extracting method of mongolian amygdalus seed grease.
Background technology
Energy security, ecological safety and food security are to concern happy and peace great and urgent realistic problem.The whole world
When property environmental problem becomes increasingly conspicuous, the renewable bioenergy of the mineral energy such as alternative with serious pollution coal, oil
Cause the highest attention of people.Meanwhile at present, the energy in China 60%, 60% edible oil relies on import, and China's energy is pacified
Entirely, food security constitutes a serious threat.And the mongolian amygdalus seed as China Desert Regions sociales and these realistic problems breath manner of breathing
Close.
Mongolian amygdalus seed (Prunus mongolica Maxim.) is Alashan Desert endemic species, is distributed mainly on China
Desert Regions and the Desert Grasslands such as Alxa, Erdos, Wuhai and Ba Yin nurs.Mongolian amygdalus seed is environmental and economical simultaneous
Some Good Indigenous Tree Species.In ecology, mongolian amygdalus seed is the sociales of Alashan Desert, is that the water and soil of these Desert Regions is protected
Plant and landscape plant are held, extremely important effect is played to this area's Ecological Stabilization.In economic value, mongolian amygdalus seed kind
Benevolence is used as medicine for brush-cherry seed.According to《Compendium of Materia Medica》Record, brush-cherry seed sweetness and bitterness and moisten, its property drop therefore can descend gas Li Shui.The traditional Chinese medical science four passes through greatly
One of allusion quotation works《Sheng Nong's herbal classic》In say：The main extensive abdominal edema of brush-cherry seed, appearance, four limbs edema, diuresis water channel.Modern times doctor
Learn research and show that mongolian amygdalus seed benevolence extract has good protective effect to Hepatic Fibrosis, can significantly reduce
The blood lipid level and resistance lipid peroxidation of hyperlipidemia ratses, and can reduce and the dangerous of angiocardiopathy occur and to liver
It is dirty to play certain protective effect (Wu Tong etc., 2016).Mongolian amygdalus seed medicinal material difference extract is to hyperlipidemia ratses blood fat, fat
Matter peroxidating and liver function have good therapeutic effect (Wu Pei match etc., 2015；Zhao Yunshan etc., 2017).As prescriptions of traditional Chinese medicine
One of medicine composition, mongolian amygdalus seed, which has, treats infant bronchitis (Chinese patent, CN106362019A), habitual constipation (in
State's patent, CN105853649A), clearing lung and eliminating phlegm (Chinese patent, CN103800650A), chronic bronchitis (Chinese patent,
CN106511732A), paranasal sinus bronchus syndrome (Chinese patent, CN105796830A), (China is specially for pemphigus erythematosus
Profit, CN105709110A), clearing lung and eliminating phlegm (Chinese patent, CN105596700A), extravasated blood storage junction type fibroid (Chinese patent,
CN104324330A), qi and blood stagnation brain tumor (Chinese patent, CN104547381A), chronic renal failure (Chinese patent,
CN104984124A), gastritis (Chinese patent, CN104825612A), infantile respiratory tract infection repeatedly (Chinese patent,
CN103041256A), multi-medicament effect such as fever in children high fever respiratory tract infection (Chinese patent, CN103041257A).
The rare oil tree of mongolian amygdalus seed or Desert Regions, its benevolence oil content are up to 40%~54%, belong to grease
The high seeds of content.Mongolian amygdalus seed grease color is golden yellow, as clear as crystal, has distinctive grease fragrance.Containing including ω -3 and
16 kinds of different types of aliphatic acid including ω -6 how unsaturated functional fatty acids, the total degree of unsaturation of aliphatic acid up to 98.16%,
Higher than the olive oil unsaturated fatty acid content for being described as " liquid golden ".Wherein, monounsaturated fatty acids oleic acid content reaches
65.95%, belong to the linoleic acid amount of omega 6 polyunsaturated fatty acid up to 29.97%, belong to the α of omega-3 polyunsaturated fatty acids-
Linolenic acid content is 0.018%.
