CN107541332A - A kind of oil ben and preparation method thereof - Google Patents
A kind of oil ben and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of oil ben and preparation method thereof.Moringa seeds are first passed through microwave treatment, thermophilic digestion, high-pressure homogeneous and alkalinity extraction pre-treating technology by this method, combine plant hydrolyzed-enzyme enzymolysis and protease hydrolyzed, high-temperature process, cryogenic freezing, defrosting and the handling process of low-temperature and high-speed centrifugation again, obtain the seed oil of Moringa oleigera rich in moringa seeds protein peptides, seed oil of Moringa oleigera recovery rate>90%；Finally, toward addition in seed oil of Moringa oleigera digests through plant hydrolyzed-enzyme, protease hydrolyzed, ethanol extract and the moringa oleifera leaf extractive of macroporous resin enrichment extraction, strengthen inoxidizability, obtain the oil ben.The oil ben nutritive value of the present invention is high, and oxidation stability is good, long shelf-life, can be widely applied in food industry.
Description
Technical field
The invention belongs to moringa seeds field of deep, and in particular to a kind of oil ben and preparation method thereof.
Background technology
Moringa, it is the plant of Moringaceae Moringa, originates in the Himalayas of north India, be planted in Asia extensively
Continent and African subtropical and tropical zones, Moringa share 14 kinds, and India's tradition Moringa (Moringa oleifera Lam.) is raw
Long fast, distribution is wide, is cultivated area maximum, the Moringa kind of most study.Plantation and developmental research master are introduced a fine variety to Moringa in China
Concentrate on the provinces such as Yunnan, Guangxi, Guangdong, Fujian, Guizhou, Taiwan.2012, leaf of Moringa was by national health and family planning
Committee's approval is used as new resource food.Moringa whole body is all precious, its blade, flower, seed and tender shoots, tender stem, root etc.
It is edible, it is the plant of integration of drinking and medicinal herbs.Hypertension, diabetes, angiocardiopathy, wind are often treated with Moringa by India and African country
The disease occurred frequently such as wet, arthritis.
Oil ben contains the very oleic acid of high content and a variety of sterols, is a kind of high-quality grease.However, due to shortage pair
The research of its intensive processing technology, seriously constrain popularization and the deep development of oil ben.Traditional grease extraction master
There are milling process and lixiviation process, as the development of science and technology, people are deepened and to green production to health with the understanding of oily concept
The weak point of the deep pursuit of processing mode, milling process and organic solvent extraction increasingly appears.And aqueous enzymatic method action condition
Gently, organic solvent-free remains, and oil extracting rate is high, is increasingly taken seriously.
The grease for not adding antioxidant is oxidizable.In recent years, as demand of the market to healthy grease increasingly increases, day
Right antioxidant is increasingly favored by food industry.Leaf of Moringa is rich in polyphenols, has strong anti-oxidation, can develop
It is applied to for natural oil antioxidant in vegetable fat.
Therefore, looking for a kind of method for efficiently, greenly extracting, preparing oil ben, there is stronger society and economy to imitate
Benefit.
The content of the invention
It is an object of the invention to provide a kind of oil ben.The oleic acid content of the oil ben>72% , behenic acid contents>
3%, nutritive value is high, and oxidation stability is good, long shelf-life, can be widely applied in food industry.
The present invention also aims to provide a kind of preparation method of described oil ben.This method first passes through moringa seeds
Microwave treatment, thermophilic digestion, high-pressure homogeneous and alkalinity extraction pre-treating technology, then combine plant hydrolyzed-enzyme enzymolysis and egg
White enzyme enzymolysis, high-temperature process, cryogenic freezing, defrosting and the handling process of low-temperature and high-speed centrifugation, obtain being rich in moringa seeds albumen
The seed oil of Moringa oleigera of peptide, seed oil of Moringa oleigera recovery rate>90%；Finally, digested toward addition in seed oil of Moringa oleigera through plant hydrolyzed-enzyme, protease
The moringa oleifera leaf extractive of enzymolysis, ethanol extraction and macroporous resin enrichment extraction, strengthens inoxidizability, obtains the oil ben.
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of oil ben, carried using microwave treatment, thermophilic digestion, high-pressure homogeneous and ultrasonic wave added alkaline process
The pre-treating technology taken, then combine plant hydrolyzed-enzyme enzymolysis, protease hydrolyzed, high-temperature process, cryogenic freezing, defrosting and low temperature
Ultracentrifugal handling process, obtains seed oil of Moringa oleigera；Finally, by adding moringa oleifera leaf extractive, oil ben is made, specifically includes
Following steps：
(1) microwave treatment：Shelled after fresh moringa seeds are dried, microwave treatment, crush, sieving, ultramicro grinding, obtain peppery
Wooden seed powder；
(2) thermophilic digestion：Obtained moringa seeds powder is subjected to thermophilic digestion；
(3) it is high-pressure homogeneous：Learn from else's experience the moringa seeds powder after thermophilic digestion, add deionized water, colloid mill is crossed after high speed shear,
Carry out again high-pressure homogeneous, obtain moringa seeds homogenate；
(4) ultrasonic wave added alkalinity extraction：Sodium hydroxide regulation pH value is added in moringa seeds powder homogenate, ultrasonic wave added carries
Take, be cooled to room temperature, obtain suspension；
(5) moringa seeds digest：The pH value of suspension is adjusted, after adding plant hydrolyzed-enzyme enzymolysis, pH value is adjusted, adds albumen
Enzyme is digested, high-temperature process, is cooled to room temperature, carries out cryogenic freezing processing, and low temperature thaws, and low-temperature and high-speed centrifugation, is obtained peppery
Wooden seed oil；
(6) preparation of oil ben：Moringa oleifera leaf extractive is dissolved in absolute ethyl alcohol, then added in seed oil of Moringa oleigera, stirring
Uniformly, the oil ben is obtained.
