CN107502446A - Camellia oleifera fruit split-phase process - Google Patents
Camellia oleifera fruit split-phase process Download PDFInfo
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- CN107502446A CN107502446A CN201710973032.3A CN201710973032A CN107502446A CN 107502446 A CN107502446 A CN 107502446A CN 201710973032 A CN201710973032 A CN 201710973032A CN 107502446 A CN107502446 A CN 107502446A
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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
- C11B1/06—Production of fats or fatty oils from raw materials by pressing
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L5/00—Solid fuels
- C10L5/40—Solid fuels essentially based on materials of non-mineral origin
- C10L5/44—Solid fuels essentially based on materials of non-mineral origin on vegetable substances
- C10L5/445—Agricultural waste, e.g. corn crops, grass clippings, nut shells or oil pressing residues
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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
- C11B1/04—Pretreatment of vegetable raw material
-
- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
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- Oil, Petroleum & Natural Gas (AREA)
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- Engineering & Computer Science (AREA)
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- Wood Science & Technology (AREA)
- Agronomy & Crop Science (AREA)
- Microbiology (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
A kind of camellia oleifera fruit split-phase process, is comprised the technical steps that：（1）Selection：Selection just harvesting, fresh full camellia oleifera fruit；（2）De- shell：Camellia oleifera fruit is removed into shell, obtains fresh full tea seed；（3）Washing：By step（2）Gained tea seed is washed；（4）Crush：By step（3）Gained tea seed puts into pulverizer, obtains tea seed particle；（5）Split-phase 1：By step（4）Gained tea seed particle puts into juice extractor, and extruding obtains solid fiber powder and liquid serum；（6）Matchmaker from：By step（5）Gained serum, which is transported in retort, to be heated, and adds medium, continues agitating and heating layering；（7）Split-phase 2：By step（6）The centrifugation of gained emulsion obtains light phase tea oil, heavy phase Tea Saponin solution and solid phase protein, starch mixture；（8）It is cold to carry.This method processing step is simple, and oil yield is high, remains substantial amounts of nutriment, can also realize the complete utilization of camellia oleifera fruit.
Description
Technical field
The present invention relates to the processing of oil-bearing fruit, particularly a kind of camellia oleifera fruit split-phase process.
Background technology
Oil tea system Theaceae Camellia Plants, tea seed are the seeds of tea oil tree, and tea oil is can obtain through leaching or squeezing
(also known as tea-seed oil, camellia oil, camellia seed oil), tea oil is a kind of health delicious edible oil, not only excellent in color, and having
The effect of angiocardiopathies such as preventing hypertension, coronary heart disease, atherosclerosis, there is important value of exploiting and utilizing.
At present, the production method of camellia oil mainly has milling process, extraction method, aqueous enzymatic method, supercritical fluid extraction
Deng.Wherein milling process, extraction method and supercritical fluid extraction is high to the moisture requirement of glyceride stock, when moisture is low to one
Determine scope, oil plant oil yield can be only achieved high level；Aqueous enzymatic method is that glyceride stock powder is thin, and biology is added after adding water regulation pH
Enzyme carries out grease extraction under certain condition, and glyceride stock crushes all as thin as possible, the moisture requirement height equally to glyceride stock；
And people are by way of using mechanical drying again after natural drying to the control of glyceride stock moisture, moisture control process needs
Cycle length；Nutriment in-fighting is produced because tea fruit leaves parent after fresh tea fruit harvesting, and in moisture control process
Oil quality declines, and may subsequently need degumming, depickling, decolouring, deodorization and winterization to carry out oil and fat refining, so not only cause to seek
Support value to decline, and more or less produce potential safety hazard.
The content of the invention
The purpose of the present invention is to overcome the above-mentioned deficiency of prior art and provide a kind of camellia oleifera fruit split-phase process, the party
Method processing step is simple, and oil yield is high, not only remains substantial amounts of nutriment, improves the quality of camellia oil, but also retains
The strong delicate fragrance flavor of ecosystem of camellia oil；Secondly, gained heavy phase Tea Saponin, solid phase protein starch are by follow-up drying
High value added product can be obtained, realizes the complete utilization of camellia oleifera fruit.
