CN105476025A - Method for extracting waxberry polyphenol from waxberry fruit residues - Google Patents
Method for extracting waxberry polyphenol from waxberry fruit residues Download PDFInfo
- Publication number
- CN105476025A CN105476025A CN201510826878.5A CN201510826878A CN105476025A CN 105476025 A CN105476025 A CN 105476025A CN 201510826878 A CN201510826878 A CN 201510826878A CN 105476025 A CN105476025 A CN 105476025A
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- CN
- China
- Prior art keywords
- filtrate
- myrica ruba
- ruba marc
- hot water
- filter
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- Pending
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- 235000009134 Myrica cerifera Nutrition 0.000 title claims abstract description 54
- 235000013824 polyphenols Nutrition 0.000 title claims abstract description 46
- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 38
- 244000269152 Myrica pensylvanica Species 0.000 title abstract description 44
- 235000007270 Gaultheria hispida Nutrition 0.000 title abstract description 13
- 235000012851 Myrica pensylvanica Nutrition 0.000 title abstract description 13
- 235000013399 edible fruits Nutrition 0.000 title abstract description 6
- 239000000706 filtrate Substances 0.000 claims abstract description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 108010059892 Cellulase Proteins 0.000 claims abstract description 14
- 229940106157 cellulase Drugs 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 13
- 108090000790 Enzymes Proteins 0.000 claims abstract description 8
- 102000004190 Enzymes Human genes 0.000 claims abstract description 8
- 229940088598 enzyme Drugs 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 241000219433 Myrica Species 0.000 claims description 47
- 241000709400 Ruba Species 0.000 claims description 47
- 239000011347 resin Substances 0.000 claims description 14
- 229920005989 resin Polymers 0.000 claims description 14
- 238000003809 water extraction Methods 0.000 claims description 8
- 238000000746 purification Methods 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 7
- 230000008719 thickening Effects 0.000 claims description 7
- 239000012141 concentrate Substances 0.000 claims description 5
- 239000000284 extract Substances 0.000 claims description 5
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000000120 microwave digestion Methods 0.000 claims description 2
- 244000061457 Solanum nigrum Species 0.000 claims 10
- 238000000605 extraction Methods 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000000638 solvent extraction Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract 4
- 230000007071 enzymatic hydrolysis Effects 0.000 abstract 2
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 abstract 2
- 239000002131 composite material Substances 0.000 abstract 1
- 230000000415 inactivating effect Effects 0.000 abstract 1
- 238000000874 microwave-assisted extraction Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- 244000132436 Myrica rubra Species 0.000 description 6
- 239000000843 powder Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 2
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 208000026935 allergic disease Diseases 0.000 description 1
- 230000007815 allergy Effects 0.000 description 1
- 235000010208 anthocyanin Nutrition 0.000 description 1
- 229930002877 anthocyanin Natural products 0.000 description 1
- 239000004410 anthocyanin Substances 0.000 description 1
- 150000004636 anthocyanins Chemical class 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- 238000013124 brewing process Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 235000013325 dietary fiber Nutrition 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- HVQAJTFOCKOKIN-UHFFFAOYSA-N flavonol Natural products O1C2=CC=CC=C2C(=O)C(O)=C1C1=CC=CC=C1 HVQAJTFOCKOKIN-UHFFFAOYSA-N 0.000 description 1
- 150000002216 flavonol derivatives Chemical class 0.000 description 1
- 235000011957 flavonols Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000021022 fresh fruits Nutrition 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000007965 phenolic acids Chemical class 0.000 description 1
- -1 polyphenol compound Chemical class 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000126 substance Substances 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
Abstract
The invention relates to a method for extracting waxberry polyphenol from waxberry fruit residues. The method comprises the following steps: 1, drying the waxberry fruit residues, crushing the dried residues, and sieving the crushed residues by a 60 mesh sieve; 2, adding an ethanol solution with the volume ratio of 50%, carrying out microwave extraction, and filtering the obtained solution to obtain a filtrate 1 and filter residues for later use; 3, adding hot water, cellulase and pectase to the filter residues obtained in step 2, carrying out enzymatic hydrolysis, carrying out enzyme inactivating treatment, and filtering the obtained solution to obtain a filtrate 2 and filter residues for later use; 4, adding hot water to the filter residues obtained in step 3, extracting, and filtering the obtained solution to obtain a filtrate 3; 5, mixing the filtrate 1, the filtrate 2 and the filtrate 3, centrifuging the obtained filtrate mixture, carrying out pumping filtration, and purifying the filtered mixture; and 6, concentrating the purified mixture, and drying the concentrated mixture. The method for extracting waxberry polyphenol from waxberry fruit residues allows waxberry polyphenols to be extracted from the waxberry fruit residues through comprehensive utilization of a composite enzymatic hydrolysis technology and a solvent extraction technology and assisted utilization of a microwave technology, so the extraction efficiency is high, and the comprehensive utilization rate of waxberry is improved.