Further, in step (1), the microwave treatment is the heated under microwave conditions 2-4min in 500-700W.
Further, in step (1), the sieving was 100 mesh sieves.
Further, in step (1), the ultramicro grinding is that 2-3h is crushed in airslide disintegrating mill, crushes to obtain peppery
The average grain diameter of wooden seed powder is 8-12 μm.
Further, in step (2), the thermophilic digestion is the boiling 20- under 100-120 DEG C of water vapor conditions
30min。
Further, in step (3), the solid-liquid ratio of moringa seeds powder and deionized water after thermophilic digestion is 1:6~8g/
mL。
Further, in step (3), the high speed shear is 10~20 points of the speed shearing in 8000~10000rpm
Clock.
Further, in step (3), the number for crossing colloid mill is 2~3 times.
Further, in step (3), the high-pressure homogeneous pressure is 20~40MPa, and high-pressure homogeneous number is 2~3
It is secondary.
Further, in step (4), the regulation pH value is that regulated value pH value is 7.0~9.0.
Further, in step (4), the ultrasonic power of the ultrasound assisted extraction is 600-800W, time 10-
20min, temperature are 40~60 DEG C.
Further, in step (5), the pH value of suspension is adjusted to 4.4-5.0.
Further, in step (5), the addition of the plant hydrolyzed-enzyme is the 2~4% of moringa seeds quality.
Further, in step (5), the plant hydrolyzed-enzyme is answering for alpha-amylase and trade names Viscozyme L
Plant hydrolyzed-enzyme is closed, the addition of alpha-amylase accounts for the 60-80% of total enzyme amount, trade names Viscozyme L composite plant
The addition of hydrolase accounts for the 20-40% of total enzyme amount.
Further, in step (5), the plant hydrolyzed-enzyme enzymolysis digests 4~6 hours under the conditions of being 50~56 DEG C.
Further, in step (5), after plant hydrolyzed-enzyme enzymolysis, regulation pH value to 7.0-8.0.
Further, in step (5), the addition of the protease is the 4~6% of moringa seeds quality.
Further, in step (5), the protease is compound protease and trade names NS37071 basic protein
Enzyme, the addition of compound protease account for the 10-30% of total enzyme amount, and the addition of trade names NS37071 alkali protease accounts for
The 70-90% of total enzyme amount.
Further, in step (5), the protease hydrolyzed digests 12~16 hours under the conditions of being 50~56 DEG C.
Further, in step (5), the high-temperature process is 100-120 DEG C of heat treatment 20-40min.
Further, in step (5), the cryogenic freezing processing is -18~-24 DEG C of freezing 8-12h.
Further, in step (5), the low temperature thaws for 4-8 DEG C of placement 8-12h.
Further, in step (5), under the conditions of the low-temperature centrifugation is 4-8 DEG C, 6000~8000g centrifugations 20~
30min。
Further, in step (5), the extraction yield of the seed oil of Moringa oleigera>90%.
Further, in step (6), the moringa oleifera leaf extractive, to be digested through plant hydrolyzed-enzyme, protease hydrolyzed, second
The handling process of alcohol extracting and macroporous resin enrichment is extracted to obtain, and specifically comprises the following steps：
Moringa cured leaf is taken, crushes, sieving, obtains leaf of Moringa powder, adds deionized water, it is well mixed to obtain suspension, adjust
The pH value of suspension is saved, after adding plant hydrolyzed-enzyme enzymolysis, adjusts pH value, protease is added and is digested, add absolute ethyl alcohol,
Heating and refluxing extraction, after extract solution is cooled to room temperature, centrifugation is removed slag, and takes supernatant, is concentrated under reduced pressure, and freeze-drying, takes freeze-dried powder
End is dissolved in water, crosses macroporous resin column, using ethanol solution gradient elution, collects eluent, freeze-drying, obtains leaf of Moringa extraction
Thing.
Further, the sieving was 40 mesh sieves.
Further, the leaf of Moringa powder and the solid-liquid ratio of deionized water are 1:8~10g/mL.
Further, the pH value of suspension is adjusted to 4.4-5.0.
Further, the addition of the plant hydrolyzed-enzyme is the 2~4% of Moringa cured leaf quality.
Further, the plant hydrolyzed-enzyme is trade names Viscozyme L composite plant hydrolase.
Further, the plant hydrolyzed-enzyme enzymolysis digests 4~6 hours under the conditions of being 50~56 DEG C.
Further, after plant hydrolyzed-enzyme enzymolysis, regulation pH value to 7.0-8.0.
Further, the addition of the protease is the 4~6% of Moringa cured leaf quality.
Further, the protease is pancreatin and trade names NS37071 alkali protease, the addition of pancreatin
The 40-60% of total enzyme amount is accounted for, the addition of trade names NS37071 alkali protease accounts for the 40-60% of total enzyme amount.
Further, the protease hydrolyzed digests 6~8 hours under the conditions of being 50~56 DEG C.
Further, the addition of absolute ethyl alcohol is ethanol content in system is reached 30~50wt%.
Further, the condition being heated to reflux is heated to reflux 1-2h under the conditions of being 90-100 DEG C.
Further, the centrifugation centrifuges 10~20min for 4000~6000g.
Further, described be concentrated under reduced pressure to be concentrated into solid content is 20~30%.
Further, it is 100-200mg/mL that freeze-dried powder, which is dissolved in the concentration after water,.
Further, the macroreticular resin is Mitsubishi chemistry macroporous absorbent resin SP207.
