CN108546591A - A kind of preparation method of selenium-rich tea oil - Google Patents
A kind of preparation method of selenium-rich tea oil Download PDFInfo
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- CN108546591A CN108546591A CN201810357037.8A CN201810357037A CN108546591A CN 108546591 A CN108546591 A CN 108546591A CN 201810357037 A CN201810357037 A CN 201810357037A CN 108546591 A CN108546591 A CN 108546591A
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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
- 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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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/007—Other edible oils or fats, e.g. shortenings, cooking oils characterised by ingredients other than fatty acid triglycerides
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
- A23D9/04—Working-up
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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
- C11B3/00—Refining fats or fatty oils
- C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
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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
- C11B3/00—Refining fats or fatty oils
- C11B3/10—Refining fats or fatty oils by adsorption
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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
- C11B3/00—Refining fats or fatty oils
- C11B3/12—Refining fats or fatty oils by distillation
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- Polymers & Plastics (AREA)
- Medicines Containing Plant Substances (AREA)
- Edible Oils And Fats (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
A kind of preparation method of selenium-rich tea oil disclosed by the invention, is related to biological medicine and food processing technology field, technological process is as follows：(1), crude oil is handled：1., crude oil selection；2., decoloration；3., deodorization；4., membrane filtration；(2), prepared by selenium-rich powder：1., impregnate；2., primary drying；3., primary crush；4., enzymolysis；5., redrying；6., separating twice；(3), miscible；(4), extract；(5), distill；(6), column is filtered；(7), wash；(8), refined filtration.Using the selenium-rich tea oil prepared by the present invention, has the characteristics that not only to remain the activity of target component in tea oil but also eliminate useless or harmful impurity and be rich in selenium element, be suitble to the people of each ages edible, it is edible to be especially suitable for the middle-aged and the old.
Description
Technical field
The present invention relates to biological medicine and food processing technology field, especially a kind of preparation method of selenium-rich tea oil.
Background technology
Oil tea is distinctive woody with four big traditional oil tree of the world of oil palm, olive, coconut and title and China
Oil plant.The comprehensive utilization value of oil tea is very high, contains many bioactive substances, such as vitamin E, tea polyphenols, squalene pair
The beneficial active material of human body.
Selenium element is respectfully called " kindling material of life " by domestic and international the world of medicine and nutrition educational circles, enjoys " long-lived element ", " anticancer
King ", the good reputations such as " heart patron saint " and " natural antidote "；Selenium content in tissue is thousand a ten thousandths, but it
The presence for determining life, the great function to human health are that other substances are irreplaceable；Selenium deficiency can directly result in human body
Immunocompetence declines, and clinical medicine proves, threatens more than 40 kinds of disease of human health and life all related with human body selenium deficiency, such as
Cancer, cardiovascular disease, hepatopathy, cataract, pancreatic disease, diabetes, genital system diseases etc..
In common edible oil and fat, the content of selenium is few.In recent years, occur some by special implantation methods come
The selenium element content in grease is improved, there are also by special preparation method, it is higher edible to obtain selenium element content
Grease.
" a kind of selenium-rich tea oil and its preparation side as disclosed in Chinese patent (number of patent application 201210137102.9)
Method " is prepared by the ginseng 5-10 of weight percent, peanut 1-5, purple sweet potato 1-8, garlic 1-5, oat 1-10 and tea seed 65-80
It forms, preparation process is：Stock, water carry, alcohol extracting, drying, squeezing, alkali cleaning, absorption, filtering, extraction is to get selenium-rich tea oil；
Its product has the characteristics that, rich in selenium element and various health care functions, selenium-rich tea oil of the invention, to be suitble to each ages
People are edible, and it is edible to be especially suitable for the middle-aged and the old.
Another Chinese patent (number of patent application 201610671691.7) is disclosed " a kind of selenium-rich tea oil and its to prepare work
Skill ", the selenium-rich tea oil are grouped as by the group of following parts by weight：150-200 parts of tea seed, 5-10 parts of Organic Selenium, 8-15 parts of Poria cocos,
7-9 parts of fructus amomi, 4-6 parts of hawthorn, 3-5 parts of spina date seed, 7-11 parts of Radix Angelicae Sinensis, 5-8 parts of Radix Notoginseng, 1-3 parts of chrysanthemum, 2-4 parts of elephants-foot, water
30-50 parts and 10-20 parts of edible alcohol.Preparation method letter preparation process of the present invention is simple, and selenium element content is higher, can meet people
Demand to selenium element, reduce the probability that people obtain the symptoms such as cancer, cardiovascular disease, hepatopathy, cataract, pancreatic disease,
Improve the health of people.
