CN105713716A - Method for extracting sea buckthorn fruit oil in grading mode through combination of aqueous enzymatic method and ultrasonic assistance - Google Patents
Method for extracting sea buckthorn fruit oil in grading mode through combination of aqueous enzymatic method and ultrasonic assistance Download PDFInfo
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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
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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
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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
- C11B1/106—Production of fats or fatty oils from raw materials by extracting using ultra-sounds
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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
- C11B1/12—Production of fats or fatty oils from raw materials by melting out
- C11B1/14—Production of fats or fatty oils from raw materials by melting out with hot water or aqueous solutions
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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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- 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
- C11B3/006—Refining fats or fatty oils by extraction
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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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Abstract
The invention discloses a method for extracting sea buckthorn fruit oil in a grading mode through combination of an aqueous enzymatic method and ultrasonic assistance, and belongs to the field of sea buckthorn fruit oil extraction. The method comprises the steps that sea buckthorn fruit is squeezed, fruit juice and filter residues are separated, fruit oil in the fruit juice is firstly extracted out through enzymolysis and the ultrasonic assistance, then freezing alcohol precipitation is performed on the fruit residues is further obtain fruit oil in the fruit residues, the fruit oil obtained in the first time and the fruit oil obtained in the second time are merged, and the precision of the merged fruit oil is improved through a supercritical carbon dioxide method. Experiments prove that the method has the advantages that operation is safe, easy and convenient; by performing grading extraction on the sea buckthorn fruit through combination of the aqueous enzymatic method and the ultrasonic assistance, the nutritional quality of the sea buckthorn fruit is guaranteed while the oil yield of the sea buckthorn fruit is guaranteed, sea buckthorn fruit resources are fully utilized, and the prepared sea buckthorn fruit oil is perfect in color and luster, nontoxic, odorless and free of any organic solvent residues and harm to a human body and the environment.
Description
Technical field
The invention discloses a kind of aqueous enzymatic method and the method for ultrasonic wave added coupling grading extraction Oleum Hippophae, belong to Oleum Hippophae and extract field.
Background technology
The one that Fructus Hippophae is rare in plant amedica can grow under severe conditions, and the plant containing various active composition, is that Ancient Times in China hides the raw conventional Chinese medicine for curing the disease of Mongolian medicine, has eliminate the phlegm profit lung, nourishing stomach and spleen, the pharmacologic effect got rid of illness of invigorating blood circulation.
Oleum Hippophae is the material extracted from Fructus Hippophae by certain physical means, it is a kind of high nutrition, the natural materials of high economic worth, it is by Palmic acid, palmitic olefinic acid, stearic acid, oleic acid, linoleic acid, the multiple beneficial fatty acid compositions such as linolenic acid, wherein unsaturated fatty acid is up to 70%, the indispensable vitamin A of carotenoid and vitamin E and various trace elements such as human body in Oleum Hippophae, selenium, magnesium, zinc, ferrum, manganese equal size is also higher, in addition, a small amount of plant sterol in Fructus Hippophae, catechin, flavone compound, the process of liquefaction is also enriched in Oleum Hippophae, these active substances mostly are human body cell composition and the indispensable material of the activity that sustains life, participate in the links of the vital movement of body, the nutrition of Fructus Hippophae has comprehensive as can be seen here, it is that other oils and fatss are incomparable, suitable in various crowds, particularly diabetes, hyperglycemic patients；But, the lipid material in Fructus Hippophae is primarily present in cell on the one hand and is wrapped up by cell wall, and the colloidal substance again with based on pectin forms the emulsifying systems of high compactness on the other hand, and therefore general method is difficult to be sufficiently separated Oleum Hippophae discharge.
At present in the Fructus Hippophae industry of China, the extraction of Oleum Hippophae mainly has natural sedimentation, three partition methods and solvent extraction.
