CN105815779A - Comprehensive processing method of rapeseed meal - Google Patents
Comprehensive processing method of rapeseed meal Download PDFInfo
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- CN105815779A CN105815779A CN201610364008.5A CN201610364008A CN105815779A CN 105815779 A CN105815779 A CN 105815779A CN 201610364008 A CN201610364008 A CN 201610364008A CN 105815779 A CN105815779 A CN 105815779A
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- rapeseed cake
- enzymolysis
- crude enzyme
- enzyme liquid
- sodium phosphate
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- 235000019779 Rapeseed Meal Nutrition 0.000 title abstract 8
- 239000004456 rapeseed meal Substances 0.000 title abstract 8
- 238000003672 processing method Methods 0.000 title abstract 2
- PCMORTLOPMLEFB-ONEGZZNKSA-N sinapic acid Chemical compound COC1=CC(\C=C\C(O)=O)=CC(OC)=C1O PCMORTLOPMLEFB-ONEGZZNKSA-N 0.000 claims abstract description 78
- PCMORTLOPMLEFB-UHFFFAOYSA-N sinapinic acid Natural products COC1=CC(C=CC(O)=O)=CC(OC)=C1O PCMORTLOPMLEFB-UHFFFAOYSA-N 0.000 claims abstract description 49
- QHJGZUSJKGVMTF-UHFFFAOYSA-N canolol Chemical compound COC1=CC(C=C)=CC(OC)=C1O QHJGZUSJKGVMTF-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000007788 liquid Substances 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000001035 drying Methods 0.000 claims abstract description 12
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 230000000433 anti-nutritional effect Effects 0.000 claims abstract description 5
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 5
- 238000006114 decarboxylation reaction Methods 0.000 claims abstract description 3
- 235000004977 Brassica sinapistrum Nutrition 0.000 claims description 108
- 240000002791 Brassica napus Species 0.000 claims description 107
- 238000010438 heat treatment Methods 0.000 claims description 34
- 102000004190 Enzymes Human genes 0.000 claims description 33
- 108090000790 Enzymes Proteins 0.000 claims description 33
- -1 sinapic acid choline ester Chemical class 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 26
- 239000007853 buffer solution Substances 0.000 claims description 23
- 239000001488 sodium phosphate Substances 0.000 claims description 23
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 23
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 23
- 229960001231 choline Drugs 0.000 claims description 20
- 230000002255 enzymatic effect Effects 0.000 claims description 19
- 210000000582 semen Anatomy 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 230000035784 germination Effects 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 11
- 238000001976 enzyme digestion Methods 0.000 claims description 10
- 241001301148 Brassica rapa subsp. oleifera Species 0.000 claims description 9
- 238000000605 extraction Methods 0.000 claims description 9
- 235000005637 Brassica campestris Nutrition 0.000 claims description 8
- 230000010355 oscillation Effects 0.000 claims description 8
- KSEBMYQBYZTDHS-HWKANZROSA-M (E)-Ferulic acid Natural products COC1=CC(\C=C\C([O-])=O)=CC=C1O KSEBMYQBYZTDHS-HWKANZROSA-M 0.000 claims description 7
- 229940114124 ferulic acid Drugs 0.000 claims description 7
- KSEBMYQBYZTDHS-UHFFFAOYSA-N ferulic acid Natural products COC1=CC(C=CC(O)=O)=CC=C1O KSEBMYQBYZTDHS-UHFFFAOYSA-N 0.000 claims description 7
- 235000001785 ferulic acid Nutrition 0.000 claims description 7
- QURCVMIEKCOAJU-UHFFFAOYSA-N trans-isoferulic acid Natural products COC1=CC=C(C=CC(O)=O)C=C1O QURCVMIEKCOAJU-UHFFFAOYSA-N 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 4
- 230000001186 cumulative effect Effects 0.000 claims description 4
- 230000007062 hydrolysis Effects 0.000 claims description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 101001065065 Aspergillus awamori Feruloyl esterase A Proteins 0.000 claims description 2
- 230000009514 concussion Effects 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- HUJXHFRXWWGYQH-UHFFFAOYSA-O sinapine Chemical compound COC1=CC(\C=C\C(=O)OCC[N+](C)(C)C)=CC(OC)=C1O HUJXHFRXWWGYQH-UHFFFAOYSA-O 0.000 abstract description 4
- 238000007669 thermal treatment Methods 0.000 abstract 2
- 239000007787 solid Substances 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 13
- 239000000203 mixture Substances 0.000 description 9
- 235000013824 polyphenols Nutrition 0.000 description 9
- 150000007965 phenolic acids Chemical class 0.000 description 8
- 150000008442 polyphenolic compounds Chemical class 0.000 description 8
- 238000004128 high performance liquid chromatography Methods 0.000 description 6
- 239000000284 extract Substances 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 108090000623 proteins and genes Proteins 0.000 description 3