The technical scheme is that：A kind of camellia oleifera fruit split-phase process, is comprised the technical steps that successively：
（1）Selection：Selection just harvesting, fresh full camellia oleifera fruit；
（2）De- shell：By step（1）Gained camellia oleifera fruit machinery peels off, and removes shell, obtains fresh full tea seed；
（3）Washing：By step（2）Gained tea seed is washed, and is removed spot, is obtained clean tea seed；
（4）Crush：By step（3）Gained tea seed puts into pulverizer, obtains tea seed particle；
（5）Split-phase 1：By step（4）Gained tea seed particle puts into juice extractor, and extruding obtains solid fiber powder and liquid serum；
（6）Matchmaker from：By step（5）Gained serum, which is transported in retort, to be heated, and adds medium, continues agitating and heating layering；
（7）Split-phase 2：By step（6）Gained emulsion is transported in centrifuge, and centrifugation obtains light phase tea oil, heavy phase Tea Saponin solution
With solid phase protein, starch mixture；
（8）It is cold to carry：By step（7）Gained light phase tea oil be transported to it is cold carry machine, purified, obtain high-quality camellia oil.
Wherein step（1）Described in fresh tea fruit be ripe fresh camellia oleifera fruit；
Step（4）Described in disintegrating machine discharging sieve aperture be 2-10 millimeters, after crushing tea seed particle less than 1 millimeter, surface without
Obvious white or yellowish coloured particles.
Wherein step（5）Described in 0.1 millimeter ~ 1 millimeter of juice extractor fence gap.
Wherein step（2）、（5）Described in shell and solid fiber powder high pressure granulation after, as biomass fuel.
Wherein step（5）Described in serum in moisture weight content 40%-60%, such as deficiency, can keep the skin wet, if water
Point content is too low, and oil yield is especially low, even not fuel-displaced.
Wherein step（6）Described in medium be food-grade straight alcohol or its aqueous solution, concentration is 30% ~ 100%, and concentration is low
In 30%, easily emulsification, fuel-displaced effect can be very poor, and oil yield is low.
Wherein step（6）Described in medium addition for serum volume：5%~30%（Food-grade straight alcohol）, 30% ~
100%（The food-grade ethanol aqueous solution, concentration are 30% ~ 100%）.
Wherein step（6）Described in 50 DEG C ~ 70 DEG C of heating-up temperature, pressure 0.1MPa ~ 0.5MPa, retention time 10min ~
120min.Temperature is too high, and obtained oil quality is bad, and temperature is too low, and demulsification is poor, fuel-displaced few；Because the system of the present invention
It is that water, saponin, protein, starch emulsify together, without certain temperature, it is difficult to completely isolated completely.
Step（6）In in matchmaker from process inflated with nitrogen, prevent oily oxydrolysis.
Step（7）Described in centrifugation be three phase centrifugation separation, 1000 ~ 10000 turns/min of centrifuge speed, centrifugation
Time 3min ~ 5min, than other good separating effects.
Step（7）Described in heavy phase Tea Saponin solution by spray drying obtain Tea Saponin particle.
Step（7）Described in solid phase protein, starch by flood dragon dry obtain protein, starch granules.
Step（8）Described in purification using food grade active charcoal adsorb, specific surface area 1200m2/g~2500m2/ g, add
Amount accounts for the 0.1 ~ 2.0% of light phase tea oil weight, 0 DEG C ~ 30 DEG C of adsorption temp, adsorption time 5min ~ 10min.
Step of the present invention（5）Extruding is obtained in solid fiber powder after addition 40%-60% water, and input juice extractor, extruding obtains
Obtain solid fiber powder and liquid serum；Gained serum is transported in retort and heated, adds medium, continues agitating and heating point
Layer；Centrifugation obtains light phase tea oil, heavy phase Tea Saponin solution and solid phase protein, starch mixture；Finally cold to carry, extraction is more thorough
Bottom.
The beneficial effects of the present invention are：
（1）This method processing step is simple, remains the strong delicate fragrance flavor of ecosystem of camellia oil, gained heavy phase Tea Saponin, consolidates
Phase protein starch can obtain high value added product by follow-up drying, realize the complete utilization of camellia oleifera fruit.