(1) natural sedimentation be by clear Xian after Fructus Hippophae squeeze the juice or pull an oar, gained juice loads in hermetic container, namely Oleum Hippophae is isolated after fermentation a period of time at a certain temperature, the product sanitary index that this method obtains is poor, especially cannot effectively controlling the content of the aflatoxin that health is extremely harmful, oil yield only has 30%～40% simultaneously；
(2) three partition methods are that the Fructus Hippophae after cleaning is squeezed the juice or pulled an oar, gained juice is separated by three disc separators and obtains fruit oil, fruit juice, sarcocarp mud, the hygienic quality of the Oleum Hippophae that this method obtains has had and has been obviously improved, but most high extraction is also only about 50%；
(3) solvent extraction is to utilize compound difference of dissolubility or partition coefficient in the solvent of two kinds immiscible (or slightly solubles), compound is made to transfer to another solvent in a kind of solvent, through repeated multiple times extraction, the compound of the overwhelming majority is extracted, although the method oil yield efficiency is up to more than 85%～90%, but exist relatively costly, have potential safety hazard, organic solvent portion remain in poisonous in oil, have taste, harmful, and the quality of oil is had the shortcomings such as certain impact.
Summary of the invention
The technical problem that present invention mainly solves: in the extracting method for Oleum Hippophae conventional at present, natural sedimentation and three partition method oil yields are relatively low, and though solvent extraction oil yield is high, but there is organic solvent portion and residue in oil, poisonous, there is taste, human body and environment there is harm, and reclaim organic solvent and there is potential safety hazard and the insufficient present situation of the Fructus Hippophae utilization of resources, provide one to be squeezed the juice by Fructus Hippophae, separate fruit juice and filtering residue, the fruit oil in fruit juice is first gone out with enzymolysis and ultrasound assisted extraction, again marc freezing precipitate with ethanol is obtained the fruit oil in marc further, merge twice fruit oil and improve fruit oil precision through supercritical carbon dioxide process, thus obtaining aqueous enzymatic method and the method for ultrasonic wave added coupling grading extraction Oleum Hippophae.The method simple and safe operation, aqueous enzymatic method and ultrasonic wave added method coupling, to Fructus Hippophae grading extraction, while ensure that Fructus Hippophae oil yield, not only more remain its nutritional quality, Fructus Hippophae resource is fully used, and the Oleum Hippophae color and luster prepared is perfect, nontoxic, tasteless, without any organic solvent residual, human body and environment are safe from harm.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
(1) take the fresh Fructus Hippophae of 2～3kg to clean and put into juice extractor and squeeze the juice, isolated by filtration obtains fruit juice, marc is standby, the fruit juice squeezed by 500～600mL is poured in enzymatic vessel, add the wall breaking enzyme of fruit juice total amount 0.5～1% and the pectase of 1～2%, hermetically sealed can mouth after stirring by stirring rod, puts into and is warming up to 40～50 DEG C in calorstat, is incubated enzymolysis 10～12h；
(2) enzymolysis solution is moved in supersound extraction instrument after terminating by enzymolysis, extracts 30～40min with the power ultrasonic of 100～150W, then pours horizontal centrifuge into, arranging rotating speed is 7000～8000r/min, high speed centrifugation 10～15min under room temperature, separates and obtains upper strata oil reservoir, standby；
(3) above-mentioned standby Fructus Hippophae filtering residue is joined in the deionized water of its quality 3～5 times, heating in water bath is to 90～100 DEG C and keeps boiling 10～15min, make cell wall rupture, fruit oil precipitates out, in the mixed liquor after precipitation fruit oil, add the dehydrated alcohol of its volume 2～3 times again, stand precipitate with ethanol 2～3h；
(4) after precipitate with ethanol terminates, adopt liquid nitrogen refrigerating, quick freezing temperature is set and is-20～-15 DEG C, after quick-freezing 3～5min, move into ice-water bath, stratification 3～5h at 4～6 DEG C, make Oleum Hippophae slow solidification float, isolated by filtration filtrate, obtain the Oleum Hippophae of solidification；
(5) the upper strata oil reservoir Oleum Hippophae of solidification and above-mentioned standby separation obtained merges and loads in distilling apparatus, and heating in water bath is warming up to 60～70 DEG C, makes the Oleum Hippophae of solidification dissolve and distill and removes unnecessary dehydrated alcohol, obtains Fructus Hippophae slightly oily；
(6) Fructus Hippophae slightly oil is moved in supercritical carbon dioxide extraction apparatus, extract and the supercritical fluid with Oleum Hippophae is exited into separating still through top from flowing into bottom detached dowel after 3～5h, detached dowel pressure is 5～7MPa, temperature is 40～50 DEG C, temperature gradually rises from lower to upper, is finally recovered and obtains refining Oleum Hippophae.