Also " a kind of selenium-rich tea oil " disclosed in Chinese patent (number of patent application 201710590966.9), raw material is pressed
Parts by weight include：400-650 parts of selenium-rich tea seed, 100-150 parts of Se-rich lucid ganoderma, 100-150 parts of selenium-rich Semen sesami nigrum, product containing organic selenium
100-150 parts, 10-20 parts of black soya bean, 10-20 parts of blackcurrant pigment, 10-20 parts of black rice, 5-35 parts of asparagus, 1-8 parts of ginseng, Rhizoma Atractylodis Macrocephalae 5-15
Part, 5-15 parts of Poria cocos, 1-9 parts of Radix Paeoniae Alba, 5-15 parts of dark plum, 6-18 parts of butterflybush flower, 10-20 parts of Radix Angelicae Sinensis, 700-1000 parts of selenium-rich water,
5-15 parts of longan.In the present invention, selenium-rich tea seed, Se-rich lucid ganoderma, selenium-rich Semen sesami nigrum, the product containing organic selenium added all has rich
Rich selenium element, and black soya bean, blackcurrant pigment, black rice, asparagus, ginseng, Rhizoma Atractylodis Macrocephalae, Poria cocos, Radix Paeoniae Alba, dark plum, butterflybush flower, Radix Angelicae Sinensis, osmanthus
Circle etc. has nourishing the stomach, health care, strong kidney function effect, can enhance immunocompetence of the body to nonspecific stimulation.
Invention content
It can retain in tea oil the activity of target component the purpose of the present invention is to provide a kind of but also reject useless or have
The processing method of harmful impurity and the tea oil rich in selenium element.
To achieve the above object, the technical measures that the present invention is taken are to invent a kind of preparation method of selenium-rich tea oil,
Technological process is as follows：
(1), crude oil is handled：
1., crude oil selection：Acid value is selected to be less than 1.0, through being cold-pressed the tea seed crude oil of squeezing method preparation as oil-tea camellia seed crude oil；
2., decoloration：Oil-tea camellia seed crude oil is heated to 80-100 DEG C (rate of heat addition is 1-3 DEG C/min), then passes through wriggling
Pump (power of peristaltic pump is 4-5L/min) is pumped into decolorizing column, is allowed oil-tea camellia seed crude oil to flow downward naturally along decolorizing column, is collected
The decoloration oil-tea camellia seed crude oil of outflow；
3., deodorization：Will decoloration oil-tea camellia seed crude oil be heated to 150-180 DEG C (rate of heat addition be 10-18 DEG C/min, and often on
30 DEG C are risen, 10-15min is stirred by 300-600r/min), the activity for accounting for decoloration oil-tea camellia seed crude oil weight 10-24% is then added
Charcoal, when stir process is to 1.2-1.8h, addition accounts for decoloration oil-tea camellia seed crude oil weight 20-35%, weight concentration is in 4-8.5%
Property saline solution (one kind in sodium chloride, potassium chloride, sodium sulphate, potassium sulfate), be stirred for processing 20-40min, then it is quiet put to
Layering is apparent, and filters out neutral saline solutions and activated carbon using separatory funnel separator while hot；Thereafter, add account for it is de-
Color oil-tea camellia seed crude oil weight 15-24%, the edible ethanol solution that volume solubility is 30-38%, stir process 20-30min are quiet
It sets, when being naturally cooling to 70 DEG C, ethanol solution is filtered out using separatory funnel separator while hot；Then it is naturally cooling to room
Temperature, filtering (filter membrane that aperture is 10-20 microns), obtains deodorization oil-tea camellia seed crude oil；
4., membrane filtration：Deodorization oil-tea camellia seed crude oil is transferred in freezer, when it is cooled to 10 DEG C or less, is in pressure
Under 1.2-1.85MPa, through permeable membrane device circulating filtration 2.5-3.5h, the membrane filtration oil-tea camellia seed crude oil that last time filters out is collected,
It is spare；
(2), prepared by selenium-rich powder：
1., impregnate：Clean dry squid is placed in 30 degree or more of white wine, impregnates 2-3 days, pull out, drain；It retransfers
To in pure vinegar, 10-20h is impregnated under room temperature, is pulled out, is drained；Then it is placed in boiling water, 1.5-3.5h is boiled in boiling, must impregnate squid；
2., primary drying：Squid will be impregnated to be transferred in normal pressure baking oven, dried to moisture at 60-70 DEG C and be less than 5%, obtained
Dry squid；
3., primary crush：Dry squid is processed into the squid fine powder of 80 mesh or more；
4., enzymolysis：1-2 times of weight is first added into squid fine powder, the warm water that temperature is 36-48 DEG C, stirs evenly, add and account for