（2）The present invention improves the edible palatability and edible safety of camellia oil using selecting, taking off shell, washing step
Property.
（3）The present invention is squeezed the juice using fresh fruit, low temperature extraction, not only remains a large number of nutrients, and oil quality is high,
Even save because of the camellia oil production hour of moisture control consumption.
（4）The present invention is squeezed the juice using fresh fruit carries oil, and grease nearly all enters in serum, therefore oil yield is high.
Embodiment
Below in conjunction with specifically the invention will be further described.
The average specific surface area of activated carbon is 1500m in embodiment2/g。
Embodiment one
The fresh tea fruit of 1000 kilograms of selections is taken, shell is removed through hulling machine（Shell accounting is less than 1% in fresh tea seed）, obtain
Fresh tea seed, fresh tea seed crush after washing again（Crusher sifting aperture 3mm）, the fresh tea seed particle after crushing squeezed
Juice（Squeeze gap 0.1mm）Obtain solid fiber powder and serum, serum moisture 40%, after being heated to 65 DEG C, according to every 40 grams
Serum adds ratio pressure release after warm 30min, stirring under system addition absolute ethyl alcohol, pressure 0.1MPa of 9mL absolute ethyl alcohols
Heating continues 1 hour, under 1000 turns/min of centrifuge speed, centrifuges 5min, collects light phase tea oil, light phase tea oil is placed in into temperature
Solvent recovery is carried out under 80 DEG C of degree, vacuum -0.09MPa 1.5 hours, obtain ethanol tea oil, add ethanol tea oil quality
0.5% activated carbon, 60min is adsorbed at 30 DEG C of temperature, is filtrated to get finished product tea oil.
After adding 40%-60% water in the solid fiber powder obtained after fresh tea seed particle is squeezed the juice, input is squeezed
Juice machine, extruding obtain solid fiber powder and liquid serum；The step of repeating below；The finished product oil extract finally obtained is more thorough.
Embodiment two
The fresh tea fruit of 1000 kilograms of selections is taken, shell is removed through hulling machine（Shell accounting is less than 1% in fresh tea seed）, obtain
Fresh tea seed, fresh tea seed crush after washing again（Crusher sifting aperture 5mm）, the fresh tea seed particle after crushing squeezed
Juice（Squeeze gap 0.3mm）Serum is obtained, serum moisture 60%, after being heated to 70 DEG C, is added according to every 40 grams of serums
The pressure release after warm 40min under system 80% ethanol water of addition, pressure 0.1MPa of the ratio of 15mL80% ethanol waters, is stirred
Mix heating and continue 50min, under 3000 turns/min of centrifuge speed, centrifuge 4min, collect light phase tea oil, light phase tea oil is placed in
Solvent recovery is carried out under 80 DEG C of temperature, vacuum -0.09MPa 1.5 hours, obtain the tea oil of ethanol, add the tea oil of ethanol
The activated carbon of quality 1.0%, 40min is adsorbed at 0 DEG C of temperature, is filtrated to get finished product tea oil.
Embodiment three
The fresh tea fruit of 1000 kilograms of selections is taken, shell is removed through hulling machine（Shell accounting is less than 1% in fresh tea seed）, obtain
Fresh tea seed, fresh tea seed crush after washing again（Crusher sifting aperture 6mm）, the fresh tea seed particle after crushing squeezed
Juice（Squeeze gap 1mm）Serum is obtained, serum moisture 45%, after being heated to 60 DEG C, is added according to every 40 grams of serums
The pressure release after warm 50min under system 90% ethanol water of addition, pressure 0.2MPa of the ratio of 12mL90% ethanol waters, is stirred
Mix heating and continue 50min, 3min is centrifuged under 5000 turns/min of centrifuge speed, collect light phase tea oil, light phase tea oil is placed in
Solvent recovery 75min is carried out under 80 DEG C of temperature, vacuum -0.09MPa, the tea oil of ethanol is obtained, adds the tea oil matter of ethanol
The activated carbon of amount 1.5%, 30min is adsorbed at 25 DEG C of temperature, is filtrated to get finished product tea oil.