- 102000004169 proteins and genes Human genes 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 230000002790 anti-mutagenic effect Effects 0.000 description 2
- 230000003026 anti-oxygenic effect Effects 0.000 description 2
- 229910001651 emery Inorganic materials 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 235000014593 oils and fats Nutrition 0.000 description 2
- 150000002989 phenols Chemical class 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- 235000014698 Brassica juncea var multisecta Nutrition 0.000 description 1
- 235000006008 Brassica napus var napus Nutrition 0.000 description 1
- 235000006618 Brassica rapa subsp oleifera Nutrition 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 244000046052 Phaseolus vulgaris Species 0.000 description 1
- 235000010627 Phaseolus vulgaris Nutrition 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000003471 anti-radiation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000019658 bitter taste Nutrition 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 208000015606 cardiovascular system disease Diseases 0.000 description 1
- 208000026106 cerebrovascular disease Diseases 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 235000019621 digestibility Nutrition 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000006911 enzymatic reaction Methods 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 235000021050 feed intake Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 238000011321 prophylaxis Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 229930000044 secondary metabolite Natural products 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/80—Food processing, e.g. use of renewable energies or variable speed drives in handling, conveying or stacking
- Y02P60/87—Re-use of by-products of food processing for fodder production
Landscapes
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Edible Oils And Fats (AREA)
Abstract
The invention relates to a comprehensive processing method of rapeseed meal .The method includes the following steps of firstly, conducting enzymolysis, wherein enzymolysis is conducted on rapeseed meal, and lots of sinapine in rapeseed meal is converted into sinapic acid through enzymolysis; secondly, conducting separation, wherein solid and liquid separation is conducted to obtain rapeseed meal residues; thirdly, conducting drying, wherein residues are put in an oven to be dried at low temperature; fourthly, conducting thermal treatment, wherein dried rapeseed meal residues are subjected to thermal treatment, so sinapic acid is converted into a target product canolol through thermal decarboxylation .The high-valued rapeseed meal of which anti-nutritional factors are remarkably reduced and the antioxidant canolol content is remarkably increased is obtained .The method has the advantages of being easy and convenient to operate, easy to implement and the like and has great value in high-valued utilization of rapeseed meal.
Description
Technical field
The present invention relates to Food Chemistry and rapeseed cake technical field of comprehensive utilization, be specifically related to the integrated conduct method of a kind of rapeseed cake.
Background technology
Plant polyphenol is the secondary metabolite that a class is widely present in plant, there is good antioxygenic property, in all many-sides such as anticancer, Antiradiation injury, resisting pathogenic microbes, blood fat reducing, preventing and treating cardiovascular system diseases, there is superior physiologically active and function.Polyphenol content in Semen Brassicae campestris is far above other oil crop, reaches 2-4%, containing about 3% in dregs of rapeseed cake after defat, is approximately 30 times of bean cake.The phenolic hydroxyl structure of polyphenol from rapeseed is allowed to have stronger Scavenging ability and antioxygenic property, can develop healthcare products and the Natural antioxidant of slow down aging, prophylaxis of tumours and cardio-cerebrovascular diseases.
Polyphenol from rapeseed is divided into phenolic acid and tannin, and phenolic acid includes again free phenolic acid and esterification phenolic acid, and wherein free phenolic acid accounts for the 9-16% of total phenols, and sinapic acid (Sinapicacid) is topmost free phenolic acid, accounts for the 70-85% of free phenolic acid total amount；Sinapic acid choline ester. (Sinapine) is the cholinester of sinapic acid, is topmost esterification phenolic acid in Semen Brassicae campestris, accounts for the 80% of total phenols, and the content in Semen Allii Tuberosi is about 0.4-1.0%.After squeezing and extraction oil producing, overwhelming majority polyphenol all remains in dregs of rapeseed cake (abbreviation rapeseed cake), and therefore rapeseed cake is good polyphenol source.