The lipase of squid fine powder weight 0.5-0.75%, the cellulase of 0.2-0.4%, mixing seal stir process 30-45h, stir
It is 30-40r/10min, filtering to mix rate；The protein excision enzyme for accounting for former squid fine powder weight 1.2-1.8% is added, in 26-
Constant temperature stir process 10-24h at 45 DEG C, stir speed (S.S.) 10-25r/min, then be added account for former 1-2 times of squid fine powder weight,
Mass fraction is in weak base (sodium carbonate or sodium bicarbonate) aqueous solution of 0.2-0.8%, the constant temperature stir process 20- at 65-80 DEG C
40min, filtering (aperture is 0.5-1 micron membrane filters), obtains enzymatic treatment squid powder；
5., redrying：Enzymatic treatment squid powder is transferred in normal pressure baking oven, dries to moisture and is less than at 60-70 DEG C
5%, obtain redrying squid powder；
6., separating twice：Redrying squid powder is processed into fine powder of the grain size less than 0.1 micron to get richness through ultra micro
Selenium squid powder (Se content is more than 2000 μ g/kg), it is spare；
(3), miscible：By selenium-rich squid powder and account for the edible surface activating agent of selenium-rich squid powder weight 0.2-1.2% is (big
One kind in Fabaceous Lecithin, sodium alginate, glycine betaine) it stirs evenly under room temperature, then will account for the membrane filtration of 6-10 times of selenium-rich squid powder weight
Oil-tea camellia seed crude oil is added, and stirs evenly, is then heated to 60-70 DEG C, ground machine constant temperature milled processed 2.0-3.5h；It is then heated to
90-110 DEG C (rate of heat addition is 5-8 DEG C/min), transfers to and carries out oscillation treatment in oscillator, and decline with oil temperature and change
Frequency of oscillation：70 DEG C of period, frequency of oscillation 800-1000Hz are dropped in oil temperature；In oil temperature 50 DEG C are dropped to by 70 DEG C
Period, frequency of oscillation is changed to 600-700Hz, and is added and accounts for membrane filtration oil-tea camellia seed crude oil weight 5-8%, mass concentration 3-
4.5%, 50 DEG C of neutral brine (one kind in sodium chloride, potassium chloride, sodium sulphate, potassium sulfate)；It is dropped to by 50 DEG C in oil temperature
The period of room temperature, frequency of oscillation is changed to 200-300Hz, and is added and accounts for former selenium-rich squid powder weight 1-1.5%, pH value 4.0
Aqueous citric acid solution；It is quiet to put to layering after oscillation treatment, it is filtered using separatory funnel separator, collects oil reservoir, obtain selenium-rich
Oil-tea camellia seed crude oil；
(4), extract：Selenium-rich oil-tea camellia seed crude oil is transferred in extraction container, the butane solvent of 2-3 times of weight is added, in room
Lower stirring extraction 1-3 times, stir speed (S.S.) 150-180r/min of temperature, stands, layering, then uses separatory funnel separator mistake
Butane extract liquor is collected in filter, spare；
(5), distill：Butane extract liquor is transferred in destilling tower, is first distilled at pressure 20-28KPa, 70-78 DEG C of temperature
It is flowed out to no liquid；It is added again into tower and accounts for selenium-rich oil-tea camellia seed crude oil weight 15-22%, the ethyl alcohol that volumetric concentration is 40-48%
Aqueous solution, distillation to no liquid flows out at pressure 5-10KPa, 90-110 DEG C of temperature；Then, remaining steaming in destilling tower is collected
Evaporate oil-tea camellia seed crude oil；
(6), column is filtered：Oil-tea camellia seed crude oil constant temperature will first be distilled to 40-50 DEG C, then (power of peristaltic pump is 2- by peristaltic pump
It 2.8L/min) is pumped into Filter column, so that distillation oil-tea camellia seed crude oil is flowed downward naturally along Filter column, collect the column oil strain tea of outflow
Seed crude oil；
(7), wash：It is filtered to column and 1-2.5 times of weight is added in oil-tea camellia seed crude oil, temperature is 60-70 DEG C, mass fraction is
The sodium bicarbonate or aqueous sodium carbonate of 0.1-0.25%, stir process 2-3h, stir speed (S.S.) 500-600r/min are then quiet
It puts to temperature and is down to room temperature, first use aperture 0.1-0.5 microns of membrane filtration, then filtered with separatory funnel separator, receive
Collection washing oil-tea camellia seed crude oil；
(8), refined filtration：Washing oil-tea camellia seed crude oil is filtered in the case where pressure is 1.5-2.5MPa through ultra-filtration membrane device, collection filters out
Fluid to get selenium-rich tea oil.