Further, the gradient elution is using 0-50vol% ethanol solution gradient elutions, is specially：1-2 post
Volume uses 100vol% water elutions, and 3-5 column volume is using 100-60vol% water, 0-40vol% ethanol elutions, 6-7 post
Volume collects 50vol% ethanol eluates using 50vol% water, 50vol% ethanol elutions.
Further, in step (6), the dissolving ratio of the moringa oleifera leaf extractive and absolute ethyl alcohol is 0.1-0.2:3-
5g/mL。
Further, in step (6), the mass ratio of the moringa oleifera leaf extractive and seed oil of Moringa oleigera is 1-2:10000.
A kind of oil ben, oleic acid content as made from the preparation method described in any of the above-described>72% , behenic acid contents>
3%.
The nutritive value of the oil ben of preparation is high, and oxidation stability is good, long shelf-life, can be widely applied to food industry
In.
Compared with prior art, the invention has the advantages that and beneficial effect：
(1) the inventive method is using microwave treatment, thermophilic digestion, high-pressure homogeneous and ultrasonic wave added alkalinity extraction preceding place
Science and engineering skill, joint plant hydrolyzed-enzyme enzymolysis, protease hydrolyzed, high-temperature process, cryogenic freezing, thaw and low-temperature and high-speed centrifuges
To seed oil of Moringa oleigera, moringa seeds oil yield is improved；
(2) the inventive method is extracted, greatly by being added in seed oil of Moringa oleigera through plant hydrolyzed-enzyme and protease hydrolyzed, ethanol
The moringa oleifera leaf extractive that hole resin concentration is extracted, obtained oil ben, the oxidation stability of oil ben is greatly improved, is extended
Shelf-life of oil ben；
(3) the inventive method is using efficient, green extraction extraction seed oil of Moringa oleigera, seed oil of Moringa oleigera recovery rate>90%, obtain
To oil ben in, oleic acid content>72% , behenic acid contents>3%, organic solvent-free residual, no chemical additive, nutriture value
Value is high, and oxidation stability is good, long shelf-life, can be widely applied in food industry.
Embodiment
Technical solution of the present invention is described in further detail below in conjunction with specific embodiment, but protection scope of the present invention
It is not limited to following examples.
In following examples, the assay method that aliphatic acid forms in grease is as follows：
Claim oil sample 10-20mg, add the boron trifluoride-methanol solution of 2mL 14%, water-bath 30min at 60 DEG C, carry out
Esterification；After being cooled to room temperature, 1mL water and 1mL n-hexanes are added, is mixed, after stratification, upper organic layer is taken, adds nothing
After aqueous sodium persulfate water removal, dried up with high pure nitrogen, add 0.4mL n-hexanes, (methyl margarate-n-hexane is molten for 0.1mL internal standards
Liquid), carry out GC-MS analyses after crossing the filtering of 0.22 micron membrane filter.
GC conditions：
(1) TR-5ms elastic quartzs chromatographic column, split ratio 100:1；
(2) column temperature heating schedule：40 DEG C of initial temperature, 2min is kept, then rise to 150 DEG C with 10 DEG C/min, kept
2min, then 280 DEG C are risen to 10 DEG C/min, maintain 5min；
(3) carrier gas is high-purity He, flow velocity 1.0mL/min.
MS conditions：
(1) electron impact ionization ion gun (EI), electron energy 70eV；
(2) 230 DEG C of ion source temperature, 250 DEG C of interface (transmission line) temperature；
(3) sweep speed 3.0scans/s, 33~350m/z of quality of scanning scope.
The assay method of oil oxidative stability uses Schaal Oven Methods, and grease is positioned in 60 DEG C of constant temperature ovens and connected
Continuous accelerated oxidation 14 days；16.00g oil samples are taken every 2d, determine its POV values, acid value.
By national Specification, the peroxide value upper limit of grease is 6mmol/kg, then public according to Arrhenius experiences
Formula, 60 DEG C of Oven Method, 1 day equivalent to 20 DEG C under the conditions of storage calculate shelf life over 16 days；The assay method ginseng of acid value
According to GB/T5009.37-2003, the measure of peroxide value is with reference to GB/T5009.37-2003.