2,6-dimethoxy-4 '-vinylphenol (2,6-dimethoxy-4-vinylphenol) it is a kind of novel polyphenol from rapeseed, reported by Koski of Univ Helsinki Finland et al. first, subsequently Wakamatsu et al. of Japan also in double low Semen Allii Tuberosi (canola) crude oils of Canada separation, purification, identify this material, and the most named canolol.Compared with sinapic acid, the antioxidant activity of Canolol is higher, and there is antimutagenic characteristic, therefore, this compound has very important using value and potentiality, can not only be used for antioxidant and be applied to the storage of oils and fats, extend oils and fats shelf life, again can be as active component development function product or medicine.
Sinapic acid choline ester. has bitterness and affects animal feed intake, makes egg have fishlike smell, is easily combined with protein and enzyme and affects the digestibility of protein simultaneously, one of topmost antinutritional factor during therefore sinapic acid choline ester. is rapeseed cake.Therefore developing the method for comprehensive utilization of a kind of rapeseed cake, the higher value application for rapeseed cake has important value.
Summary of the invention
It is an object of the invention to provide the integrated conduct method of a kind of rapeseed cake, it has the characteristics such as easy and simple to handle, easy realization, and the higher value application for rapeseed cake has important value.
To achieve these goals, the technical solution used in the present invention is as follows:
The integrated conduct method of a kind of rapeseed cake, comprises the steps:
(1) enzymolysis: rapeseed cake is carried out enzyme digestion reaction, makes a large amount of sinapic acid choline ester. enzymolysis existed in rapeseed cake be converted into sinapic acid；
(2) separate: solid-liquid separation, obtain rapeseed cake residue；
(3) it is dried: residue is placed in cold drying in baking oven；
(4) heat treatment: dry rapeseed cake residue is carried out heat treatment, makes sinapic acid thermal decarboxylation be converted into target product canolol, obtains that antinutritional factor substantially reduces, antioxidant canolol content dramatically increases high-valued rapeseed cake.
According to above scheme, the enzymolysis of described step (1) is: adds buffer solution of sodium phosphate in rapeseed cake, adds enzymatic solution, and fully concussion carries out enzyme digestion reaction；
Described enzymatic solution is ferulic acid ester enzymatic solution or the crude enzyme liquid being obtained by extraction from germination Semen Allii Tuberosi；
Described crude enzyme liquid is to be germinateed in climatic chamber by the Semen Brassicae campestris with germination vigor, adds water as required during germination, makes Semen Allii Tuberosi keep moisture state；Pulverize after terminating germinateing by Brassica campestris L bud, then with buffer solution of sodium phosphate stirring extraction, after centrifugation, take what supernatant i.e. crude enzyme liquid obtained.
According to such scheme, in described step (1), when enzymatic solution is ferulic acid ester enzymatic solution, feruloyl esterase enzyme unit (U) alive is 0.1～1.0:1 with quality (g) ratio of substrate (rapeseed cake)；
Rapeseed cake quality is 1:5～8 (g:mL) with the ratio of the cumulative volume of buffer solution of sodium phosphate and enzymatic solution；
Hydrolysis temperature scope is 25～60 DEG C, and oscillation rate is 100～300rmp, and enzymolysis time is 1～24h.
According to such scheme, when in described step (1), enzymatic solution is the crude enzyme liquid being obtained by extraction in germination Semen Allii Tuberosi, crude enzyme liquid is 1 (ml): 0.5～1.25 (g) with the volume mass ratio of rapeseed cake；
Rapeseed cake quality is 1:3～8 (g:mL) with the ratio of the cumulative volume of buffer solution of sodium phosphate and enzymatic solution；
Hydrolysis temperature is 30～50 DEG C, and enzymolysis time is 1～20h.