Too high dietary fat intake can promote the generation of the chronic diseases such as obesity, coronary heart disease, diabetes and tumour, because
And Intake status fatty in meals is always the problem of western countries pay close attention to.In China, with the change of Dietary Pattern of Residents,
The composition of dietary fat intake, food source and aliphatic acid also occurs to change accordingly.As people are recognized diet nutritional
Go deep into, the polyunsaturated fatty acid in dietary fat, especially ω -3 (ω -3-polyunsaturated fatty acid,
ω -3-PUFA) and ω -6 (ω -6-polyunsaturated fatty acid, ω -3-PUFA) polyunsaturated fatty acid it is more next
More pay close attention to.Research finds that these polyunsaturated fatty acids tool is significantly reduced blood fat, cholesterol, reduces the work(of risk of cancer
Effect.Thorsdottir etc. (2004) people confirms that ω -6: the ω -3 ratios height in meals is closely bound up with some diseases occurred frequently,
Such as：When ratio is too high, the diseases such as diabetes, coronary heart disease, breast cancer, colon cancer and prostate cancer are susceptible to suffer from, now supplement linoleic acid
It can alleviate these symptoms with leukotrienes.Research show (2012), intake optimum ratio be present in both, when ratio ω -6: ω -
When 3 ratios are 4~6: 1, human body can play the immunization of maximum potential.The World Health Organization (World Health
Organization, WHO) and FAO (Food and Agriculture Organization of the United Nation) (Food and agriculture organization of the
United nations, FAO) as defined in meals both ratio it is more wide in range, be 5~10: 1.For compatriots' in China
Each side's factor thinks ω -6: ω -3 ratio for 4~6: 1 health (Chinese Soclety of Nutrition, 2006) for being best suitable for Chinese.So
And China's bulk edible oil sunflower oil, peanut oil, rapeseed oil, soybean oil, the ω -3 of Canola oil and ω -6 how unsaturated fat at present
Fat acid content is relatively low, and especially its ω -6 and ω -3 ratios are undesirable.And not only degree of unsaturation is high for xylophyta oil fatty acid,
And different effective components are rich in, increasingly favored by market.
Due to traditional oil tree strong stress resistance, it is not take up ploughing, can once plants and harvest for many years；And seed oil content
Height, it is nutritious, it is pollution-free, most of species have natural anticancer, it is anti-angiogenic hardening etc. health-care effect, be oil-collecting, fruit, medicine,
Material, afforest, view and admire, protecting, the multi-functional seeds that water and soil conservation is integrated, by extensive concern, by some developing countries
Raw material sources of the Devoting Major Efforts To Developing as biodiesel.China still has nearly 1 × 108hm2Waste mountain waste suitable for afforestation, salt-soda soil, sand ground and
Mine, oil field reclaimed land etc. are not suitable for the soil of agro-farming, mostly suitably cultivate specific energy forest oil tree.In view of development wood
Its own strategic significance of this oilseed plant resource, General Office of the State Council's issue in 2015《On accelerating woody oleiferous plants industry hair
The opinion of exhibition》And in No.1 Central File in 2016 all special emphasized development traditional oil tree resource it is urgent with it is important
Property.
Mongolian amygdalus seed grease is rich in vitamin E, Flavonoid substances, amarogentin isoreactivity composition, and oxidation stability is extremely strong,
Exploitation is expected into new " feature edible oil and fat ".Mongolian amygdalus seed oil utilization research is had no into report at present.
Grease extraction process is oilseed plant, the bottle in especially rare wild plant oil resource exploitation and process
Neck factor.It is studied extensively at present mainly to have with oil-producing technique that is applying：Hot milling process, cold milling process, organic solvent lixiviation process,
Supercritical extraction, water substitution and aqueous enzymatic method etc..
Milling process (expression) is acted on by mechanical external force, and grease is squeezed out to the tradition come from oil plant and carries oil
Method, it is divided into hot moulding method and cold-press.Oil plant is crushed in hot moulding method, steams stir-fry, extruding, promotes grease to separate, is domestic
The method generally used of vegetable fat extraction.Cold-press is the technology for producing edible oil and fat by squeezing at a lower temperature.