Description
Technical field
The invention belongs to garden stuff processing technical field, relate to a kind of method extracting bayberry polyphenol from myrica ruba marc.
Background technology
Myrica ruba marc is that red bayberry is squeezed the juice processing byproduct, in a large number without in the pomace utilized containing abundant polyphenol compound (anthocyanin, flavonols and phenolic acid etc.) and dietary fiber.Existing large quantity research shows at present, and bayberry polyphenol has stronger antioxidation activity, and human body cell can be protected from radical damage, strengthens blood vessel elasticity, improves the circulatory system, and promote the smoothness of skin, inflammation-inhibiting and allergy, improve the pliability in joint.Therefore, bayberry polyphenol has a wide range of applications in food and medicine etc., and demand increases day by day, and this just needs more aldehydes matter to extract resource.
Red bayberry fresh fruit can be squeezed the juice and be carried out the manufacture that waxberry wine etc. brewages product, and be almost taken as offal treatment containing the myrica ruba marc enriching bayberry polyphenol, at present, extract the raw material mainly Waxberry fruit of bayberry polyphenol, this makes the comprehensive utilization value of red bayberry be weakened severely.
In the extraction process of bayberry polyphenol, main adopt Hot water extraction or ethanol immersion, these two kinds of methods have extraction time long, the shortcoming such as solvent-oil ratio is large, extraction efficiency is low, can not extract bayberry polyphenol efficiently from myrica ruba marc.
Summary of the invention
The object of the invention is to solve the problem that red bayberry utilization rate is low and bayberry polyphenol extraction efficiency is low, a kind of method extracting bayberry polyphenol from myrica ruba marc is provided.
A kind of method extracting bayberry polyphenol from myrica ruba marc of the present invention, is characterized in that comprising the following steps:
A. myrica ruba marc is dried, and pulverizes 60 mesh sieves;
B. add the ethanolic solution of 50% volume ratio, microwave digestion, filter and obtain filtrate 1., filter residue is for subsequent use;
C. in the filter residue of step b, add 40-45 DEG C of hot water and cellulase, pectase, enzymolysis 60-65min, 95 DEG C of process 10min carry out going out enzyme immediately, and filter and obtain filtrate 2., filter residue is for subsequent use;
D. in the filter residue of step c, add 45-50 DEG C of hot water extraction 50-60min, filter and obtain filtrate 3.;
E. merge 1. 2. 3. filtrate, after centrifugal, suction filtration, use DA-201 macroreticular resin to carry out purifying;
F. with Rotary Evaporators, the sample after macroporous resin purification being concentrated, until flow out without ethanol, with being placed on 24h in 50 DEG C of drying boxes, obtaining bayberry polyphenol.
A kind of method extracting bayberry polyphenol from myrica ruba marc of the present invention in preferred scheme, is characterized in that: the myrica ruba marc bake out temperature described in step a is 40-45 DEG C, dry to the moisture in myrica ruba marc be 10-15%.
A kind of method extracting bayberry polyphenol from myrica ruba marc of the present invention in preferred scheme, is characterized in that: the ethanolic solution addition described in step b is 25-30 times of myrica ruba marc after drying, and microwave power is 600-650W, and the microwave time is 10-15min.
A kind of method extracting bayberry polyphenol from myrica ruba marc of the present invention in preferred scheme, it is characterized in that: the hot water addition described in step c is 30-35 times of step b filter residue, the total addition level of cellulase and pectase is the 0.25-0.3% of hot water addition, and the adding proportion of cellulase and pectase is 1.5:1.
A kind of method extracting bayberry polyphenol from myrica ruba marc of the present invention in preferred scheme, is characterized in that: the hot water addition described in steps d is 15-20 times of step c filter residue.