According to such scheme, in described crude enzyme liquid preparation process, the germination temperature of Semen Brassicae campestris is 30 ± 2 DEG C, and germinating time is 4～5 days；
According to such scheme, in described crude enzyme liquid preparation process, Brassica campestris L bud is 1:2～10g/mL with the mass volume ratio of buffer solution of sodium phosphate.
According to such scheme, in described crude enzyme liquid preparation process, the concentration of buffer solution of sodium phosphate is 5～15mM, and pH value is 6.5～7.5.
According to such scheme, in described crude enzyme liquid preparation process, extraction time is 10～30min.
According to such scheme, in described crude enzyme liquid preparation process, stirring is mechanical agitation or magnetic agitation, and mixing speed is 150～300rmp；Using centrifugal rotational speed is 10000～15000rmp.
According to such scheme, in described step (2), the method for solid-liquid separation can be centrifugal, it is also possible to being to filter, centrifugal rotational speed is 5000～15000rmp.
According to such scheme, in described step (3), baking temperature is 30～65 DEG C, and drying time is 2～6h.
According to above scheme, the concentration of the buffer solution of sodium phosphate used in enzymolysis process in described step (1) is 10～50mM, and pH value is 6.5～7.5.
According to such scheme, in described step (4), heat treatment mode can be steam heating, microwave heating, oil bath heating etc..
According to such scheme, in described step (4), when using steam heating, vapor (steam) temperature is 140～160 DEG C, and heat time heating time is 5～20min.
According to such scheme, in described step (4), when using microwave heating, microwave power is 400～800w, and the microwave time is 5～9min.
According to such scheme, in described step (4), when using oil bath heating, oil bath temperature is 140～160 DEG C, and heat time heating time is 10～30min.
The rapeseed cake integrated conduct method that the present invention provides can efficiently utilize the sinapic acid choline ester. in rapeseed cake, being allowed to Efficient Conversion is canolol, on the one hand the content of antinutritional factor sinapic acid choline ester. in rapeseed cake is advantageously reduced, it is eventually converted into antioxidant activity higher simultaneously, and there is the canolol of antimutagenic characteristic, can greatly improve rapeseed cake value and potentiality.
The invention has the beneficial effects as follows:
(1) integrated artistic of the present invention is simple and direct, simple to operate, easily realizes.
(2) present invention uses enzymatic method to make sinapic acid choline ester. be converted into sinapic acid, has mild condition, an advantage that efficiency is high.
(3) present invention uses the method for cold drying to remove moisture in rapeseed cake, has low cost, polyphenol from rapeseed is destroyed little advantage.
(4) present invention uses steam, microwave and oil bath that rapeseed cake is carried out heat treatment, wherein steam and microwave heating have that the time is short, efficiency is high, cake protein are destroyed little advantage, oil bath is relatively long for heat time heating time, but has low cost, easy-operating advantage.
Detailed description of the invention
Below in conjunction with embodiment, technical scheme is illustrated.
Example 1:
The method of comprehensive utilization of a kind of rapeseed cake, comprises the steps:
(1) enzymolysis: weigh 50g rapeseed cake in conical flask, be separately added into 299mL concentration be 50mM, pH value be 7.0 buffer solution of sodium phosphate and 1mL ferulic acid ester enzymatic solution (be equivalent to 7 enzymes live units), be sufficiently stirred for making system mix homogeneously.Conical flask is placed in shaking bath, arrange temperature be 40 DEG C, oscillation rate be 200rmp, carry out enzyme digestion reaction, enzymolysis reaction after 16h.
(2) separate: taking out conical flask and be cooled to room temperature, centrifugation solution and rapeseed cake, centrifuge speed is 12000rmp, obtains rapeseed cake residue.
(3) being dried: being placed in baking oven by rapeseed cake residue, arranging temperature is 60 DEG C, take out and be cooled to room temperature after being dried 2.5h, now rapeseed cake moisture is 9.08%.
(4) heat treatment: be placed in plate by dried rapeseed cake, put into microwave oven, arranging microwave power is 560w, and microwave heating 7min, now temperature of charge reaches 162 DEG C.Room temperature it is cooled to after taking-up.