Its advantage of milling process is to be adapted to the extraction of each vegetable oil, and technological operation is simple, comparision of production safety, is adapted to different vegetable oil
The extraction processing of fat.Shortcoming is that oil cut rate is low, labor intensity is big, low production efficiency, in hot moulding dregs of beans protein mutability, grease
Activity is divided into easily inactivation etc., and its commercial Application is limited, and is unfavorable for the long term growth of enterprise, especially to small-scale special oil
Prepare unsuitable.
Lixiviation process (solvent extraction) is the principle using liquid-solid extraction, and oil plant is soaked by organic solvent
Or backflow makes the technology of oil extraction in oil plant, mainly there is mixed solvent extraction, mixed oil negative pressure evaporation, flash distillation precipitation to extract,
Liquid gas leaching, extraction-refining integrated technique, supercritical gas extraction, it is expanded extraction 7 kinds of methods, be at present in the world
Generally acknowledged more advanced production technology.Its advantage is that labor intensity is low, oil yield is high, and quality is preferable, and protein denaturation degree is small,
It can mass produce.Shortcoming is that extraction time is long, efficiency is low, solvent loss is big, the grease color of extraction is deeper, in grease easily
There is a dissolvent residual, production security is poor, it is difficult to meets requirement of the oil prodution industry to high-quality grease.At present prosperity country and
Area, leaching refining method technique account for more than the 90% of whole liquefaction ability, and leaching refining method technique has accounted for whole liquefaction ability
More than 80%.
Although traditional vegetable oil extracting method such as milling process and organic solvent lixiviation process with higher oil yield,
Most of oil plants need to carry out steaming the heat treatment of stir-fry or baking before squeezing or leaching, oilseed protein is highly denatured, so as to destroy
Its eucaryotic cell structure, reach favourable fuel-displaced condition.Not only step is more, and equipment is complicated, and more important is oil plant to carry albumen after oil
Serious degenerative and utilize difficult, cause the very big wasting of resources.
In recent years to lower production cost, production efficiency is improved, grease extraction efficiency is improved, reduces to grease active ingredient
Destruction, improve product quality, and emerged some new grease extraction processes and technology.
Aqueous enzymatic method (aqueous enzymatic extraction) be with the development of biology enzyme IE and
The new oil extraction process emerged.The method acts on by the selective degradation of enzyme and destroys oilseed eucaryotic cell structure, makes
Grease is discharged, and the purpose for improving oil yield is reached with this.Compared with traditional milling process, organic solvent lixiviation process, its work
Skill is simple, and equipment requirement is low, avoids the residual of destruction and organic solvent of the high temperature to active component so that oil quality is more
It is good, there is the advantages of green, safety, nutrition.
For the method that simultaneously using the grease and protein of oil plant, Sugarman has initiated water extraction vegetable oil for 1956.
On this basis, protease is applied in the water law separation of soybean oil and protein by Olsen in 1981, with enzyme protein degradation matter
Molecule is to discharge grease, so that the yield of soybean oil water extraction is close to 60%.King is superfine to be shown using aqueous enzymatic method research,
Alcalase 2.0L albumen enzyme dosage be 0.02mL/g, solid-to-liquid ratio 1: 6 (m: v), 55 DEG C, pH8.0, hydrolyze 4h under the conditions of, oil tea
Reachable grease extraction efficiency is 78.25%；Sajid Latif etc. (2009) researchs find that the vitamin E in oil obtained by aqueous enzymatic method contains
Amount is high, and removes free radical and suppress linoleic acid peroxidation effect also superior to organic solvent extraction.Yang Hui etc. (2012) compares
The tea oil that milling process, organic solvent lixiviation process, supercritical extraction, aqueous enzymatic method and water substitution are extracted, the results showed that aqueous enzymatic method
There is the intrinsic delicate fragrance of tea oil with the tea oil of water substitution extraction, light yellow in color, clear, its acid value and peroxide value are all than passing
System method is lower, and quality is better than the tea oil of other method extraction, meets country-level food sanitation standard (table 1).
Tea oil quality preservation prepared by the Different Extraction Method of table 1
Aqueous enzymatic method is swift and violent as its development with perfect oil-producing technique is studied.The research of aqueous enzymatic method liquefaction technology and push away
Wide apply is started late in China, but is developed also very fast.At present apricot kernel oil, milk thistle seed kernel oil, peanut oil, rapeseed oil,
Aqueous enzymatic method technical study is applied in vegetable seed oil extract, obtains more satisfied effect.