Example IV
The fresh tea fruit of 1000 kilograms of selections is taken, shell is removed through hulling machine（Shell accounting is less than 1% in fresh tea seed）, obtain
Fresh tea seed, fresh tea seed crush after washing again（Crusher sifting aperture 7mm）, the fresh tea seed particle after crushing squeezed
Juice（Squeeze gap 0.5mm）Serum is obtained, serum moisture 60%, after being heated to 50 DEG C, is added according to every 40 grams of serums
The pressure release after warm 60min under system 70% ethanol water of addition, pressure 0.5MPa of the ratio of 15mL70% ethanol waters, is stirred
Mix heating to continue 1 hour, under 3000 turns/min of centrifuge speed, centrifuge 4min, collect light phase tea oil, light phase tea oil is placed in
Solvent recovery 75min is carried out under 80 DEG C of temperature, vacuum -0.09MPa, the tea oil of ethanol is obtained, adds the tea oil matter of ethanol
The activated carbon of amount 1.0%, 50min is adsorbed at 5 DEG C of temperature, is filtrated to get finished product tea oil.
Embodiment five
The fresh tea fruit of 1000 kilograms of selections is taken, shell is removed through hulling machine（Shell accounting is less than 1% in fresh tea seed）, obtain
Fresh tea seed, fresh tea seed crush after washing again（Crusher sifting aperture 10mm）, the fresh tea seed particle progress after crushing
Squeeze the juice（Squeeze gap 0.3mm）Serum is obtained, serum moisture 50%, after being heated to 55 DEG C, is added according to every 40 grams of serums
The ratio of 8mL absolute ethyl alcohols pressure release after warm 50min, stirring under system addition absolute ethyl alcohol, pressure 0.3MPa continue
70min, centrifuges 3min under 8000 turns/min of centrifuge speed, collects light phase tea oil, and light phase tea oil is placed in into 80 DEG C of temperature, true
Solvent recovery 30min is carried out under reciprocal of duty cycle -0.09MPa, the tea oil of ethanol is obtained, adds the activity of the tea oil quality 1.5% of ethanol
Charcoal, 30min is adsorbed at 10 DEG C of temperature, is filtrated to get finished product tea oil.
Embodiment six
The fresh tea fruit of 1000 kilograms of selections is taken, shell is removed through hulling machine（Shell accounting is less than 1% in fresh tea seed）, obtain
Fresh tea seed, fresh tea seed crush after washing again（Crusher sifting aperture 8mm）, the fresh tea seed particle after crushing squeezed
Juice（Squeeze gap 0.2mm）Serum is obtained, serum moisture 55%, after being heated to 70 DEG C, is added according to every 40 grams of serums
The pressure release after warm 30min under system 90% ethanol water of addition, pressure 0.1MPa of the ratio of 15mL90% ethanol waters, is stirred
Mix heating and continue 30min, 2min is centrifuged under 10000 turns/min of centrifuge speed, collect light phase tea oil, light phase tea oil is placed in
Solvent recovery is carried out under 80 DEG C of temperature, vacuum -0.09MPa 2 hours, obtain the tea oil of ethanol, add the tea oil matter of ethanol
The activated carbon of amount 1.5%, 20min is adsorbed at 20 DEG C of temperature, is filtrated to get finished product tea oil.
Contrast groups 1
The fresh tea fruit of 1000 kilograms of selections is taken, shell is removed through hulling machine（Shell accounting is less than 1% in fresh tea seed）, obtain
Fresh tea seed, fresh tea seed crush after washing again（Crusher sifting aperture 3mm）, the fresh tea seed particle after crushing squeezed
Juice（Squeeze gap 0.1mm）Serum is obtained, serum moisture 35%, after being heated to 65 DEG C, 9mL is added according to every 40 grams of serums
The pressure release after warm 30min under system addition absolute ethyl alcohol, pressure 0.1MPa of the ratio of absolute ethyl alcohol, it is small that agitating and heating continues 1
When, under 1000 turns/min of centrifuge speed, 5min is centrifuged, light phase tea oil is collected, light phase tea oil is placed in 80 DEG C of temperature, vacuum
Solvent recovery is carried out under degree -0.09MPa 1.5 hours, obtains ethanol tea oil, add the activated carbon of ethanol tea oil quality 0.5%,
60min is adsorbed at 30 DEG C of temperature, is filtrated to get finished product tea oil.