Decolorizing column in the decolorization process is to be prepared as follows：It is 80-120 purposes by the mesh number handled well
Silica decoloration sand and the quartz sand of 40-80 mesh press 1：The ratio mixing dress column of 2-2.5, dress pillar height degree is the 40-50% of pillar height.
Decolorizing column in the decolorization process is to be prepared as follows：By the silicon that the mesh number handled well is 100 mesh
The quartz sand of glue decoloration sand and 60 mesh presses 1：2.2 ratio mixing dress column, dress pillar height degree is the 45% of pillar height.
In permeable membrane device in the membrane filtration step, the specification of permeable membrane is that molecular weight is only allowed to be 500-1000
Substance pass through.
Filter column in the column filters step is to be prepared as follows：It is 80-120 mesh by the mesh number handled well
The quartz sand of silica decoloration sand and 40-80 mesh press 1：The ratio mixing dress column of 5-7, dress pillar height degree is the 40-50% of pillar height.
Filter column in the column filters step is to be prepared as follows：It is 100 purposes by the mesh number handled well
The quartz sand of silica decoloration sand and 60 mesh presses 1：6 ratio mixing dress column, dress pillar height degree is the 45% of pillar height.
In ultra-filtration membrane device in the refined filtration step, the specification of ultrafiltration membrane is only to allow molecular weight less than 2000
Substance passes through.
Activated carbon in the deodorising step is handled as follows：The activated carbon of 20-40 mesh is first put into body
In the ethanol solution of product concentration 60-70%, weight ratio between the two is activated carbon：Ethanol solution=1：6-8, in 60-65
30-45min is stirred at DEG C；It adds and accounts for activated carbon weight 0.2-1.45%, the phosphoric acid solution that mass fraction is 10-15%, stir
It mixes；Then, it every the phosphoric acid solution that the 2-5% for accounting for above-mentioned volumes of aqueous ethanol is added in 15min, mass fraction is 10-15%, stirs
It mixes, is added 3 times altogether, filtering obtains alcohol treatment activated carbon；Then it is added into alcohol treatment activated carbon and accounts for former activated carbon weight 2-
3 times, the aqueous alkali that mass fraction is 1.2-3.4%, the stir process 30-40min at 4-10 DEG C, filtering obtain alkali process work
Property charcoal；Alkali process activated carbon is dried to 10-15h under 100-110 DEG C, normal pressure again to get the activated carbon in deodorising step.
The present invention selenium-rich tea oil preparation method, by add selenium-rich raw material, and using crude oil processing (including crude oil choosing
Select, decolourize, being deodorized, membrane filtration), selenium-rich powder prepare (including immersion, primary drying, primary crushing, redrying, separating twice),
This unique processing technology such as miscible, extraction, distillation, column filter, washing and refined filtration, is effectively rejecting crude oil and selenium-rich raw material
In useless or harmful impurity while, remain the activity of target component in raw material tea oil, and be relatively enriched with and improve
The content of selenium element in finished product tea oil, a large amount of monounsaturated fatty acids, unsaturated fat are also contained in finished product tea oil in addition
The beneficial active material of all multipair human bodies such as acid, vitamin E, Tea Saponin, squalene and Flavonoid substances, thus, have a variety of
Healthcare function.
Following table 1 is the effective ingredient detection data (content of 100g) of the selenium-rich tea oil prepared using the present invention：
Table 1
It can be seen that the selenium-rich tea oil prepared using the present invention from the data of table 1 above, not only its selenium element content is very high
(reaching 382.6 micrograms per hectogram amount), moreover, being also rich in unsaturated fatty acid and monounsaturated fatty acids and many right
The beneficial trace element of human body.
Specific implementation mode
With reference to embodiments, the present invention is further illustrated.Following explanation is but this hair in a manner of enumerating
Bright protection domain is not limited thereto.