Embodiment 1
A kind of preparation of oil ben, specifically comprises the following steps：
(1) microwave treatment：Shell after fresh moringa seeds are dried, after microwave power 500W heats 2min, crush, mistake
100 mesh sieves, crush 2h in airslide disintegrating mill, obtain the moringa seeds powder that average grain diameter is 12 μm；
(2) thermophilic digestion：By obtained moringa seeds powder under 100 DEG C of water vapor conditions boiling 20min；
(3) it is high-pressure homogeneous：Learn from else's experience the moringa seeds powder after thermophilic digestion, according to solid-liquid ratio 1:6g/mL adds deionized water, with
8000rpm speed is sheared 10 minutes, is crossed colloid mill 2 times, is obtained moringa seeds homogenate, high-pressure homogeneous 2 times of 20MPa；
(4) ultrasonic wave added alkalinity extraction：It is 7.0 that sodium hydroxide regulation pH value is added in moringa seeds powder homogenate, ultrasound
Power 600W, temperature are 40 DEG C of extraction 10min, are cooled to room temperature, obtain suspension；
(5) moringa seeds digest：The pH value of suspension is adjusted to 4.4, adds 2% alphalise starch that quality is moringa seeds quality
The composite plant hydrolase of enzyme and trade names Viscozyme L, the addition of alpha-amylase account for the 60% of total enzyme amount, commodity board
The addition of number Viscozyme L composite plant hydrolase accounts for the 40% of total enzyme amount, is digested 4 hours under conditions of 50 DEG C；Plant
After thing enzymatic hydrolysis, regulation pH value to 7.0,4% compound protease and trade names that quality is moringa seeds quality are added
NS37071 alkali protease, the addition of compound protease account for the 10% of total enzyme amount, trade names NS37071 alkaline egg
The addition of white enzyme accounts for the 90% of total enzyme amount, is digested 12 hours under conditions of 50 DEG C；100 DEG C of heating 20min, are cooled to room
Wen Hou, -18 DEG C of freezing 8h；Place 8h for 4 DEG C and carry out low temperature defrosting, 6000g centrifugation 20min, obtain seed oil of Moringa oleigera 1, seed oil of Moringa oleigera 1
Recovery rate be 92%；
(6) prepared by moringa oleifera leaf extractive：Moringa cured leaf is taken, is crushed, after crossing 40 mesh sieves, according to solid-liquid ratio 1:8g/mL is added
Deionized water, after being well mixed, the pH value of suspension is adjusted to 4.4, adds the 2% commodity board that quality is Moringa cured leaf quality
Number Viscozyme L composite plant hydrolase, digest 4 hours under conditions of 50 DEG C；After plant hydrolyzed-enzyme enzymolysis, pH value is adjusted
To 7.0, quality is added as 4% pancreatin of Moringa cured leaf quality and trade names NS37071 alkali protease, pancreatin adds
Enter amount accounts for total enzyme amount 40%, the addition of trade names NS37071 alkali protease accounts for the 60% of total enzyme amount, 50 DEG C of bar
Digested 6 hours under part；Absolute ethyl alcohol is added, ethanol content in system is reached 30wt%, 90 DEG C are heated to reflux 1h, are cooled to room
Wen Hou, 4000g centrifuge 10min, take supernatant, and it is 20% to be concentrated under reduced pressure into solid content, freeze-drying, takes freeze-dried powder to match somebody with somebody
Into the 100mg/mL aqueous solution, Mitsubishi chemistry macroporous absorbent resin SP207 posts are crossed, are entered using 0-50vol% ethanol solutions
7 column volume gradient elutions of row, flow velocity 2mL/min, it is specially：1-5 column volume uses 100% water, 0% ethanol elution,
6-7 column volume is collected 50vol% ethanol eluates, freeze-drying, obtained peppery using 50vol% water, 50vol% ethanol elutions
Wooden leaf extract；In the moringa oleifera leaf extractive of extraction, polyphenol content 22%；
(7) preparation of oil ben：0.1g moringa oleifera leaf extractives are dissolved in 3mL absolute ethyl alcohols, are then added to 1000g Moringas
Stirred in seed oil, oil ben 1 is made.
In obtained oil ben 1, oleic acid content is that 74.2% , behenic acid contents are 3.18%, and nutritive value is high, according to
Arrhenius empirical equations, thus it is speculated that its shelf-life under conditions of room temperature, lucifuge is 72 months.
Embodiment 2
A kind of preparation of oil ben, specifically comprises the following steps：
(1) microwave treatment：Shell after fresh moringa seeds are dried, after microwave power 600W heats 3min, crush, mistake
100 mesh sieves, crush 2.5h in airslide disintegrating mill, obtain the moringa seeds powder that average grain diameter is 10 μm；
(2) thermophilic digestion：By obtained moringa seeds powder under 110 DEG C of water vapor conditions boiling 25min；
(3) it is high-pressure homogeneous：Learn from else's experience the moringa seeds powder after thermophilic digestion, according to solid-liquid ratio 1:7g/mL adds deionized water, with
9000rpm speed is sheared 15 minutes, is crossed colloid mill 3 times, is obtained moringa seeds homogenate, high-pressure homogeneous 3 times of 30MPa；
(4) ultrasonic wave added alkalinity extraction：It is 8.0 that sodium hydroxide regulation pH value is added in moringa seeds powder homogenate, ultrasound
Power 700W, temperature are 50 DEG C of extraction 15min, are cooled to room temperature, obtain suspension；
(5) moringa seeds digest：The pH value of suspension is adjusted to 4.7, adds 3% alphalise starch that quality is moringa seeds quality
The composite plant hydrolase of enzyme and trade names Viscozyme L, the addition of alpha-amylase account for the 70% of total enzyme amount, commodity board
The addition of number Viscozyme L composite plant hydrolase accounts for the 30% of total enzyme amount, is digested 5 hours under conditions of 53 DEG C；Plant
After thing enzymatic hydrolysis, regulation pH value to 7.5,5% compound protease and trade names that quality is moringa seeds quality are added
NS37071 alkali protease, the addition of compound protease account for the 20% of total enzyme amount, trade names NS37071 alkaline egg
The addition of white enzyme accounts for the 80% of total enzyme amount, is digested 14 hours under conditions of 53 DEG C；110 DEG C of heating 30min, are cooled to room
Wen Hou, -21 DEG C of freezing 10h；Place 10h for 6 DEG C and carry out low temperature defrosting, 7000g centrifugation 25min, obtain seed oil of Moringa oleigera 2, moringa seeds
The recovery rate of oil 2 is 91%；
(6) prepared by moringa oleifera leaf extractive：Moringa cured leaf is taken, is crushed, after crossing 40 mesh sieves, according to solid-liquid ratio 1:9g/mL is added
Deionized water, after being well mixed, the pH value of suspension is adjusted to 4.7, adds the 3% commodity board that quality is Moringa cured leaf quality
Number Viscozyme L composite plant hydrolase, digest 5 hours under conditions of 53 DEG C；After plant hydrolyzed-enzyme enzymolysis, pH value is adjusted
To 7.5, quality is added as 5% pancreatin of Moringa cured leaf quality and trade names NS37071 alkali protease, pancreatin adds
Enter amount accounts for total enzyme amount 50%, the addition of trade names NS37071 alkali protease accounts for the 50% of total enzyme amount, 53 DEG C of bar
Digested 7 hours under part；Absolute ethyl alcohol is added, ethanol content in system is reached 40wt%, 95 DEG C are heated to reflux 1.5h, are cooled to
After room temperature, 5000g centrifugation 10min, supernatant is taken, it is 25% to be concentrated under reduced pressure into solid content, freeze-drying, takes freeze-dried powder
The 150mg/mL aqueous solution is made into, Mitsubishi chemistry macroporous absorbent resin SP207 posts are crossed, using 0-50vol% ethanol solutions
7 column volume gradient elutions are carried out, flow velocity 2mL/min, are specially：1-2 column volume is washed using 100% water, 0% ethanol
De-, 3-5 column volume is washed using 80% water, 20% ethanol elution, 6-7 column volume using 50vol% water, 50vol% ethanol
It is de-, 50vol% ethanol eluates are collected, freeze-drying, obtain moringa oleifera leaf extractive；In the moringa oleifera leaf extractive of extraction, polyphenol contains
Measure as 23%；
(7) preparation of oil ben：0.15g moringa oleifera leaf extractives are dissolved in 4mL absolute ethyl alcohols, are added to 1000g Moringas
Stirred in seed oil, oil ben 2 is made.