The parameter of described supercritical carbon dioxide extraction apparatus is: extracting pressure is 20～30MPa, and extraction temperature is 40～50 DEG C, and carbon dioxide flow is 20～30L/h.
The application process of the present invention is: the Oleum Hippophae that the present invention prepares is direct-edible, wherein every day 1～3 time, each 5～10mL, in edible process, it is possible to be equipped with 200～250mL warm water delivery service, adhere to edible 7～14 days, substantially can feel that resistance of human body obtains enhancing, especially diabetics, blood glucose can be recorded after edible and be reduced to 5.3～5.0mmol/L from 7.2～7.5mmol/L, reducing more than 26%, effect is very good.
The invention has the beneficial effects as follows:
(1) present invention is not related to the use of poisonous, to have taste organic solvent, and easy and simple to handle in extraction process, process costs is cheap, is suitable for large-scale production and application；
(2) aqueous enzymatic method of the present invention and ultrasonic wave added method coupling, to Fructus Hippophae grading extraction, more remains its nutritional quality so that Fructus Hippophae resource is fully used while ensure that Fructus Hippophae oil yield；
(3) Oleum Hippophae that the present invention prepares is without objectionable impurities, long shelf-life, it is possible to be directly used in the field such as medicine, cosmetics.
Detailed description of the invention
First take the fresh Fructus Hippophae of 2～3kg to clean and put into juice extractor and squeeze the juice, isolated by filtration obtains fruit juice, marc is standby, the fruit juice squeezed by 500～600mL is poured in enzymatic vessel, add the wall breaking enzyme of fruit juice total amount 0.5～1% and the pectase of 1～2%, hermetically sealed can mouth after stirring by stirring rod, puts into and is warming up to 40～50 DEG C in calorstat, is incubated enzymolysis 10～12h；Then enzymolysis solution is moved in supersound extraction instrument after terminating by enzymolysis, extracts 30～40min with the power ultrasonic of 100～150W, then pours horizontal centrifuge into, arranging rotating speed is 7000～8000r/min, high speed centrifugation 10～15min under room temperature, separates and obtains upper strata oil reservoir, standby；Afterwards above-mentioned standby Fructus Hippophae filtering residue is joined in the deionized water of its quality 3～5 times, heating in water bath is to 90～100 DEG C and keeps boiling 10～15min, make cell wall rupture, fruit oil precipitates out, in the mixed liquor after precipitation fruit oil, add the dehydrated alcohol of its volume 2～3 times again, stand precipitate with ethanol 2～3h；After precipitate with ethanol terminates, adopt liquid nitrogen refrigerating, quick freezing temperature is set and is-20～-15 DEG C, after quick-freezing 3～5min, move into ice-water bath, stratification 3～5h at 4～6 DEG C, make Oleum Hippophae slow solidification float, isolated by filtration filtrate, obtain the Oleum Hippophae of solidification；Next upper strata oil reservoir Oleum Hippophae and the above-mentioned standby separation of solidification obtained merges and loads in distilling apparatus, and heating in water bath is warming up to 60～70 DEG C, makes the Oleum Hippophae of solidification dissolve and distill and removes unnecessary dehydrated alcohol, obtains Fructus Hippophae slightly oily；Finally Fructus Hippophae slightly oil is moved in supercritical carbon dioxide extraction apparatus, extract and the supercritical fluid with Oleum Hippophae is exited into separating still through top from flowing into bottom detached dowel after 3～5h, detached dowel pressure is 5～7MPa, temperature is 40～50 DEG C, temperature gradually rises from lower to upper, is finally recovered and obtains refining Oleum Hippophae；The parameter of wherein said supercritical carbon dioxide extraction apparatus is: extracting pressure is 20～30MPa, and extraction temperature is 40～50 DEG C, and carbon dioxide flow is 20～30L/h.