The preparation method of the selenium-rich tea oil of the present embodiment, preparation process are as follows：
The preparation method of selenium-rich tea oil, technological process are as follows：
(1), crude oil is handled：
1., crude oil selection：Acid value is selected to be less than 1.0, through being cold-pressed the tea seed crude oil of squeezing method preparation as oil-tea camellia seed crude oil；
2., decoloration：First by the quartz sand of silica decoloration sand and 60 mesh that the mesh number handled well is 100 mesh by 1：2.2 ratio
Example mixing dress column, dress pillar height degree is the 45% of pillar height；Then, by oil-tea camellia seed crude oil be heated to 90 DEG C (rate of heat addition be 1-3 DEG C/
Min), then by peristaltic pump (power of peristaltic pump be 4.5L/min) be pumped into decolorizing column, allow oil-tea camellia seed crude oil along decolorizing column from
It so flows downward, collects the decoloration oil-tea camellia seed crude oil of outflow；
3., deodorization：First the activated carbon of 30 mesh is put into the ethanol solution of volumetric concentration 65%, weight ratio between the two
Example is activated carbon：Ethanol solution=1：7,40min is stirred at 62 DEG C, adds and accounts for activated carbon weight 1%, mass fraction is
12% phosphoric acid solution, stirring；Then, above-mentioned volumes of aqueous ethanol 4%, phosphoric acid same as described above are accounted for every 15min additions
Solution, stirring；It is added 3 times altogether, filtering (using centrifuge filtering more than 800 mesh of filter bag aperture) obtains alcohol treatment activated carbon；
Then the sodium hydroxide that addition accounts for 2.5 times of former activated carbon weight into alcohol treatment activated carbon, mass fraction is 2.5% is water-soluble
Liquid, the stir process 35min at 7 DEG C, filtering (using centrifuge filtering more than 800 mesh of filter bag aperture) obtain alkali process activity
Charcoal；Alkali process activated carbon is dried to 12h under 105 DEG C, normal pressure again, obtains processing activated carbon；It again will decoloration oil-tea camellia seed crude oil heating
To 160 DEG C (rate of heat addition is 15 DEG C/min, and often rises 30 DEG C, and 12min is stirred by 450r/min), then it is added and accounts for bleached oil
The processing activated carbon of tea seed crude oil weight 18%, when stir process (stir speed (S.S.) 25r/min) is to 1.2-1.8h, addition accounts for de-
Color oil-tea camellia seed crude oil weight 28%, weight concentration be 6.5% sodium-chloride water solution, handle 30min, then it is quiet put to be layered it is bright
It is aobvious, and sodium-chloride water solution and activated carbon are filtered out using separatory funnel separator while hot；Thereafter, it adds and accounts for decoloration oil tea
Seed crude oil weight 20%, the edible ethanol solution that volume solubility is 35%, stir process 25min stand, wait being naturally cooling to 70
DEG C when, ethanol solution is filtered out using separatory funnel separator while hot；Then it is naturally cooling to room temperature, filters (aperture 10-
20 microns of filter membrane), obtain deodorization oil-tea camellia seed crude oil；
4., membrane filtration：Deodorization oil-tea camellia seed crude oil is transferred in freezer, when it is cooled to 10 DEG C or less, is in pressure
Under 1.5MPa, through permeable membrane device (specification of permeable membrane is only the substance that molecular weight is 500-1000 to be allowed to pass through) circulating filtration
3h collects the membrane filtration oil-tea camellia seed crude oil that last time filters out, spare；
(2), prepared by selenium-rich powder：
1., impregnate：Clean dry squid is placed in 35 degree of white wine, impregnates 2.5 days, pull out, drain；It transfers to pure
In vinegar, 15h is impregnated under room temperature, is pulled out, is drained；Then it is placed in boiling water, 2.5h is boiled in boiling, must impregnate squid；
2., primary drying：Squid will be impregnated to be transferred in normal pressure baking oven, dried to moisture at 65 DEG C and be less than 5%, obtain drying
Squid；
3., primary crush：Dry squid is processed into the squid fine powder of 80 mesh or more；
4., enzymolysis：1.5 times of weight are first added into squid fine powder, the warm water that temperature is 40 DEG C, stir evenly, add and account for squid
0.6% lipase of fish fine powder weight, 0.3% cellulase, mixing seal stir process 38h, stir speed (S.S.) 35r/
10min, filtering；Add the protein excision enzyme for accounting for former squid fine powder weight 1.5%, the constant temperature stir process 18h at 35 DEG C,