Detecting through high performance liquid chromatography, after enzymolysis and centrifugal drying, in rapeseed cake, sinapic acid choline ester. content is reduced to 0.22mg/g by the 7.71mg/g before enzymolysis, and sinapic acid content is increased to 5.60mg/g by 1.23mg/g, sinapic acid choline ester. almost all enzymolysis is described, and changes into sinapic acid；After microwave heating treatment, in rapeseed cake, sinapic acid content is reduced to 1.68mg/g, Canolol content by 5.60mg/g and increases to 1.05mg/g.
Example 2:
The method of comprehensive utilization of a kind of rapeseed cake, comprises the steps:
(1) enzymolysis: weigh 5g rapeseed cake in conical flask, be separately added into 30mL concentration be 20mM, pH value be 7.0 buffer solution of sodium phosphate and 120 μ L ferulic acid ester enzymatic solution (be equivalent to 0.84 enzyme live in unit), be sufficiently stirred for making system mix homogeneously.Conical flask is placed in shaking bath, arrange temperature be 35 DEG C, oscillation rate be 120rmp, carry out enzyme digestion reaction, enzymolysis reaction after 8h.
(2) separate: take out conical flask and be cooled to room temperature, filter and separate solution and rapeseed cake, obtain rapeseed cake residue.
(3) being dried: being placed in baking oven by rapeseed cake residue, arranging temperature is 55 DEG C, take out and be cooled to room temperature after being dried 2h, now rapeseed cake moisture is 7.34%.
(4) heat treatment: dried rapeseed cake is placed in beaker sealing, puts into high-pressure sterilizing pot, arranges temperature 160 DEG C, heats 8min, is cooled to room temperature after taking-up.
Detecting through high performance liquid chromatography, after enzymolysis and centrifugal drying, in rapeseed cake, sinapic acid choline ester. content is reduced to not detect by the 11.15mg/g before enzymolysis, and sinapic acid content is increased to 8.64mg/g by 3.95mg/g, the whole enzymolysis of sinapic acid choline ester. is described, and changes into sinapic acid；After steam heat treated, in rapeseed cake, sinapic acid content is reduced to 1.38mg/g, Canolol content by 8.64mg/g and increases to 1.69mg/g.
Example 3:
The method of comprehensive utilization of a kind of rapeseed cake, comprises the steps:
(1) enzymolysis: weigh 10g rapeseed cake in conical flask, be separately added into 50mL concentration be 15mM, pH value be 7.0 buffer solution of sodium phosphate and 500 μ L ferulic acid ester enzymatic solution (be equivalent to 3.5 enzymes live in units), be sufficiently stirred for making system mix homogeneously.Conical flask is placed in shaking bath, arrange temperature be 45 DEG C, oscillation rate be 200rmp, carry out enzyme digestion reaction, enzymolysis reaction after 5h.
(2) separate: taking out conical flask and be cooled to room temperature, centrifugation solution and rapeseed cake, centrifuge speed is 10000rmp, obtains rapeseed cake residue.
(3) being dried: being placed in baking oven by rapeseed cake residue, arranging temperature is 45 DEG C, take out and be cooled to room temperature after being dried 3h, now rapeseed cake moisture is 6.81%.
(4) heat treatment: be placed in round-bottomed flask by dried rapeseed cake, pre-sets and after oil bath temperature reaches 150 DEG C, is immersed by round-bottomed flask in oil bath, heats 20min, is cooled to room temperature after taking-up.
Detecting through high performance liquid chromatography, after enzymolysis and centrifugal drying, in rapeseed cake, sinapic acid choline ester. content is reduced to 0.14mg/g by the 8.56mg/g before enzymolysis, and sinapic acid content is increased to 6.07mg/g by 1.58mg/g, sinapic acid choline ester. almost all enzymolysis is described, and changes into sinapic acid；After oil bath heat treated, in rapeseed cake, sinapic acid content is reduced to 1.38mg/g, Canolol content by 6.07mg/g and increases to 1.83mg/g.