Enzyme effect effect is relevant with the technique of oil plant cytochemistry compositing characteristic and use.Yi Jianhua etc. have studied neutral egg
White enzyme, medium temperature amylase, pectase and cellulase are used alone and two kinds of compounding uses, 3 kinds of compounding uses are total to walnut kernel
The influence of oil and free oil yield.As a result show, protease is best to free oil yield effect, and cellulase effect is taken second place；Two
During kind enzyme compounding use, up to more than 40%, amylase is answered with cellulase for protease and cellulase compounding free oil yield
It is also preferable with effect；During 3 kinds of enzyme compounding uses, the compounding effect of protease, cellulase and pectase is best, amylase, egg
The compounding effect of white enzyme and cellulase is taken second place；But free oil yield raising is acted on little.At present, aqueous enzymatic method oil-producing technique
Oil yield also certain gap, maximum difficult point compared with traditional handicraft are the separation of oil emulsion and edible vegetable oil.Emulsion is
A kind of complicated fluid, its property are relevant with the interaction between emulsion droplet and the property of drop.Oily work is put forward in aqueous enzymatic method
In skill, it is to prevent or mitigate the formation of emulsion, carry oil to select the compound use of suitable demulsification technology and several enzymes
The key of rate.
Problems be present in exploitation mongolian amygdalus seed oil：
1. mongolian amygdalus seed is oil plant and the medicinal wild woody plants resources having concurrently, it is in short supply in the market to be expected to exploitation
Feature edible oil.But due to limits throughput, it is necessary to retrofit.
2. conventional milling process needs high-temperature process to toast, easily inactivate active component；And organic solvent extraction is a large amount of
Using organic solvent, not only production cost is high, and production security is poor, easily causes the drawbacks such as environmental pollution.Though aqueous enzymatic method
Right extraction conditions are gentle, but for the high raw material of protein content, emulsification is serious, is seriously difficult to separate, recovery rate is not high.
For problem above, aqueous enzymatic method and solvent extraction method are fused into solvent-aqueous enzymatic method, broken using biology enzyme by the present invention
Being broken raw cell structure discharges grease, and extracts grease with a small amount of organic solvent, solves and emulsifies and profit point
From the problem of difficulty, grease extraction efficiency is substantially increased.
The content of the invention
It is an object of the invention to provide the extracting method of mongolian amygdalus seed grease, to solve what is proposed in above-mentioned background technology
Problem.
To achieve the above object, the present invention provides following technical scheme：
The extracting method of mongolian amygdalus seed grease, comprises the following steps：
(1) shell：Prunus Mongolica seeds are chosen, slough shell；
(2) crush：Prunus Mongolica seeds are crushed to 60~80 mesh, then by the Prunus Mongolica seeds of crushing according to 1:
2.5-3.5 solid-liquid ratios are inserted in the phosphate buffer solution that pH is 7.3~7.8；
(3) neutral proteinase enzyme preparation is added：N-hexane is added with 1: 1.5-2.5 solid-liquid ratio, adds 1-1.5%w/w
Neutral proteinase enzyme preparation is sufficiently stirred；
(4) enzyme is degraded：At 35 DEG C~40 DEG C, enzymolysis 1-3h is stirred continuously, is heated to 80 DEG C~90 DEG C, 3~5min enzyme deactivations
Vigor, stop reaction；
(5) oil extraction：Room temperature is cooled to, n-hexane is added by 1: 1.5-2.5 solid-liquid ratio, at a temperature of 75-90 DEG C
Extract 40min~50min；
(6) grease separates：10min~15min is centrifuged under 2000r/min~2400r/min speed, takes supernatant；
(7) organic solvent is removed：Supernatant is depressured into distillation removing organic solvent to produce.
As the further scheme of the present invention：In step (2), solid-liquid ratio 1: 3.
As the further scheme of the present invention：In step (3), solid-liquid ratio 1: 2.