Contrast groups 2
Fresh tea fruit shells impurity elimination, squeezes defibrination, and the water content in adjustment gained slurries, it is 75% to make its water content, stirring
After more than 60min, sedimentation separation, supernatant liquor and lower floor's turbid solution are obtained.Supernatant liquid is taken, is separated with centrifuge, is obtained
Refined tea oil 1；Layer turbid solution filtering, a centrifugation are removed, refined tea oil 2 is obtained, merges 1 and 2, obtains refined tea oil 3, process conditions
With contrast groups 1.
Contrast groups 3
Contrast groups 3 are that traditional pressing method produces camellia oil, and specific method is as follows：Fresh tea fruit goes shell impurity elimination, dries and dries
Do, de- tea seed episperm, after frying of steaming to tea seed moisture 4-8%, enter oil press squeezing, camellia oil is squeezed in filtering acquisition.
According to embodiment one, embodiment two, embodiment three, example IV, embodiment five and embodiment six and contrast groups
And 9 groups of oil yields are compared（Tea seed oil content is 33%）, as a result such as table 1.
Table 1
。
The camellia oil produced of method using the present invention is learnt from table 1, and oil yield is higher than in general method.
According to embodiment one, embodiment two, embodiment three, example IV, embodiment five and embodiment six and contrast groups
And 9 groups of light phase tea oil acid values and peroxide value are compared, as a result such as table 2.
Table 2
。
The camellia oil produced using the method for the present invention is learnt from table 2, acid value and peroxide value are well below in general side
Method.
Detection experiment
Light phase tea oil obtained by previous embodiments and contrast groups is detected by following standard and method；Acid value refers to
The animal and plant fat acid numbers of GB/T 5530 and acidometry；Peroxide value refers to the vegetable and animals oils lipid peroxidations of GB/T 5538
It is worth determination method.
According to embodiment one, embodiment two, embodiment three, example IV, embodiment five and embodiment six and contrast groups,
And 9 groups of light phase tea oil flavones, OPC, tsubakisaponin, total triterpene and carotenoid are compared, as a result such as table 3.
Table 3
。
Learn the camellia oil produced of method using the present invention from table 3, flavones, OPC, tsubakisaponin, total triterpene and
Carotenoid is significantly larger than in general method.
Detection experiment
（1）Flavones
Detection reagent：Absolute ethyl alcohol, natrium nitrosum, aluminum nitrate, sodium hydroxide, it is that analysis is pure；Rutoside standard sample（Measure is yellow
Standard sample used in ketone, HPLC >=98%）, it is purchased from Shanghai Yuan Ye bio tech ltd.
Detecting step：
A. sample preparation：20 grams of greases are weighed in flask, add 20 milliliter of 60% ethanol solution, stirring extraction 1 is small at 70 DEG C
When, centrifugation, supernatant is collected, by grease again with 20 milliliter of 60% ethanol solution, stirring extraction 1 hour at 70 DEG C, centrifugation,
Supernatant is collected again, is merged supernatant twice and is transferred in 50 milliliters of volumetric flasks, it is to be measured with 60% ethanol solution constant volume.
B. standard curve making：Rutoside standard sample is dissolved with 60% ethanol solution, and prepare 8ug/mL, 16ug/mL,
32ug/mL, 48ug/mL, 64ug/mL normal gradients solution, draw 1 milliliter of each normal gradients solution and be respectively placed in different 25
In milliliter volumetric flask, added respectively with 60% ethanol solution to 10 milliliters, add 1 milliliter of 5% sodium nitrite solution, shake up, placed
6min, adds 1 milliliter of 10% aluminum nitrate solution, and 10 milliliter of 4% sodium hydroxide solution is added after 6min, mixes, then with 60% ethanol
Solution is settled to scale, shakes up, and absorbance, using absorbance as ordinate, rutin are determined at wavelength 510nm again after placing 15min
Normal gradients concentration is abscissa, draws standard curve.