In obtained oil ben 2, oleic acid content is that 73.4% , behenic acid contents are 3.11%, and nutritive value is high, according to
Arrhenius empirical equations, thus it is speculated that its shelf-life under conditions of room temperature, lucifuge is 74 months.
Embodiment 3
A kind of preparation of oil ben, specifically comprises the following steps：
(1) microwave treatment：Shell after fresh moringa seeds are dried, after microwave power 700W heats 4min, crush, mistake
100 mesh sieves, crush 3h in airslide disintegrating mill, obtain the moringa seeds powder that average grain diameter is 8 μm；
(2) thermophilic digestion：By obtained moringa seeds powder under 120 DEG C of water vapor conditions boiling 30min；
(3) it is high-pressure homogeneous：Learn from else's experience the moringa seeds powder after thermophilic digestion, according to solid-liquid ratio 1:8g/mL adds deionized water, with
10000rpm speed is sheared 20 minutes, is crossed colloid mill 3 times, is obtained moringa seeds homogenate, high-pressure homogeneous 2 times of 40MPa；
(4) ultrasonic wave added alkalinity extraction：It is 9.0 that sodium hydroxide regulation pH value is added in moringa seeds powder homogenate, ultrasound
Power 800W, temperature are 60 DEG C of extraction 20min, are cooled to room temperature, obtain suspension；
(5) moringa seeds digest：The pH value of suspension is adjusted to 5.0, adds 4% alphalise starch that quality is moringa seeds quality
The composite plant hydrolase of enzyme and trade names Viscozyme L, the addition of alpha-amylase account for the 80% of total enzyme amount, commodity board
The addition of number Viscozyme L composite plant hydrolase accounts for the 20% of total enzyme amount, is digested 6 hours under conditions of 56 DEG C；Plant
After thing enzymatic hydrolysis, regulation pH value to 8.0,6% compound protease and trade names that quality is moringa seeds quality are added
NS37071 alkali protease, the addition of compound protease account for the 30% of total enzyme amount, trade names NS37071 alkaline egg
The addition of white enzyme accounts for the 70% of total enzyme amount, is digested 16 hours under conditions of 56 DEG C；120 DEG C of heating 40min, are cooled to room
Wen Hou, -24 DEG C of freezing 12h；Place 12h for 8 DEG C and carry out low temperature defrosting, 8000g centrifugation 30min, obtain seed oil of Moringa oleigera 3, moringa seeds
The recovery rate of oil 3 is 93%；
(6) prepared by moringa oleifera leaf extractive：Moringa cured leaf is taken, is crushed, after crossing 40 mesh sieves, according to solid-liquid ratio 1:10g/mL is added
Deionized water, after being well mixed, the pH value of suspension is adjusted to 5.0, adds the 4% commodity board that quality is Moringa cured leaf quality
Number Viscozyme L composite plant hydrolase, digest 6 hours under conditions of 56 DEG C；After plant hydrolyzed-enzyme enzymolysis, pH value is adjusted
To 8.0, quality is added as 6% pancreatin of Moringa cured leaf quality and trade names NS37071 alkali protease, pancreatin adds
Enter amount accounts for total enzyme amount 60%, the addition of trade names NS37071 alkali protease accounts for the 40% of total enzyme amount, 56 DEG C of bar
Digested 8 hours under part；Absolute ethyl alcohol is added, ethanol content in system is reached 50wt%, 100 DEG C are heated to reflux 2h, are cooled to
After room temperature, 6000g centrifugation 20min, supernatant is taken, it is 30% to be concentrated under reduced pressure into solid content, freeze-drying, takes freeze-dried powder
The 200mg/mL aqueous solution is made into, Mitsubishi chemistry macroporous absorbent resin SP207 posts are crossed, using 0-50vol% ethanol solutions
7 column volume gradient elutions are carried out, flow velocity 2mL/min, are specially：1-2 column volume is washed using 100% water, 0% ethanol
De-, 3-5 column volume is washed using 60% water, 40% ethanol elution, 6-7 column volume using 50vol% water, 50vol% ethanol
It is de-, 50vol% ethanol eluates are collected, freeze-drying, obtain moringa oleifera leaf extractive；In the moringa oleifera leaf extractive of extraction, polyphenol contains
Measure as 24%.
(7) preparation of oil ben：0.2g moringa oleifera leaf extractives are dissolved in 5mL absolute ethyl alcohols, are added to 1000g moringa seeds
Stirred in oil, oil ben 3 is made.