As the further scheme of the present invention：In step (3), enzyme activity/Ug of neutral proteinase enzyme preparation-1：≥
60000。
As the further scheme of the present invention：In step (4), enzymolysis time 2h.
As the further scheme of the present invention：In step (4), enzymolysis pH value is 6.5-8.
As the further scheme of the present invention：In step (4), enzymolysis pH value is 7.
As the further scheme of the present invention：Enzymatic hydrolysis condition is that neutral proteinase enzyme preparation addition is 1.25%, digested
Temperature is 40 DEG C, enzymolysis time 3h, enzymolysis pH value are 7.5.
As the further scheme of the present invention：In step (5), extraction temperature is 85 DEG C.
As the further scheme of the present invention：In step (5), solid-liquid ratio 1: 2.
Compared with prior art, the beneficial effects of the invention are as follows：
The extraction of biological enzyme formulation degradation and organic solvent is acted on fusion application by the present invention, simplifies traditional handicraft
The power consumptions such as heating, baking, the Physical Processing technique for easily causing active component to inactivate, reduce production cost, save raw material
Active component, extraction time is substantially reduced, improve grease extraction efficiency.
The invention has the characteristics that：
It is that the soil-and-water conservation effect of these desert steppes and landscape are planted 1. mongolian amygdalus seed is Alashan Desert constructive species
Thing, it is the maximally effective approach for protecting Desert Regions ecological environment to recover mongolian amygdalus seed population.And increase mongolian amygdalus seed population economy
Value is that enhancing peasants and herdsmen plant mongolian amygdalus seed enthusiasm, recovers the effective ways of mongolian amygdalus seed population.Covered by planting
Ancient almond can reach the purpose to improve People's livelihood with Revegetation of Eco-environment doulbe-sides' victory.
2. mongolian amygdalus seed benevolence fat content is high, and unsaturated fatty acid content is high, containing omega-3 polyunsaturated fatty acids, dimension
The multiple biological activities compositions such as raw plain E, amygdalin, exploitation is expected into high-end edible oil, high-end cosmetics etc..After grease extraction
Leftover bits and pieces in rich in a variety of Peak output compositions, the extraction and application such as activated protein can extend mongolian amygdalus seed industrial chain, can increase
The output value of mongolian amygdalus seed.Solvent-aqueous enzymatic extraction can avoid conventional milling process, the high temperature parch used in organic solvent extraction
Deng loss of the Physical to some active components.
3. due to solvent-aqueous enzymatic method without using high-temperature process, without substantial amounts of organic solvent, extraction time is short, to biology
The advantages that loss of active component is small, recovery rate is of a relatively high, can be considered energy-conservation, safe and environment-friendly, efficient extraction method, and
It is applicable in different scales production, is suitable for the extraction and production of small-scale wild plant grease.
4. mongolian amygdalus seed distributed area is China's ecology Desert Regions the most fragile, it is not suitable for the excessive of underground mineral resources
Utilization, also due to water source extremely shortage, developing agricultural, industry will be seriously restricted.This area is also economical simultaneously
The ethnic group border areas of weak foundation, implement precisely shaking off poverty for the Party Central Committee, the call to improve People's livelihood acquires a certain degree of difficulty.It is woody
Oilseed plant resource, be especially distributed across Desert Regions wild woody plants resources be concern national energy security, grain security and
The grand strategy resource of ecological safety.Therefore, using local wild plant resource, it is to be adapted to work as to develop sand industry, develop the economy
Ground natural environment, and there is great potential.
Brief description of the drawings
Fig. 1 is treatment of different temperature to the influence result figure with n-hexane surname extraction effect.
Fig. 2 is that enzymolysis is preceding added with influence result figure of the solvent sofening treatment to grease extraction effect.
Fig. 3 is the influence result figure for digesting pH to grease extraction efficiency.