Stir speed (S.S.) is 18r/min, and it is water-soluble in 0.5% sodium carbonate to account for former 1.5 times of squid fine powder weight, mass fraction for then addition
Liquid, the constant temperature stir process 30min at 70 DEG C, filtering (filter membrane that aperture is 0.5-1 microns) obtain enzymatic treatment squid powder；
5., redrying：Enzymatic treatment squid powder is transferred in normal pressure baking oven, is dried to moisture at 65 DEG C and is less than 5%, obtained
Redrying squid powder；
6., separating twice：Redrying squid powder is processed into fine powder of the grain size less than 0.1 micron to get richness through ultra micro
Selenium squid powder (Se content is more than 2000 μ g/kg), it is spare；
(3), miscible：By selenium-rich squid powder with account for and will be stirred evenly under the soybean lecithin room temperature of selenium-rich squid powder weight 0.7%, then
The membrane filtration oil-tea camellia seed crude oil of 8 times of selenium-rich squid powder weight is added by accounting for, stirs evenly, is then heated to 65 DEG C, ground machine constant temperature
Milled processed 2.8h；100 DEG C (rate of heat addition is 7 DEG C/min) are then heated to, transfers to and carries out oscillation treatment in oscillator,
And declines with oil temperature and change frequency of oscillation：70 DEG C of period, frequency of oscillation 900Hz are dropped in oil temperature；Oil temperature by
70 DEG C of periods for dropping to 50 DEG C, frequency of oscillation are changed to 650Hz, and are added that account for membrane filtration oil-tea camellia seed crude oil weight 6%, quality dense
The sodium-chloride water solution that degree is 4%, 50 DEG C；In the period that oil temperature drops to room temperature by 50 DEG C, frequency of oscillation is changed to 250Hz,
And it is added and accounts for former selenium-rich squid powder weight 1.2%, the aqueous citric acid solution that pH value is 4.0；It is quiet to put to layering after oscillation treatment,
It is filtered using separatory funnel separator, collects oil reservoir, obtain selenium-rich oil-tea camellia seed crude oil；
(4), extract：Selenium-rich oil-tea camellia seed crude oil is transferred in extraction container, the butane solvent of 2.5 times of weight is added, in room
The lower stirring extraction 2 times, stir speed (S.S.) 160r/min of temperature, stands, layering, then separatory funnel separator is used to filter, receive
Collect butane extract liquor, it is spare；
(5), distill：Butane extract liquor is transferred in destilling tower, is first distilled to aneroid at pressure 25KPa, 75 DEG C of temperature
Body flows out；It is added again into tower and accounts for selenium-rich oil-tea camellia seed crude oil weight 18%, the ethanol water that volumetric concentration is 45%, in pressure
Distillation to no liquid flows out at 8KPa, 100 DEG C of temperature；Then, remaining distillation oil-tea camellia seed crude oil in destilling tower is collected；
(6), column is filtered：First by the quartz sand of silica decoloration sand and 60 mesh that the mesh number handled well is 100 mesh by 1：6 ratio
Mixing dress column is (i.e.：Filter column), dress pillar height degree is the 45% of pillar height；Then, by distillation oil-tea camellia seed crude oil constant temperature to 45 DEG C, then lead to
It crosses peristaltic pump (power of peristaltic pump is 2.5L/min) to be pumped into Filter column, keeps distillation oil-tea camellia seed crude oil naturally downward along Filter column
The column filter oil-tea camellia seed crude oil of outflow is collected in flowing；
(7), wash：It is filtered to column and 1.8 times of weight is added in oil-tea camellia seed crude oil, temperature is 65 DEG C, mass fraction is 0.18%
Sodium bicarbonate aqueous solution, stir process 2.5h, stir speed (S.S.) 550r/min, then quiet put to temperature be down to room temperature, first use
The membrane filtration that 0.3 micron of aperture, then filtered with separatory funnel separator, collect washing oil-tea camellia seed crude oil；
(8), refined filtration：Washing oil-tea camellia seed crude oil is filtered into (the rule of its ultrafiltration membrane in the case where pressure is 1.8MPa through ultra-filtration membrane device
Lattice are that substance of the molecular weight less than 2000 is only allowed to pass through), the fluid filtered out is collected to get selenium-rich tea oil.
Using selenium-rich tea oil prepared by the present invention, it is suitble to the people of each ages edible, is especially suitable for the middle-aged and the old
It is edible.