In obtained oil ben 3, oleic acid content is that 73.1% , behenic acid contents are 3.23%, and nutritive value is high, according to
Arrhenius empirical equations, thus it is speculated that its shelf-life under conditions of room temperature, lucifuge is 78 months.
Comparative example 1
A kind of preparation of oil ben, specifically comprises the following steps：
(1) microwave treatment：Shell after fresh moringa seeds are dried, after microwave power 700W processing heating 4min, crush, mistake
100 mesh sieves, crush 3h in airslide disintegrating mill, obtain the moringa seeds powder that average grain diameter is 8 μm；
(2) thermophilic digestion：By obtained moringa seeds powder under 120 DEG C of water vapor conditions boiling 30min；
(3) it is high-pressure homogeneous：Learn from else's experience the moringa seeds powder after thermophilic digestion, according to solid-liquid ratio 1:8g/mL adds deionized water, with
10000rpm speed is sheared 20 minutes, is crossed colloid mill 3 times, is obtained moringa seeds homogenate, high-pressure homogeneous 2 times of 40MPa；
(4) ultrasonic wave added alkalinity extraction：It is 9.0 that sodium hydroxide regulation pH value is added in moringa seeds powder homogenate, ultrasound
Power 800W, temperature are 60 DEG C of extraction 20min, are cooled to room temperature, obtain suspension；
(5) moringa seeds digest：The pH value of suspension is adjusted to 5.0, adds 4% alphalise starch that quality is moringa seeds quality
The composite plant hydrolase of enzyme and trade names Viscozyme L, the addition of alpha-amylase account for the 80% of total enzyme amount, commodity board
The addition of number Viscozyme L composite plant hydrolase accounts for the 20% of total enzyme amount, is digested 6 hours under conditions of 56 DEG C；Plant
After thing enzymatic hydrolysis, regulation pH value to 8.0,6% compound protease and trade names that quality is moringa seeds quality are added
NS37071 alkali protease, the addition of compound protease account for the 30% of total enzyme amount, trade names NS37071 alkaline egg
The addition of white enzyme accounts for the 70% of total enzyme amount, is digested 16 hours under conditions of 56 DEG C；120 DEG C of heating 40min, are cooled to room
Wen Hou, -24 DEG C of freezing 12h；Place 12h for 8 DEG C and carry out low temperature defrosting, 8000g centrifugation 30min, obtain seed oil of Moringa oleigera 4, moringa seeds
The recovery rate of oil 4 is 93%；
(6) preparation of oil ben：0.2g TBHQs (TBHQ) are dissolved in 5mL absolute ethyl alcohols, are added to
Stirred in 1000g seed oil of Moringa oleigera, oil ben 4 is made.
In obtained oil ben 4, oleic acid content is that 73.3% , behenic acid contents are 3.13%, and nutritive value is high, according to
Arrhenius empirical equations, thus it is speculated that its shelf-life under conditions of room temperature, lucifuge is 68 months.
Comparative example 2
A kind of preparation of oil ben, specifically comprises the following steps：
(1) microwave treatment：Shell after fresh moringa seeds are dried, after microwave power 700W heats 4min, crush, mistake
100 mesh sieves, crush 3h in airslide disintegrating mill, obtain the moringa seeds powder that average grain diameter is 8 μm；
(2) thermophilic digestion：By obtained moringa seeds powder under 120 DEG C of water vapor conditions boiling 30min；
(3) it is high-pressure homogeneous：Learn from else's experience the moringa seeds powder after thermophilic digestion, according to solid-liquid ratio 1:8g/mL adds deionized water, with
10000rpm speed is sheared 20 minutes, is crossed colloid mill 3 times, is obtained moringa seeds homogenate, high-pressure homogeneous 2 times of 40MPa；
(4) ultrasonic wave added alkalinity extraction：It is 9.0 that sodium hydroxide regulation pH value is added in moringa seeds powder homogenate, ultrasound
Power 800W, temperature are 60 DEG C of extraction 20min, are cooled to room temperature, obtain suspension；
(5) moringa seeds digest：The pH value of suspension is adjusted to 5.0, adds 4% alphalise starch that quality is moringa seeds quality
The composite plant hydrolase of enzyme and trade names Viscozyme L, the addition of alpha-amylase account for the 80% of total enzyme amount, commodity board
The addition of number Viscozyme L composite plant hydrolase accounts for the 20% of total enzyme amount, is digested 6 hours under conditions of 56 DEG C；Plant
After thing enzymatic hydrolysis, regulation pH value to 8.0,6% compound protease and trade names that quality is moringa seeds quality are added
NS37071 alkali protease, the addition of compound protease account for the 30% of total enzyme amount, trade names NS37071 alkaline egg
The addition of white enzyme accounts for the 70% of total enzyme amount, is digested 16 hours under conditions of 56 DEG C；120 DEG C of heating 40min, are cooled to room
Wen Hou, -24 DEG C of freezing 12h；Place 12h for 8 DEG C and carry out low temperature defrosting, 8000g centrifugation 30min, obtain seed oil of Moringa oleigera 5；
The obtained recovery rate of seed oil of Moringa oleigera 5 is 93%, and oleic acid content is that 72.5% , behenic acid contents are 3.21%, nutrition
Value is high, according to Arrhenius empirical equations, thus it is speculated that its shelf-life under conditions of room temperature, lucifuge is 14 months.
The total fatty acids composition of oil ben prepared by embodiment 1~3 and comparative example 1~2 is as shown in table 1.