Fig. 4 is influence result figure of the enzymolysis time to grease extraction efficiency.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
Solvent-aqueous enzymatic method is also known as aqueous phase enzymolysis organic solvent extractionprocess (The method of aqueous enzymatic
Organic solvent extraction), oil plant carrys out extraction oil in aqueous phase and enzyme effect, addition organic solvent in the method
Fat, then separate aqueous phase and organic phase, organic phase solvent recovered under vacuum obtain grease.The process is divided to two kinds again, Yi Zhongshi
Organic solvent is added in enzymolysis, and enzymolysis and extraction are carried out simultaneously；Another kind is that organic solvent adds after enzymolysis terminates,
It is similar to aqueous enzymatic method, simply employ organic solvent extraction separation method when separating grease.The addition of organic solvent, mainly makes enzyme
The oil dispersed that solution discharges is in in water-insoluble organic phase, to increase the effect for taking oil, while also making oil, albumen and water
(liquid phase) is easier to separate.Grease obtained quality is high, and the grade of edible oil is just can reach without refining or the refining of lower cost
It is required that the lipidated protein of recovery is higher.Aqueous phase digests organic solvent extraction process compared with aqueous enzymatic extraction, due to having
The presence of solvent not only promotes the process of oil plant release grease so that grease is more easy to enter organic phase, and make oil from
More easily separated in albumen and aqueous phase, thus improve oil yield.
Fengyi (Shanghai) Biotechnology Research ＆ Development Center Co., Ltd. is exactly to utilize aqueous phase enzymolysis polar organic solvent extraction work
Skill, ethanol is used as digestion agent while extracts the grease in camellia seed kernel and Tea Saponin.Its experimental arrangement is：5g dry materials are taken,
The polar solvent aqueous solution of a certain amount of various concentrations, shaken well are added respectively.PH=5 is adjusted, adds wet stock weight 2%
Acid protease Novozym25008, be put into water bath with thermostatic control shaking table, mixing speed 150r/min, reaction a period of time.
In V ethanol: V water=1: 2.5, solid-liquid ratio=：1: 4,55 DEG C of reaction temperature, under the conditions of reaction time 1.5h, the single of tea-seed oil
Oil extracting rate 58.9%, 3 total oil extracting rates are 99.82%, while total thick Tea Saponin yield 39.48%.
And the specific embodiment and related experiment of the present invention are as described below.
Embodiment 1
1. in the embodiment of the present invention, the extracting method of mongolian amygdalus seed grease, comprise the following steps：
(1) shell：Prunus Mongolica seeds are chosen, slough shell (endocarp)；
(2) crush：Prunus Mongolica seeds are crushed to 60~80 mesh, then by the Prunus Mongolica seeds of crushing according to 1: 3
Solid-liquid ratio is inserted in the phosphate buffer solution that pH is 7.3~7.8；
(3) enzyme preparation is added：N-hexane is added with 1: 2 solid-liquid ratio, adds 1.25%w/w neutral proteinases
(Solarbio companies, code name：SoMZD-1, enzyme activity/Ug-1：>=60 000) enzyme preparation be sufficiently stirred；
(4) enzyme is degraded：At 35 DEG C~40 DEG C, enzymolysis 1-3h is stirred continuously, 80 DEG C~90 DEG C 3~5min enzyme deactivations is heated and lives
Power, stop reaction；
(5) oil extraction：Room temperature is cooled to, n-hexane is added by 1: 2 solid-liquid ratio, is being extracted at a temperature of 75-90 DEG C
40min~50min；
(6) grease separates：10min~15min is centrifuged in 2000r/min~2400r/min, takes supernatant；
(7) organic solvent is removed：Decompression distillation removes organic solvent and obtains edible vegetable oil；
(8) now disposable recovery rate is 52.54%.
2. the optimizing research of experiment condition
This experimental result is to carry out multinomial single experiment result orthogonal experiment optimization acquired results.
Referring to Fig. 1, with soxhlet extraction in different temperatures extraction results such as Fig. 1.Show it is optimal in 85 DEG C of effect of extracting,
Oil content is up to 52.5%.
Referring to Fig. 2, addition organic solvent makes raw material sofening treatment contribute to the contact of enzyme-to-substrate before enzymolysis, enzyme is improved
Effect is solved, is released grease, so as to improve recovery rate.
As can be known from Fig. 3, the recovery rate highest when digesting pH and being 7, is secondly pH=7.5 up to 47.39%.