Example 1
First take the fresh Fructus Hippophae of 2kg to clean and put into juice extractor and squeeze the juice, isolated by filtration obtains fruit juice, marc is standby, the fruit juice squeezed by 500mL is poured in enzymatic vessel, add the wall breaking enzyme of fruit juice total amount 0.5% and the pectase of 1%, hermetically sealed can mouth after stirring by stirring rod, puts into and is warming up to 40 DEG C in calorstat, is incubated enzymolysis 10h；Then enzymolysis solution is moved in supersound extraction instrument after terminating by enzymolysis, extracts 30min with the power ultrasonic of 100W, then pours horizontal centrifuge into, and arranging rotating speed is 7000r/min, high speed centrifugation 10min under room temperature, separates and obtains upper strata oil reservoir, standby；Afterwards above-mentioned standby Fructus Hippophae filtering residue is joined in the deionized water of its quality 3 times, heating in water bath is to 90 DEG C and keeps boiling 10min, makes cell wall rupture, and fruit oil precipitates out, in the mixed liquor after precipitation fruit oil, add the dehydrated alcohol of its volume 2 times again, stand precipitate with ethanol 2h；After precipitate with ethanol terminates, adopt liquid nitrogen refrigerating, quick freezing temperature is set and is-20 DEG C, after quick-freezing 3min, move into ice-water bath, stratification 3h at 4 DEG C, make Oleum Hippophae slow solidification float, isolated by filtration filtrate, obtain the Oleum Hippophae of solidification；Next upper strata oil reservoir Oleum Hippophae and the above-mentioned standby separation of solidification obtained merges and loads in distilling apparatus, and heating in water bath is warming up to 60 DEG C, makes the Oleum Hippophae of solidification dissolve and distill and removes unnecessary dehydrated alcohol, obtains Fructus Hippophae slightly oily；Finally Fructus Hippophae slightly oil is moved in supercritical carbon dioxide extraction apparatus, extract and the supercritical fluid with Oleum Hippophae is exited into separating still through top from flowing into bottom detached dowel after 3h, detached dowel pressure is 5MPa, temperature is 40 DEG C, temperature gradually rises from lower to upper, is finally recovered and obtains refining Oleum Hippophae.
This example operation is simple, the Oleum Hippophae that the present invention prepares is direct-edible, wherein every day 1 time, each 5mL, in edible process, also can be equipped with 200mL warm water delivery service, adhere to edible 7 days, hence it is evident that can feel that resistance of human body obtains enhancing, especially diabetics, can recording blood glucose after edible and be reduced to 5.3mmol/L from 7.2mmol/L, reduce 26%, effect is very good.
Example 2
First take the fresh Fructus Hippophae of 2.5kg to clean and put into juice extractor and squeeze the juice, isolated by filtration obtains fruit juice, marc is standby, the fruit juice squeezed by 550mL is poured in enzymatic vessel, add the wall breaking enzyme of fruit juice total amount 0.8% and the pectase of 1.5%, hermetically sealed can mouth after stirring by stirring rod, puts into and is warming up to 45 DEG C in calorstat, is incubated enzymolysis 11h；Then enzymolysis solution is moved in supersound extraction instrument after terminating by enzymolysis, extracts 35min with the power ultrasonic of 130W, then pours horizontal centrifuge into, and arranging rotating speed is 7500r/min, high speed centrifugation 13min under room temperature, separates and obtains upper strata oil reservoir, standby；Afterwards above-mentioned standby Fructus Hippophae filtering residue is joined in the deionized water of its quality 4 times, heating in water bath is to 95 DEG C and keeps boiling 13min, makes cell wall rupture, and fruit oil precipitates out, in the mixed liquor after precipitation fruit oil, add the dehydrated alcohol of its volume 2.5 times again, stand precipitate with ethanol 2.5h；After precipitate with ethanol terminates, adopt liquid nitrogen refrigerating, quick freezing temperature is set and is-18 DEG C, after quick-freezing 4min, move into ice-water bath, stratification 4h at 5 DEG C, make Oleum Hippophae slow solidification float, isolated by filtration filtrate, obtain the Oleum Hippophae of solidification；Next upper strata oil reservoir Oleum Hippophae and the above-mentioned standby separation of solidification obtained merges and loads in distilling apparatus, and heating in water bath is warming up to 65 DEG C, makes the Oleum Hippophae of solidification dissolve and distill and removes unnecessary dehydrated alcohol, obtains Fructus Hippophae slightly oily；Finally Fructus Hippophae slightly oil is moved in supercritical carbon dioxide extraction apparatus, extract and the supercritical fluid with Oleum Hippophae is exited into separating still through top from flowing into bottom detached dowel after 4h, detached dowel pressure is 6MPa, temperature is 45 DEG C, temperature gradually rises from lower to upper, is finally recovered and obtains refining Oleum Hippophae.