Example 4:
The method of comprehensive utilization of a kind of rapeseed cake, comprises the steps:
(1) preparation of germination Semen Allii Tuberosi crude enzyme liquid:
Taking 5, germination box, first 4 layers of toilet paper of paving are in bottom, repave one layer of emery cloth above, moistening of sprinkling water.Weighing 3g Semen Brassicae campestris, on the dispersed culture dish being covered with moistening emery cloth, watering keeps Semen Allii Tuberosi to be in moisture state, is placed in by culture dish in 30 DEG C of climatic chambers, the most suitably adds water.After 4 days, Brassica campestris L bud is taken off and be placed in-20 DEG C of refrigerators, terminate germinateing.Being pulverized by Brassica campestris L bud, weigh 10g and be placed in conical flask, addition 50mL concentration is 10mM, pH value is the buffer solution of sodium phosphate of 7.0, and mix homogeneously is placed on magnetic stirring apparatus, arranges rotating speed 250rmp, extracts 20min.Under the conditions of rotating speed is 12000rmp, it is centrifugally separating to obtain supernatant afterwards, obtains crude enzyme liquid.
(2) enzymolysis: weigh 5g rapeseed cake in conical flask, be separately added into 20mL concentration be 10mM, pH value be 7.5 buffer solution of sodium phosphate and 10mL crude enzyme liquid, be sufficiently stirred for making system mix homogeneously.Conical flask is placed in shaking bath, arrange temperature be 40 DEG C, oscillation rate be 300rmp, carry out enzyme digestion reaction, enzymolysis reaction after 18h.
(3) separate: taking out conical flask and be cooled to room temperature, centrifugation solution and rapeseed cake, centrifuge speed is 10000rmp, obtains rapeseed cake residue.
(4) being dried: being placed in baking oven by rapeseed cake residue, arranging temperature is 60 DEG C, take out and be cooled to room temperature after being dried 2h, now rapeseed cake moisture is 7.52%.
(5) heat treatment: be placed in round-bottomed flask by rapeseed cake, pre-sets and after oil bath temperature reaches 160 DEG C, is immersed by round-bottomed flask in oil bath, heats 20min, is cooled to room temperature after taking-up.
Detecting through high performance liquid chromatography, after enzymolysis and centrifugal drying, in rapeseed cake, sinapic acid choline ester. content is reduced to 0.47mg/g by the 6.56mg/g before enzymolysis, and sinapic acid content is increased to 4.86mg/g by 1.32mg/g, sinapic acid choline ester. almost all enzymolysis is described, and changes into sinapic acid；After oil bath heat treated, in rapeseed cake, sinapic acid content is reduced to 0.98mg/g, Canolol content by 4.86mg/g and increases to 1.69mg/g.
Example 5:
The method of comprehensive utilization of a kind of rapeseed cake, comprises the steps:
(1) Semen Allii Tuberosi germinates with embodiment 4.Pulverizing terminating the Brassica campestris L bud after germinateing, weigh 10g and be placed in conical flask, addition 80mL concentration is 8mM, pH value is the buffer solution of sodium phosphate of 6.5, and mix homogeneously is placed on magnetic stirring apparatus, arranges rotating speed 300rmp, extracts 25min.It is centrifugally separating to obtain supernatant afterwards, i.e. crude enzyme liquid under the conditions of rotating speed is 15000rmp.(2) enzymolysis: weigh 50g rapeseed cake in conical flask, be separately added into 150mL concentration be 10mM, pH value be 6.5 buffer solution of sodium phosphate and 50mL crude enzyme liquid, be sufficiently stirred for making system mix homogeneously.Conical flask is placed in shaking bath, arrange temperature be 45 DEG C, oscillation rate be 250rmp, carry out enzyme digestion reaction, enzymolysis reaction after 10h.
(3) separate: take out conical flask and be cooled to room temperature, filter and separate solution and rapeseed cake, obtain rapeseed cake residue.
(4) being dried: being placed in baking oven by rapeseed cake residue, arranging temperature is 45 DEG C, take out and be cooled to room temperature after being dried 3h, now rapeseed cake moisture is 7.56%.
(5) being placed in plate by dried rapeseed cake, put into microwave oven, arranging microwave power is 800w, and microwave heating 7min, now temperature of charge reaches 166 DEG C.Room temperature it is cooled to after taking-up.
Detecting through high performance liquid chromatography, after enzymolysis and centrifugal drying, in rapeseed cake, sinapic acid choline ester. content is reduced to 0.48mg/g by the 6.95mg/g before enzymolysis, and sinapic acid content is increased to 5.86mg/g by 1.67mg/g, sinapic acid choline ester. almost all enzymolysis is described, and changes into sinapic acid；After microwave heating treatment, in rapeseed cake, sinapic acid content is reduced to 1.47mg/g, Canolol content by 5.85mg/g and increases to 2.46mg/g.