Claims (8)
1. a kind of preparation method of selenium-rich tea oil, which is characterized in that technological process is as follows：
(1), crude oil is handled：
1., crude oil selection：Acid value is selected to be less than 1.0, through being cold-pressed the tea seed crude oil of squeezing method preparation as oil-tea camellia seed crude oil；
2., decoloration：Oil-tea camellia seed crude oil is heated to 80-100 DEG C, is then pumped into decolorizing column by wriggling, allows tea seed hair
Oil flows downward naturally along decolorizing column, collects the decoloration oil-tea camellia seed crude oil of outflow；
3., deodorization：Decoloration oil-tea camellia seed crude oil is heated to 150-180 DEG C, is then added and accounts for decoloration oil-tea camellia seed crude oil weight 10-
24% activated carbon, when stir process is to 1.2-1.8h, addition accounts for decoloration oil-tea camellia seed crude oil weight 20-35%, weight concentration is
The neutral saline solutions of 4-8.5% are stirred for processing 20-40min, then quiet to put to layering obviously, and use liquid separation to leak while hot
Bucket separator filters out neutral saline solutions and activated carbon；Thereafter, add account for decoloration oil-tea camellia seed crude oil weight 15-24%,
Volume solubility is the edible ethanol solution of 30-38%, and stir process 20-30min is stood, when being naturally cooling to 70 DEG C, while hot
Ethanol solution is filtered out using separatory funnel separator；Then it is naturally cooling to room temperature, filters, obtains deodorization oil-tea camellia seed crude oil；
4., membrane filtration：Deodorization oil-tea camellia seed crude oil is transferred in freezer, is 1.2- in pressure when it is cooled to 10 DEG C or less
Under 1.85MPa, through permeable membrane device circulating filtration 2.5-3.5h, the membrane filtration oil-tea camellia seed crude oil that last time filters out is collected, it is spare；
(2), prepared by selenium-rich powder：
1., impregnate：Clean dry squid is placed in 30 degree or more of white wine, impregnates 2-3 days, pull out, drain；It transfers to pure
In vinegar, 10-20h is impregnated under room temperature, is pulled out, is drained；Then it is placed in boiling water, 1.5-3.5h is boiled in boiling, must impregnate squid；
2., primary drying：Squid will be impregnated to be transferred in normal pressure baking oven, dried to moisture at 60-70 DEG C and be less than 5%, obtain drying
Squid；
3., primary crush：Dry squid is processed into the squid fine powder of 80 mesh or more；
4., enzymolysis：1-2 times of weight is first added into squid fine powder, the warm water that temperature is 36-48 DEG C, stirs evenly, add and account for squid
The lipase of fine powder weight 0.5-0.75%, the cellulase of 0.2-0.4%, mixing seal stir process 30-45h, filtering；
The protein excision enzyme for accounting for former squid fine powder weight 1.2-1.8% is added, the constant temperature stir process 10-24h at 26-45 DEG C,
Then it is added and accounts for former 1-2 times of squid fine powder weight, mass fraction in the weak base aqueous solution of 0.2-0.8%, the constant temperature at 65-80 DEG C
Stir process 20-40min, filtering, obtains enzymatic treatment squid powder；
5., redrying：Enzymatic treatment squid powder is transferred in normal pressure baking oven, is dried to moisture at 60-70 DEG C and is less than 5%, obtained
Redrying squid powder；
6., separating twice：Redrying squid powder is processed into fine powder of the grain size less than 0.1 micron to get selenium-rich squid through ultra micro
Fish meal, it is spare；
(3), miscible：By selenium-rich squid powder with account for and will be stirred under the edible surface activating agent room temperature of selenium-rich squid powder weight 0.2-1.2%
It is even, then the membrane filtration oil-tea camellia seed crude oil of 6-10 times of selenium-rich squid powder weight is added by accounting for, it stirs evenly, is then heated to 60-70 DEG C, it is permanent
Warm milled processed 2.0-3.5h；It is then heated to 90-110 DEG C, transfers to and carries out oscillation treatment in oscillator, and under oil temperature
It drops and changes frequency of oscillation：70 DEG C of period, frequency of oscillation 800-1000Hz are dropped in oil temperature；In oil temperature by 70 DEG C
It is down to 50 DEG C of period, frequency of oscillation is changed to 600-700Hz, and is added that account for membrane filtration oil-tea camellia seed crude oil weight 5-8%, quality dense
Degree is 3-4.5%, 50 DEG C of neutral brine；In the period that oil temperature drops to room temperature by 50 DEG C, frequency of oscillation is changed to 200-
300Hz, and be added and account for former selenium-rich squid powder weight 1-1.5%, the aqueous citric acid solution that pH value is 4.0；It is quiet to put after oscillation treatment
It to layering, is filtered using separatory funnel separator, collects oil reservoir, obtain selenium-rich oil-tea camellia seed crude oil；
(4), extract：Selenium-rich oil-tea camellia seed crude oil is transferred in extraction container, the butane solvent of 2-3 times of weight is added, at room temperature
Stirring extraction 1-3 times stands, layering, then separatory funnel separator is used to filter, and collects butane extract liquor, spare；
(5), distill：Butane extract liquor is transferred in destilling tower, is first distilled to nothing at pressure 20-28KPa, 70-78 DEG C of temperature
Liquid flows out；The ethyl alcohol that addition accounts for selenium-rich oil-tea camellia seed crude oil weight 15-22% into tower again, volumetric concentration is 40-48% is water-soluble
Liquid, distillation to no liquid flows out at pressure 5-10KPa, 90-110 DEG C of temperature；Then, remaining distilled oil in destilling tower is collected
Tea seed crude oil；
(6), column is filtered：First distillation oil-tea camellia seed crude oil constant temperature is pumped into 40-50 DEG C, then by wriggling in Filter column, makes distilled oil
Tea seed crude oil flows downward naturally along Filter column, collects the column filter oil-tea camellia seed crude oil of outflow；
(7), wash：It is filtered to column and 1-2.5 times of weight is added in oil-tea camellia seed crude oil, temperature is 60-70 DEG C, mass fraction 0.1-
0.25% sodium bicarbonate or aqueous sodium carbonate, stir process 2-3h, then quiet put to temperature be down to room temperature, first use aperture
0.1-0.5 microns of membrane filtration, then filtered with separatory funnel separator, collect washing oil-tea camellia seed crude oil；
(8), refined filtration：Washing oil-tea camellia seed crude oil is filtered in the case where pressure is 1.5-2.5MPa through ultra-filtration membrane device, the oil filtered out is collected
Liquid is to get selenium-rich tea oil.