C. detect：Draw 5 milliliters of solution to be measured to be placed in 25 milliliters of different volumetric flasks, added with 60% ethanol solution to 10
Milliliter, 1 milliliter of 5% sodium nitrite solution is added, is shaken up, place 6min, added 1 milliliter of 10% aluminum nitrate solution, add after 6min
Enter 10 milliliter of 4% sodium hydroxide solution, mix, then scale is settled to 60% ethanol solution, shake up, in wavelength after placement 15min
Absorbance is determined at 510nm, concentration and content is calculated according to corresponding to absorbance is found out on standard curve.
（2）OPC
Detection reagent：Methanol, n-butanol, hydrochloric acid, ammonium ferric sulfate, it is that analysis is pure；OPC standard sample（HPLC≥
95%）, it is purchased from Shanghai Yuan Ye bio tech ltd.
Detecting step：
A. sample preparation：10 grams of greases are weighed in flask, add 20 milliliter of 50% methanol solution, stirring extraction 1 is small at 70 DEG C
When, centrifugation, supernatant is collected, by grease again with 20 milliliter of 50% methanol solution, stirring extraction 1 hour at 70 DEG C, centrifugation,
Supernatant is collected again, is merged supernatant twice and is transferred in 50 milliliters of volumetric flasks, it is to be measured with 50% methanol solution constant volume.
B. standard curve making：OPC standard sample is dissolved with 50% methanol solution, and prepare 10ug/mL,
20ug/mL, 40ug/mL, 80ug/mL, 100ug/mL normal gradients solution, draw 1 milliliter of each normal gradients solution and put respectively
In 10 milliliters of different tool plug conical flasks, the mixed liquor of 6 milliliters of n-butanols and hydrochloric acid is separately added into（N-butanol:Hydrochloric acid=95:5）,
Add 0.2 milliliter of 2% ammonium ferric sulfate solution（2% solution is made into concentration 2mmol/L hydrochloric acid）, mix, put boiling water bath backflow,
After police dog heating 40min, 2min is cooled down to ice-water bath immediately, room temperature 10min is placed after taking-up, determined and inhale at wavelength 546nm
Luminosity, using absorbance as ordinate, OPC normal gradients concentration is abscissa, draws standard curve.
C. detect：Draw 1 milliliter of solution to be measured to be respectively placed in 10 milliliters of tool plug conical flasks, add 6 milliliters of n-butanols and salt
The mixed liquor of acid（N-butanol:Hydrochloric acid=95:5）, add 0.2 milliliter of 2% ammonium ferric sulfate solution（Matched somebody with somebody with concentration 2mmol/L hydrochloric acid
Into 2% solution）, mix, put boiling water bath backflow, after accurately heating 40min, cool down 2min to ice-water bath immediately, placed after taking-up
Room temperature 10min, determines absorbance at wavelength 546nm, concentration and is calculated according to corresponding to absorbance is found out on standard curve
Content.
（3）Tsubakisaponin
Detection reagent：Ethanol, the concentrated sulfuric acid, vanillic aldehyde, it is that analysis is pure；Tsubakisaponin standard sample, it is purchased from Shanghai source leaf biology
Science and Technology Ltd..
Detecting step：
A. sample preparation：5 grams of greases are weighed in flask, add 20 milliliter of 50% ethanol solution, stirring extraction 1 is small at 70 DEG C
When, centrifugation, supernatant is collected, by grease again with 20 milliliter of 50% ethanol solution, stirring extraction 1 hour at 70 DEG C, centrifugation,
Supernatant is collected again, is merged supernatant twice and is transferred in 50 milliliters of volumetric flasks, it is to be measured with 50% ethanol solution constant volume.
B. standard curve making：Tsubakisaponin standard sample is dissolved with 50% ethanol solution, and prepare 10ug/mL,
100ug/mL, 400ug/mL, 800ug/mL, 1000ug/mL normal gradients solution, draw 1 milliliter of each normal gradients solution point
It is not placed in 10 milliliters of different color-comparison tubes, is separately added into 1 milliliter of 8% vanillic aldehyde solution（8 grams of vanillic aldehydes are dissolved in 100 milliliters
Absolute ethyl alcohol）, mix, then be placed in ice-water bath and be slowly added to 3 milliliter of 77% sulfuric acid solution, mix, put 60 DEG C of water-baths
15min, take out it is rapid place ice-water bath 2min, place room temperature 10min and absorbance determined at wavelength 545nm, using absorbance as
Ordinate, tsubakisaponin normal gradients concentration are abscissa, draw standard curve.