Example 6
The method of comprehensive utilization of a kind of rapeseed cake, comprises the steps:
(1) Semen Allii Tuberosi germinates with embodiment 4.Simply germination temperature 28 DEG C, germinating time 5 days.
Pulverizing terminating the Brassica campestris L bud after germinateing, weigh 5g and be placed in conical flask, addition 20mL concentration is 15mM, pH value is the buffer solution of sodium phosphate of 7.5, and mix homogeneously is placed on magnetic stirring apparatus, arranges rotating speed 300rmp, extracts 20min.It is centrifugally separating to obtain supernatant afterwards, i.e. crude enzyme liquid under the conditions of rotating speed is 10000rmp.
(2) enzymolysis: weigh 10g rapeseed cake in conical flask, be separately added into 30mL concentration be 12mM, pH value be 7.5 buffer solution of sodium phosphate and 8mL crude enzyme liquid, be sufficiently stirred for making system mix homogeneously.Conical flask is placed in shaking bath, arrange temperature be 35 DEG C, oscillation rate be 300rmp, carry out enzyme digestion reaction, enzymolysis reaction after 10h.
(3) separate: taking out conical flask and be cooled to room temperature, centrifugation solution and rapeseed cake, centrifuge speed is 8000rmp, obtains rapeseed cake residue.
(4) being dried: being placed in baking oven by rapeseed cake residue, arranging temperature is 45 DEG C, take out and be cooled to room temperature after being dried 3h, now rapeseed cake moisture is 7.56%.
(5) heat treatment: dried rapeseed cake is placed in beaker sealing, puts into high-pressure sterilizing pot, arranges temperature 158 DEG C, heats 9min, is cooled to room temperature after taking-up.
Detecting through high performance liquid chromatography, after enzymolysis and centrifugal drying, in rapeseed cake, sinapic acid choline ester. content is reduced to 0.69mg/g by the 5.46mg/g before enzymolysis, and sinapic acid content is increased to 4.57mg/g by 1.24mg/g, sinapic acid choline ester. almost all enzymolysis is described, and changes into sinapic acid；After sterilized pot heat treated, in rapeseed cake, sinapic acid content is reduced to 1.08mg/g, Canolol content by 4.57mg/g and increases to 2.06mg/g.
Above example is only in order to illustrative not limiting technical scheme, although the present invention has been described in detail by above-described embodiment, the person skilled of this area is it is understood that can modify to the present invention or replace on an equal basis, but any amendment and local without departing from spirit and scope of the invention is replaced and all should be contained in scope of the presently claimed invention.
Claims (10)
1. the integrated conduct method of a rapeseed cake, it is characterised in that: comprise the steps:
(1) enzymolysis: rapeseed cake is carried out enzyme digestion reaction, makes a large amount of sinapic acid choline ester. enzymolysis existed in rapeseed cake be converted into sinapic acid；
(2) separate: solid-liquid separation, obtain rapeseed cake residue；
(3) it is dried: residue is placed in cold drying in baking oven；
(4) heat treatment: dry rapeseed cake residue is carried out heat treatment, makes sinapic acid thermal decarboxylation be converted into target product canolol, obtains that antinutritional factor substantially reduces, antioxidant canolol content dramatically increases high-valued rapeseed cake.
The integrated conduct method of rapeseed cake the most according to claim 1, it is characterised in that: the enzymolysis of described step (1) is: adds buffer solution of sodium phosphate in rapeseed cake, adds enzymatic solution, and fully concussion carries out enzyme digestion reaction；
Described enzymatic solution is ferulic acid ester enzymatic solution or the crude enzyme liquid being obtained by extraction from germination Semen Allii Tuberosi；Described crude enzyme liquid is to be germinateed in climatic chamber by the Semen Brassicae campestris with germination vigor, adds water as required during germination, makes Semen Allii Tuberosi keep moisture state；Pulverize after terminating germinateing by Brassica campestris L bud, then with buffer solution of sodium phosphate stirring extraction, after centrifugation, take what supernatant i.e. crude enzyme liquid obtained.