This example operation is simple, the Oleum Hippophae that the present invention prepares is direct-edible, wherein every day 2 times, each 8mL, in edible process, also can be equipped with 230mL warm water delivery service, adhere to edible 10 days, hence it is evident that can feel that resistance of human body obtains enhancing, especially diabetics, can recording blood glucose after edible and be reduced to 5.15mmol/L from 7.35mmol/L, reduce 30%, effect is very good.
Example 3
First take the fresh Fructus Hippophae of 3kg to clean and put into juice extractor and squeeze the juice, isolated by filtration obtains fruit juice, marc is standby, the fruit juice squeezed by 600mL is poured in enzymatic vessel, add the wall breaking enzyme of fruit juice total amount 1% and the pectase of 2%, hermetically sealed can mouth after stirring by stirring rod, puts into and is warming up to 50 DEG C in calorstat, is incubated enzymolysis 12h；Then enzymolysis solution is moved in supersound extraction instrument after terminating by enzymolysis, extracts 40min with the power ultrasonic of 150W, then pours horizontal centrifuge into, and arranging rotating speed is 8000r/min, high speed centrifugation 15min under room temperature, separates and obtains upper strata oil reservoir, standby；Afterwards above-mentioned standby Fructus Hippophae filtering residue is joined in the deionized water of its quality 5 times, heating in water bath is to 100 DEG C and keeps boiling 15min, makes cell wall rupture, and fruit oil precipitates out, in the mixed liquor after precipitation fruit oil, add the dehydrated alcohol of its volume 3 times again, stand precipitate with ethanol 3h；After precipitate with ethanol terminates, adopt liquid nitrogen refrigerating, quick freezing temperature is set and is-15 DEG C, after quick-freezing 5min, move into ice-water bath, stratification 5h at 6 DEG C, make Oleum Hippophae slow solidification float, isolated by filtration filtrate, obtain the Oleum Hippophae of solidification；Next upper strata oil reservoir Oleum Hippophae and the above-mentioned standby separation of solidification obtained merges and loads in distilling apparatus, and heating in water bath is warming up to 70 DEG C, makes the Oleum Hippophae of solidification dissolve and distill and removes unnecessary dehydrated alcohol, obtains Fructus Hippophae slightly oily；Finally Fructus Hippophae slightly oil is moved in supercritical carbon dioxide extraction apparatus, extract and the supercritical fluid with Oleum Hippophae is exited into separating still through top from flowing into bottom detached dowel after 5h, detached dowel pressure is 7MPa, temperature is 50 DEG C, temperature gradually rises from lower to upper, is finally recovered and obtains refining Oleum Hippophae.
This example operation is simple, the Oleum Hippophae that the present invention prepares is direct-edible, wherein every day 3 times, each 10mL, in edible process, also can be equipped with 250mL warm water delivery service, adhere to edible 14 days, hence it is evident that can feel that resistance of human body obtains enhancing, especially diabetics, can recording blood glucose after edible and be reduced to 5.0mmol/L from 7.5mmol/L, reduce 33.3%, effect is very good.