C. detect：Draw 1 milliliter of solution to be measured to be placed in 10 milliliters of color-comparison tubes, add 1 milliliter of 8% vanillic aldehyde solution
（8 grams of vanillic aldehydes are dissolved in 100 milliliters of absolute ethyl alcohols）, mix, then be placed in ice-water bath and be slowly added to 3 milliliter of 77% sulfuric acid solution, mix
It is even, 60 DEG C of water-bath 15min are put, rapid placement ice-water bath 2min is taken out, places room temperature 10min and determined at wavelength 545nm
Absorbance, concentration and content is calculated according to corresponding to absorbance is found out on standard curve.
（4）Total triterpene
Detection reagent：Ethanol, glacial acetic acid, perchloric acid, vanillic aldehyde, it is that analysis is pure；Ursolic acid standard sample（For determining total three
Terpene, HPLC >=98%）, it is purchased from Shanghai Yuan Ye bio tech ltd.
Detecting step：
A. sample preparation：5 grams of greases are weighed in flask, add 20 milliliters of absolute ethyl alcohols, stirring extraction 1 hour at 70 DEG C,
Centrifugation, supernatant is collected, by grease again with 20 milliliters of absolute ethyl alcohols, stirring extraction 1 hour, centrifugation, is received again at 70 DEG C
Collect supernatant, merge supernatant twice and be transferred in 50 milliliters of volumetric flasks, it is to be measured with absolute ethyl alcohol constant volume.
B. standard curve making：Ursolic acid standard sample is dissolved with absolute ethyl alcohol, and prepare 10ug/mL, 20ug/mL,
40ug/mL, 60ug/mL, 80ug/mL normal gradients solution, draw 1 milliliter of each normal gradients solution and be respectively placed in different 10
In milliliter color-comparison tube, then it is placed in boiling water bath and volatilizes solvent, is separately added into 0.4 milliliter of 5% vanillic aldehyde solution（5 grams of vanillic aldehydes
It is dissolved in 100 milliliters of glacial acetic acid）With 1 milliliter of perchloric acid, mix, then be placed in 60 DEG C of heating water bath 15min, taking-up is placed in ice-water bath
2min, 3.6 milliliters of glacial acetic acid are added, mixed, room temperature places 10min and absorbance is determined at wavelength 545nm, is vertical using absorbance
Coordinate, ursolic acid normal gradients concentration are abscissa, draw standard curve.
D. detect：Draw 0.5 milliliter of solution to be measured be placed in 10 milliliters of color-comparison tubes, then be placed in boiling water bath volatilize it is molten
Agent, add 0.4 milliliter of 5% vanillic aldehyde solution（5 grams of vanillic aldehydes are dissolved in 100 milliliters of glacial acetic acid）With 1 milliliter of perchloric acid, mix, then put
In 60 DEG C of heating water bath 15min, taking-up is placed in ice-water bath 2min, adds 3.6 milliliters of glacial acetic acid, mixes, room temperature place 10min in
Absorbance is determined at wavelength 545nm, concentration and content is calculated according to corresponding to absorbance is found out on standard curve.
（5）Carotenoid
Detection reagent：Ethanol, analysis are pure；Bata-carotene standard sample（For determining carotenoid, HPLC >=98%）, it is purchased from
Hai Yuanye bio tech ltd.
Detecting step：
A. sample preparation：20 grams of greases are weighed in flask, add 20 milliliters of absolute ethyl alcohols, stirring extraction 1 hour at 70 DEG C,
Centrifugation, supernatant is collected, by grease again with 20 milliliters of absolute ethyl alcohols, stirring extraction 1 hour, centrifugation, is received again at 70 DEG C
Collect supernatant, merge supernatant twice and be transferred in 50 milliliters of volumetric flasks, it is to be measured with absolute ethyl alcohol constant volume.