2. the preparation method of selenium-rich tea oil according to claim 1, which is characterized in that the decolorizing column in the decolorization process is
It is prepared as follows：By the quartz sand of silica decoloration sand and 40-80 mesh that the mesh number handled well is 80-120 mesh by 1：
The ratio mixing dress column of 2-2.5, dress pillar height degree is the 40-50% of pillar height.
3. the preparation method of selenium-rich tea oil according to claim 2, which is characterized in that the decolorizing column in the decolorization process is
It is prepared as follows：By the quartz sand of silica decoloration sand and 60 mesh that the mesh number handled well is 100 mesh by 1：2.2 ratio
Example mixing dress column, dress pillar height degree is the 45% of pillar height.
4. the preparation method of selenium-rich tea oil according to claim 1, it is characterised in that：Permeable membrane in the membrane filtration step
In device, the specification of permeable membrane is only the substance that molecular weight is 500-1000 to be allowed to pass through.
5. the preparation method of selenium-rich tea oil according to claim 1, it is characterised in that：Filter column in the column filters step
It is to be prepared as follows：By the quartz sand of silica decoloration sand and 40-80 mesh that the mesh number handled well is 80-120 mesh by
1：The ratio mixing dress column of 5-7, dress pillar height degree is the 40-50% of pillar height.
6. the preparation method of selenium-rich tea oil according to claim 5, it is characterised in that：Filter column in the column filters step
It is to be prepared as follows：By the quartz sand of silica decoloration sand and 60 mesh that the mesh number handled well is 100 mesh by 1：6 ratio
Example mixing dress column, dress pillar height degree is the 45% of pillar height.
7. the preparation method of selenium-rich tea oil according to claim 1, it is characterised in that：Ultrafiltration membrane in the refined filtration step
In device, the specification of ultrafiltration membrane is that substance of the molecular weight less than 2000 is only allowed to pass through.
8. the preparation method of selenium-rich tea oil according to claim 1, which is characterized in that the activated carbon in the deodorising step
It handles as follows：First by the ethanol solution of the activated carbon of 20-40 mesh input volumetric concentration 60-70%, the two it
Between weight ratio be activated carbon：Ethanol solution=1：6-8 stirs 30-45min at 60-65 DEG C；It adds and accounts for activated carbon weight
Measure 0.2-1.45%, the phosphoric acid solution that mass fraction is 10-15%, stirring；Then, every 15min additions, to account for above-mentioned ethyl alcohol molten
The 2-5% of liquid product, the phosphoric acid solution that mass fraction is 10-15%, stirring are added 3 times altogether, and filtering obtains alcohol treatment activity
Charcoal；Then the buck that addition accounts for 2-3 times of former activated carbon weight into alcohol treatment activated carbon, mass fraction is 1.2-3.4% is molten
Liquid, the stir process 30-40min at 4-10 DEG C, filtering obtain alkali process activated carbon；Again by alkali process activated carbon in 100-110
DEG C, under normal pressure dry 10-15h to get the activated carbon in deodorising step.
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| CN103931794A (en) * | 2014-03-21 | 2014-07-23 | 安徽省怀远县鑫泰粮油有限公司 | Selenium-rich sea-flavor peanut oil and its preparation method |
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| CN103931794A (en) * | 2014-03-21 | 2014-07-23 | 安徽省怀远县鑫泰粮油有限公司 | Selenium-rich sea-flavor peanut oil and its preparation method |
| CN104857940A (en) * | 2015-05-27 | 2015-08-26 | 山东福田药业有限公司 | Regeneration method of granular active carbon |
| CN105942530A (en) * | 2016-05-06 | 2016-09-21 | 浙江海洋大学 | Squid protein powder |
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