The oil ben total fatty acids of table 1 form
As shown in Table 1, similar, the oleic acid content of aliphatic acid composition of embodiment 1-3 and the oil ben obtained by comparative example 1-2
Highest, more than 72%, for behenyl acid content more than 3%, grease extraction efficiency is higher than 90%；And the seed oil of Moringa oleigera in embodiment 1-3
Moringa oleifera leaf extractive is with the addition of, and that comparative example 1 is added is TBHQ, comparative example 2 is not added with any antioxidant, is protected with reference to grease
The difference of matter phase, moringa oleifera leaf extractive is remarkably improved seed oil of Moringa oleigera oxidation stability, and seed oil of Moringa oleigera is resisted better than TBHQ
Oxidation.
The present invention uses microwave treatment, thermophilic digestion, high-pressure homogeneous and ultrasonic wave added alkalinity extraction pre-treating technology,
Combine plant hydrolyzed-enzyme enzymolysis, protease hydrolyzed, high-temperature process, cryogenic freezing again, thaw and low-temperature and high-speed centrifuge to obtain it is peppery
Wooden seed oil, then by the way that addition digests through plant hydrolyzed-enzyme in seed oil of Moringa oleigera, protease hydrolyzed, ethanol extract and macroreticular resin
The prepared moringa oleifera leaf extractive of enrichment, obtained oil ben.Using the preparation-obtained moringa seeds of efficient, green extraction
Oil extract rate is high, and in obtained oil ben, organic solvent-free residual, no chemical additive, nutritive value is high, and long shelf-life can
It is widely used in food industry.
Above example is only preferrred embodiment of the present invention, is only used for explaining the present invention, is not intended to limit the present invention, this
Change that art personnel are made under without departing from spirit of the invention, replacement, modification etc. all should belong to the guarantor of the present invention
Protect scope.
Claims (10)
1. a kind of preparation method of oil ben, it is characterised in that using microwave treatment, thermophilic digestion, high-pressure homogeneous and ultrasonic
The pre-treating technology of alkalinity extraction is aided in, joint plant hydrolyzed-enzyme enzymolysis, protease hydrolyzed, high-temperature process, cryogenic freezing, is thawed
And the handling process of low-temperature and high-speed centrifugation, obtain seed oil of Moringa oleigera；Finally, by adding moringa oleifera leaf extractive, obtained oil ben,
Specifically comprise the following steps：
（1）Microwave treatment：Shelled after fresh moringa seeds are dried, microwave treatment, crush, sieving, ultramicro grinding, obtain moringa seeds
Powder；
（2）Thermophilic digestion：Obtained moringa seeds powder is subjected to thermophilic digestion；
（3）It is high-pressure homogeneous：Learn from else's experience the moringa seeds powder after thermophilic digestion, add deionized water, cross colloid mill after high speed shear, then enter
Horizontal high voltage homogeneous, obtain moringa seeds homogenate；
（4）Ultrasonic wave added alkalinity extraction：The addition sodium hydroxide regulation pH value in moringa seeds powder homogenate, ultrasound assisted extraction,
Room temperature is cooled to, obtains suspension；
（5）Moringa seeds digest：The pH value of suspension is adjusted, after adding plant hydrolyzed-enzyme enzymolysis, adjusts pH value, protease is added and enters
Row enzymolysis, high-temperature process, is cooled to room temperature, carries out cryogenic freezing processing, and low temperature thaws, and low-temperature and high-speed centrifugation, obtains moringa seeds
Oil；
（6）The preparation of oil ben：Moringa oleifera leaf extractive is dissolved in absolute ethyl alcohol, added in seed oil of Moringa oleigera, stirred, is made
Obtain the oil ben.
A kind of 2. preparation method of oil ben according to claim 1, it is characterised in that step（1）In, at the microwave
Reason power is the heated under microwave conditions 2-4 min in 500-700 W；The sieving was 100 mesh sieves；The ultramicro grinding is
2-3 h are crushed in airslide disintegrating mill, the average grain diameter for the moringa seeds powder for crushing to obtain is 8-12 μm；Step（2）In, it is described
Thermophilic digestion is the boiling 20-30 min under 100-120 DEG C of water vapor conditions.
A kind of 3. preparation method of oil ben according to claim 1, it is characterised in that step（3）In, after thermophilic digestion
Moringa seeds powder and deionized water solid-liquid ratio be 1:6~8 g/mL；The high speed shear is the speed in 8000 ~ 10000 rpm
Shearing 10 ~ 20 minutes；The number for crossing colloid mill is 2 ~ 3 times；The high-pressure homogeneous pressure is 20 ~ 40 MPa, and high pressure is equal
The number of matter is 2 ~ 3 times；Step（4）In, the regulation pH value is that regulated value pH value is 7.0 ~ 9.0；The ultrasound assisted extraction
Ultrasonic power be 600-800 W, the time is 10-20 min, and temperature is 40 ~ 60 DEG C.
A kind of 4. preparation method of oil ben according to claim 1, it is characterised in that step（5）In, adjust suspension
PH value to 4.4-5.0；The plant hydrolyzed-enzyme enzymolysis digests 4 ~ 6 hours under the conditions of being 50 ~ 56 DEG C；Plant hydrolyzed-enzyme digests
Afterwards, pH value is adjusted to 7.0-8.0；The protease hydrolyzed digests 12 ~ 16 hours under conditions of being 50 ~ 56 DEG C；At the high temperature
Manage as 100-120 DEG C of heat treatment 20-40 min；The cryogenic freezing processing is -18 ~ -24 DEG C of freezing 8-12 h；The low temperature
Thaw and place 8-12 h for 4-8 DEG C；Under the conditions of the low-temperature centrifugation is 4-8 DEG C, 6000 ~ 8000g centrifuges 20 ~ 30min；It is described peppery
The extraction yield of wooden seed oil>90%.