The integrated conduct method of rapeseed cake the most according to claim 2, it is characterized in that: in described step (1), when enzymatic solution is ferulic acid ester enzymatic solution, feruloyl esterase enzyme unit (U) alive is 0.1～1.0:1 with quality (g) ratio of substrate rapeseed cake；
Rapeseed cake quality is 1:5～8 (g/mL) with the ratio of the cumulative volume of buffer solution of sodium phosphate and enzymatic solution；
Hydrolysis temperature scope is 25～60 DEG C, and oscillation rate is 100～300rmp, and enzymolysis time is 1～24h.
The integrated conduct method of rapeseed cake the most according to claim 2, it is characterized in that: when in described step (1), enzymatic solution is the crude enzyme liquid being obtained by extraction in germination Semen Allii Tuberosi, the volume mass of crude enzyme liquid and rapeseed cake is than for 1:0.5～1.25 (ml/g)；
Rapeseed cake quality is 1:3～8 (g/mL) with the ratio of the cumulative volume of buffer solution of sodium phosphate and enzymatic solution；
Hydrolysis temperature is 30～50 DEG C, and enzymolysis time is 1～20h.
The integrated conduct method of rapeseed cake the most according to claim 2, it is characterised in that: in described crude enzyme liquid preparation process, the germination temperature of Semen Brassicae campestris is 30 ± 2 DEG C, and germinating time is 4～5 days；
In described crude enzyme liquid preparation process, extraction time is 10～30min；
In described crude enzyme liquid preparation process, stirring is mechanical agitation or magnetic agitation, and mixing speed is 150～300rmp；Centrifugal rotational speed is 10000～15000rmp.
The integrated conduct method of rapeseed cake the most according to claim 2, it is characterised in that: in described crude enzyme liquid preparation process, Brassica campestris L bud is 1:2～10 (g/mL) with the mass volume ratio of buffer solution of sodium phosphate.
The integrated conduct method of rapeseed cake the most according to claim 1, it is characterised in that: in described crude enzyme liquid preparation process, the concentration of buffer solution of sodium phosphate is 5～15mM, and pH value is 6.5～7.5.
The integrated conduct method of rapeseed cake the most according to claim 1, it is characterised in that: in described step (2), the method for solid-liquid separation can be centrifugal, it is also possible to being to filter, centrifugal rotational speed is 5000～15000rmp；
In described step (3), baking temperature is 30～65 DEG C, and drying time is 2～6h.
The integrated conduct method of rapeseed cake the most according to claim 2, it is characterised in that: the concentration of the buffer solution of sodium phosphate used in enzymolysis process in described step (1) is 10～50mM, and pH value is 6.5～7.5.
The integrated conduct method of rapeseed cake the most according to claim 1, it is characterised in that: in described step (4), heat treatment mode can be steam heating, microwave heating, oil bath heating；
When using steam heating, vapor (steam) temperature is 140～160 DEG C, and heat time heating time is 5～20min；
When using microwave heating, microwave power is 400～800w, and the microwave time is 5～9min；
When using oil bath heating, oil bath temperature is 140～160 DEG C, and heat time heating time is 10～30min.
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| CN111234917A (en) * | 2020-03-05 | 2020-06-05 | 中国农业科学院油料作物研究所 | Preparation method of cold-pressed rapeseed oil rich in Canoll |
| DE102020002144A1 (en) | 2020-04-03 | 2021-10-07 | Christian Schein | Processing of rapeseed |
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| CN110615731A (en) * | 2019-09-16 | 2019-12-27 | 中国农业科学院油料作物研究所 | Method for preparing 2, 6-dimethoxy-4-vinylphenol |
| CN110615731B (en) * | 2019-09-16 | 2022-10-14 | 中国农业科学院油料作物研究所 | Method for preparing 2, 6-dimethoxy-4-vinylphenol |
| CN111234917A (en) * | 2020-03-05 | 2020-06-05 | 中国农业科学院油料作物研究所 | Preparation method of cold-pressed rapeseed oil rich in Canoll |
| DE102020002144A1 (en) | 2020-04-03 | 2021-10-07 | Christian Schein | Processing of rapeseed |
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