B. standard curve making：Ursolic acid standard sample is dissolved with absolute ethyl alcohol, and prepares 0.1ug/mL, 0.2ug/
ML, 0.3ug/mL, 0.4ug/mL, 0.5ug/mL normal gradients solution, absorbance is determined at wavelength 454nm, with absorbance
For ordinate, bata-carotene normal gradients concentration is abscissa, draws standard curve.
C. prepare liquid is determined into absorbance at wavelength 454nm, it is dense according to corresponding to absorbance is found out on standard curve
Spend and calculate content.
Claims (10)
1. a kind of camellia oleifera fruit split-phase process, it mainly includes：
（1）Selection：Select the camellia oleifera fruit just plucked；
（2）De- shell：By step（1）Gained camellia oleifera fruit machinery peels off, and removes shell, obtains fresh tea seed；
（3）Washing：By step（2）The fresh tea seed of gained is washed, and is removed spot, is obtained clean tea seed；
（4）Crush：By step（3）Gained tea seed puts into pulverizer, obtains tea seed particle；
（5）Split-phase 1：By step（4）Gained tea seed particle puts into juice extractor, and extruding obtains solid fiber powder and liquid serum；
（6）Matchmaker from：By step（5）Gained serum, which is transported in retort, to be heated, and adds medium, continues agitating and heating layering；
（7）Split-phase 2：By step（6）Gained emulsion is transported in centrifuge, and centrifugation obtains light phase tea oil, heavy phase Tea Saponin solution
With solid phase protein, starch mixture；
（8）It is cold to carry：By step（7）Gained light phase tea oil be transported to it is cold carry machine, purified, obtain camellia oil.
2. camellia oleifera fruit split-phase process as described in claim 1, it is characterised in that step（2）Described in de- shell,
Shell accounting is less than 1% in fresh tea seed.
3. camellia oleifera fruit split-phase process as described in claim 1, it is characterised in that step（4）Described in pulverizer go out
Material screen hole is 2-10 millimeters, and tea seed particle is less than 1 millimeter after crushing.
4. camellia oleifera fruit split-phase process as described in claim 1, it is characterised in that step（5）Described in juice extractor grid
0.1 millimeter ~ 1 millimeter of column gap.
5. camellia oleifera fruit split-phase process as claimed in claim 1, it is characterised in that step（5）Described in serum in moisture
Content 40-60%.
6. camellia oleifera fruit split-phase process as described in claim 1, it is characterised in that step（6）Described in medium be second
Alcohol, addition be serum volume 5-30%, step（6）Described in 50 DEG C ~ 70 DEG C, pressure 0.1-0.5MPa of heating-up temperature, protect
Hold time 10-120min.
7. camellia oleifera fruit split-phase process as described in claim 1, it is characterised in that step（5）Extruding obtains solid fiber
After adding 40-60% water in powder, juice extractor is put into, extruding obtains solid fiber powder and liquid serum；Gained serum is transported to
Heated in retort, add medium, continue agitating and heating layering；Centrifugation obtains light phase tea oil, heavy phase Tea Saponin solution and solid phase
Protein, starch mixture；It is finally cold to carry.
8. camellia oleifera fruit split-phase process as described in claim 1, it is characterised in that step（7）Described in centrifugation
Separated for three phase centrifugation, centrifuge speed 1000 ~ 10000 turns/min, centrifugation time 3min ~ 5min.
A kind of 9. camellia oleifera fruit split-phase process described in claim 1, it is characterised in that step（7）Described in heavy phase tea
Saponin solution obtains Tea Saponin particle by spray drying.
10. camellia oleifera fruit split-phase process as described in claim 1, it is characterised in that step（7）Described in solid phase egg
White matter starch is dried by flood dragon and obtains Tea Saponin particle；Step（8）Described in purification using food grade active charcoal adsorb, than
1200 ~ 2500m of surface area2/ g, addition account for light phase tea oil weight 0.1 ~ 2.0%, 0 DEG C ~ 30 DEG C of adsorption temp, adsorption time
5min~10min。
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| CN108329991A (en) * | 2018-02-13 | 2018-07-27 | 江南大学 | A kind of method of water-borne method extraction camellia seed oil |
| CN115305146A (en) * | 2022-08-31 | 2022-11-08 | 湖南大三湘茶油股份有限公司 | Method for directly preparing edible oil from fresh oil |
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