A kind of 5. preparation method of oil ben according to claim 1, it is characterised in that step（5）In, the vegetation water
The addition for solving enzyme is the 2 ~ 4% of moringa seeds quality；The plant hydrolyzed-enzyme is alpha-amylase and trade names Viscozyme L
Composite plant hydrolase, the addition of alpha-amylase accounts for the 60-80% of total enzyme amount, trade names Viscozyme L compound plant
The addition of thing hydrolase accounts for the 20-40% of total enzyme amount；The addition of the protease is the 4 ~ 6% of moringa seeds quality；The egg
White enzyme is compound protease and trade names NS37071 alkali protease, and the addition of compound protease accounts for the 10- of total enzyme amount
30%, the addition of trade names NS37071 alkali protease accounts for the 70-90% of total enzyme amount.
A kind of 6. preparation method of oil ben according to claim 1, it is characterised in that step（6）In, the leaf of Moringa
Extract extracts to obtain as follows：
Moringa cured leaf is taken, crushes, sieving, obtains leaf of Moringa powder, adds deionized water, well mixed to obtain suspension, regulation is mixed
The pH value of suspension, after adding plant hydrolyzed-enzyme enzymolysis, pH value is adjusted, add protease and digested, add absolute ethyl alcohol, heating
Refluxing extraction, after extract solution is cooled to room temperature, centrifugation is removed slag, and takes supernatant, is concentrated under reduced pressure, and freeze-drying, takes freeze-dried powder molten
Yu Shui, macroporous resin column is crossed, using ethanol solution gradient elution, collect eluent, freeze-drying, obtain moringa oleifera leaf extractive.
7. the preparation method of a kind of oil ben according to claim 6, it is characterised in that the sieving was 40 mesh sieves；
The leaf of Moringa powder and the solid-liquid ratio of deionized water are 1:8~10g/mL；The pH value of suspension is adjusted to 4.4-5.0；The plant
The addition of hydrolase is the 2 ~ 4% of Moringa cured leaf quality；The plant hydrolyzed-enzyme is the compound of trade names Viscozyme L
Plant hydrolyzed-enzyme；The plant hydrolyzed-enzyme enzymolysis digests 4 ~ 6 hours under the conditions of being 50 ~ 56 DEG C；After plant hydrolyzed-enzyme enzymolysis, regulation
PH value is to 7.0-8.0；The addition of the protease is the 4 ~ 6% of Moringa leaf quality；The protease is pancreatin and trade names
NS37071 alkali protease, the addition of pancreatin account for the 40-60% of total enzyme amount, trade names NS37071 alkali protease
Addition account for the 40-60% of total enzyme amount；The protease hydrolyzed digests 6 ~ 8 hours under the conditions of being 50 ~ 56 DEG C.
8. the preparation method of a kind of oil ben according to claim 6, it is characterised in that the addition of absolute ethyl alcohol is to make
Ethanol content reaches 30 ~ 50wt% in system；It is described to be heated to reflux being heated to reflux 1-2h under the conditions of 90-100 DEG C；The centrifugation
10 ~ 20min is centrifuged for 4000 ~ 6000g；Described be concentrated under reduced pressure to be concentrated into solid content is 20 ~ 30%；Freeze-dried powder is dissolved in
Concentration after water is 100-200 mg/mL；The macroreticular resin is Mitsubishi chemistry macroporous absorbent resin SP207；The ladder
Degree elution is using 0-50 vol% ethanol solution gradient elutions, is specially：1-2 column volume uses 100vol% water elutions, 3-5
Individual column volume is using 100-60 vol% water, 0-40 vol% ethanol elutions, and 6-7 column volume is using 50 vol% water, 50 vol%
Ethanol elution, collect 50 vol% ethanol eluates.
A kind of 9. preparation method of oil ben according to claim 1, it is characterised in that step（6）In, the leaf of Moringa
The dissolving ratio of extract and absolute ethyl alcohol is 0.1-0.2:3-5 g /mL；The matter of the moringa oleifera leaf extractive and seed oil of Moringa oleigera
It is 1-2 to measure ratio:10000.
A kind of 10. oil ben as made from the preparation method described in claim any one of 1-9, it is characterised in that oleic acid content>
72% , behenic acid contents>3%.
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| CN108219920A (en) * | 2018-02-06 | 2018-06-29 | 佛山科学技术学院 | A kind of extracting method of seed oil of Moringa oleigera |
| CN112088904A (en) * | 2020-10-22 | 2020-12-18 | 丽水市农林科学研究院 | Preparation method and application of paris polyphylla extractive solution |
| CN112574811A (en) * | 2020-12-15 | 2021-03-30 | 佳格食品(厦门)有限公司 | Moderate processing method of sunflower seed oil |
| US11903390B1 (en) | 2023-09-05 | 2024-02-20 | King Faisal University | Enhanced Curcuma longa productivity and medicinal values by using Moringa oleifera leaf extract |
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| CN106282282A (en) * | 2016-08-10 | 2017-01-04 | 华南农业大学 | A kind of extract oils and fats and albumen and/or the method for glucosides in moringa seeds simultaneously |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108219920A (en) * | 2018-02-06 | 2018-06-29 | 佛山科学技术学院 | A kind of extracting method of seed oil of Moringa oleigera |
| CN112088904A (en) * | 2020-10-22 | 2020-12-18 | 丽水市农林科学研究院 | Preparation method and application of paris polyphylla extractive solution |
| CN112574811A (en) * | 2020-12-15 | 2021-03-30 | 佳格食品(厦门)有限公司 | Moderate processing method of sunflower seed oil |
| US11903390B1 (en) | 2023-09-05 | 2024-02-20 | King Faisal University | Enhanced Curcuma longa productivity and medicinal values by using Moringa oleifera leaf extract |
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