Referring to Fig. 4, enzymolysis time has 1h to increase to 2h, 7 percentage points of grease extraction efficiency increase increase, but extend again then
Grease extraction efficiency declines again.
Every combined factors are considered, carry out orthogonal experiment, as a result as shown in table 2.
The neutral proteinase of table 2 pre-processes Orthogonal experiment results
On the basis of above-mentioned neutral protease enzymolysis condition experiment of single factor, to enzyme addition, enzymolysis temperature in enzymolysis process
4 factors such as degree, enzymolysis time and enzymolysis pH value carry out L9(34) orthogonal experiment, using grease extraction efficiency as par index, to solvent
The pretreatment extraction of aqueous enzymatic method neutral proteinase carries out process optimization.(Orthogonal experiment results such as table 2)
It is big from table 2 and further variance analysis, influence of four factors of neutral protease enzymolysis to grease extraction efficiency
It is small to be followed successively by B (hydrolysis temperature) ＞ A (enzyme addition) ＞ D (enzymolysis pH value) ＞ C (enzymolysis time), optimum combination A2B1C2D3,
I.e. enzymolysis optimal conditions be enzyme addition be 1.25%, hydrolysis temperature is 40 DEG C, enzymolysis time 3h, enzymolysis pH value be 7.5,
Confirmatory experiment is carried out under this optimal conditions, obtains grease extraction efficiency as 52.54%.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
It is appreciated that other embodiment.
Claims (10)
1. the extracting method of mongolian amygdalus seed grease, it is characterised in that comprise the following steps：
(1) shell：Prunus Mongolica seeds are chosen, slough shell；
(2) crush：Prunus Mongolica seeds are crushed to 60~80 mesh, then by the Prunus Mongolica seeds of crushing according to 1: 2.5-
3.5 solid-liquid ratios are inserted in the phosphate buffer solution that pH is 7.3~7.8；
(3) neutral proteinase enzyme preparation is added：N-hexane is added with 1: 1.5-2.5 solid-liquid ratio, adds 1-1.5%w/w neutrality
Protease enzyme preparation is sufficiently stirred；
(4) enzyme is degraded：At 35 DEG C~40 DEG C, enzymolysis 1-3h is stirred continuously, is heated to 80 DEG C~90 DEG C, 3~5min enzyme deactivation vigor,
Stop reaction；
(5) oil extraction：Room temperature is cooled to, n-hexane is added by 1: 1.5-2.5 solid-liquid ratio, is extracted at a temperature of 75-90 DEG C
40min~50min；
(6) grease separates：10min~15min is centrifuged under 2000r/min~2400r/min speed, takes supernatant；
(7) organic solvent is removed：Supernatant is depressured into distillation removing organic solvent to produce.
2. the extracting method of mongolian amygdalus seed grease according to claim 1, it is characterised in that in step (2), solid-liquid ratio is
1∶3。
3. the extracting method of mongolian amygdalus seed grease according to claim 1, it is characterised in that in step (3), solid-liquid ratio is
1∶2。
4. the extracting method of mongolian amygdalus seed grease according to claim 1, it is characterised in that in step (3), neutral protein
Enzyme activity/Ug of enzyme enzyme preparation-1：≥60 000.
5. the extracting method of mongolian amygdalus seed grease according to claim 1, it is characterised in that in step (4), enzymolysis time
For 2h.
6. the extracting method of mongolian amygdalus seed grease according to claim 1, it is characterised in that in step (4), digest pH value
For 6.5-8.
7. the extracting method of mongolian amygdalus seed grease according to claim 6, it is characterised in that in step (4), digest pH value
For 7.
8. the extracting method of mongolian amygdalus seed grease according to claim 1, it is characterised in that enzymatic hydrolysis condition is neutral protein
Enzyme enzyme preparation addition is 1.25%, hydrolysis temperature is 40 DEG C, enzymolysis time 3h, enzymolysis pH value are 7.5.
9. the extracting method of mongolian amygdalus seed grease according to claim 1, it is characterised in that in step (5), extraction temperature
For 85 DEG C.
10. the extracting method of mongolian amygdalus seed grease according to claim 1, it is characterised in that in step (5), solid-liquid ratio
For 1: 2.
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