Claims (2)
1. the method for an aqueous enzymatic method and ultrasonic wave added coupling grading extraction Oleum Hippophae, it is characterised in that concrete preparation process is:
(1) take the fresh Fructus Hippophae of 2～3kg to clean and put into juice extractor and squeeze the juice, isolated by filtration obtains fruit juice, marc is standby, the fruit juice squeezed by 500～600mL is poured in enzymatic vessel, add the wall breaking enzyme of fruit juice total amount 0.5～1% and the pectase of 1～2%, hermetically sealed can mouth after stirring by stirring rod, puts into and is warming up to 40～50 DEG C in calorstat, is incubated enzymolysis 10～12h；
(2) enzymolysis solution is moved in supersound extraction instrument after terminating by enzymolysis, extracts 30～40min with the power ultrasonic of 100～150W, then pours horizontal centrifuge into, arranging rotating speed is 7000～8000r/min, high speed centrifugation 10～15min under room temperature, separates and obtains upper strata oil reservoir, standby；
(3) above-mentioned standby Fructus Hippophae filtering residue is joined in the deionized water of its quality 3～5 times, heating in water bath is to 90～100 DEG C and keeps boiling 10～15min, make cell wall rupture, fruit oil precipitates out, in the mixed liquor after precipitation fruit oil, add the dehydrated alcohol of its volume 2～3 times again, stand precipitate with ethanol 2～3h；
(4) after precipitate with ethanol terminates, adopt liquid nitrogen refrigerating, quick freezing temperature is set and is-20～-15 DEG C, after quick-freezing 3～5min, move into ice-water bath, stratification 3～5h at 4～6 DEG C, make Oleum Hippophae slow solidification float, isolated by filtration filtrate, obtain the Oleum Hippophae of solidification；
(5) the upper strata oil reservoir Oleum Hippophae of solidification and above-mentioned standby separation obtained merges and loads in distilling apparatus, and heating in water bath is warming up to 60～70 DEG C, makes the Oleum Hippophae of solidification dissolve and distill and removes unnecessary dehydrated alcohol, obtains Fructus Hippophae slightly oily；
(6) Fructus Hippophae slightly oil is moved in supercritical carbon dioxide extraction apparatus, extract and the supercritical fluid with Oleum Hippophae is exited into separating still through top from flowing into bottom detached dowel after 3～5h, detached dowel pressure is 5～7MPa, temperature is 40～50 DEG C, temperature gradually rises from lower to upper, is finally recovered and obtains refining Oleum Hippophae.
2. the method for a kind of aqueous enzymatic method according to claim 1 and ultrasonic wave added coupling grading extraction Oleum Hippophae, it is characterized in that: the parameter of described supercritical carbon dioxide extraction apparatus is: extracting pressure is 20～30MPa, extraction temperature is 40～50 DEG C, and carbon dioxide flow is 20～30L/h.
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| CN111518611A (en) * | 2020-04-28 | 2020-08-11 | 上海容邦企业集团有限公司 | Sea-buckthorn fruit oil compound and preparation method thereof |
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2016
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| CN110643582A (en) * | 2019-09-29 | 2020-01-03 | 浙江工业大学 | Method for extracting SOD from fresh sea-buckthorn fruit |
| CN110643582B (en) * | 2019-09-29 | 2021-07-27 | 浙江工业大学 | Method for extracting SOD from fresh sea-buckthorn fruit |
| CN110927351A (en) * | 2019-12-04 | 2020-03-27 | 荣海生物科技有限公司 | Method for detecting quality of linseed oil |
| CN111518611A (en) * | 2020-04-28 | 2020-08-11 | 上海容邦企业集团有限公司 | Sea-buckthorn fruit oil compound and preparation method thereof |
| CN113913267A (en) * | 2021-10-15 | 2022-01-11 | 江苏恒顺醋业股份有限公司 | Preparation method of seabuckthorn fruit vinegar powder with oxidation resistance |
| CN114668089A (en) * | 2022-03-09 | 2022-06-28 | 山东省食品发酵工业研究设计院 | Production method for preventing oil floating of sea buckthorn fruit beverage |
| CN114668089B (en) * | 2022-03-09 | 2024-02-02 | 山东省食品发酵工业研究设计院 | Production method for preventing sea buckthorn fruit beverage grease from floating upwards |
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