A kind of method extracting bayberry polyphenol from myrica ruba marc of the present invention in preferred scheme, is characterized in that: the centrifugation rate described in step e is 3000-3500rpm.
A kind of method extracting bayberry polyphenol from myrica ruba marc of the present invention in preferred scheme, is characterized in that: the thickening temperature described in step f and pressure are respectively 50-55 DEG C, 0.07-0.08MPa.
A kind of method extracting bayberry polyphenol from myrica ruba marc of the present invention, is characterized in that comprising the following steps:
A. myrica ruba marc is dried to moisture under 40-45 DEG C of condition is 10-15%, pulverizes 60 mesh sieves;
B. add the ethanolic solution of myrica ruba marc 25-30 50% volume ratio doubly after drying, 600-650W microwave power lixiviate 10-15min, filter and obtain filtrate 1., filter residue is for subsequent use;
C. in the filter residue of step b, add 30-35 40-45 DEG C of hot water doubly, account for the cellulase of hot water addition 0.25-0.3%, pectase, the adding proportion of cellulase and pectase is preferably 1.5:1, enzymolysis 60-65min, 95 DEG C of process 10min carry out going out enzyme immediately, 2. filtration obtains filtrate, and filter residue is for subsequent use;
D. in the filter residue of step c, add 15-20 45-50 DEG C of hot water extraction 50-60min doubly, filter and obtain filtrate 3.;
E. merge 1. 2. 3. filtrate, 3000-3500rpm is centrifugal, uses DA-201 macroreticular resin to carry out purifying after suction filtration;
F. concentrate the sample after macroporous resin purification with Rotary Evaporators, thickening temperature and pressure are respectively 50-55 DEG C, 0.07-0.08MPa, until flow out without ethanol, with being placed on 24h in 50 DEG C of drying boxes, obtain bayberry polyphenol, its yield is 1.5-1.8%.
A kind of method extracting bayberry polyphenol from myrica ruba marc of the present invention take myrica ruba marc as raw material, utilize comprehensive utilization conbined enzymolysis and solvent extraction method, and being aided with the extraction that microwave technology carries out bayberry polyphenol, extraction efficiency is high, improves the comprehensive utilization ratio of red bayberry.
A kind of method extracting bayberry polyphenol from myrica ruba marc of the present invention has the following advantages and effect relative to prior art tool:
(1) the present invention extracts bayberry polyphenol with the accessory substance myrica ruba marc in waxberry wine brewing process for raw material, will brewage discarded object and again utilize, and improve the comprehensive utilization value of red bayberry;
(2) conbined enzymolysis and solvent extraction method use simultaneously, and are extracted by three times, farthest obtain bayberry polyphenol;
(3) the auxiliary microwave that uses extracts, and improves extraction efficiency.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but working of an invention mode is not limited thereto.
Embodiment 1: a kind of method extracting bayberry polyphenol from myrica ruba marc of the present invention, comprises the following steps:
A. myrica ruba marc is dried to moisture under 40 DEG C of conditions is 10%, pulverizes 60 mesh sieves, takes 1Kg myrica ruba marc powder;
B. adding 25L volume ratio is 50% ethanolic solution, 600W microwave power lixiviate 10min, and filter and obtain filtrate 1., filter residue is for subsequent use;
C. in the filter residue of step b, add 33L40 DEG C of hot water, 49.5g cellulase, 33g pectase, enzymolysis 60-65min, 95 DEG C of process 10min carry out going out enzyme immediately, and filter and obtain filtrate 2., filter residue is for subsequent use, and remaining 1.2Kg filter residue is for subsequent use;
D. in the filter residue of step c, add 18L45 DEG C of hot water extraction 50min, filter and obtain filtrate 3.;
E. merge 1. 2. 3. filtrate, 3000rpm is centrifugal, uses DA-201 macroreticular resin to carry out purifying after suction filtration;
F. concentrate the sample after macroporous resin purification with Rotary Evaporators, thickening temperature and pressure are respectively 50 DEG C, 0.07MPa, until flow out without ethanol, with being placed on 24h in 50 DEG C of drying boxes, obtain 15g bayberry polyphenol, its yield is 1.5%.
Embodiment 2: a kind of method extracting bayberry polyphenol from myrica ruba marc of the present invention, comprises the following steps:
A. myrica ruba marc is dried to moisture under 43 DEG C of conditions is 12%, pulverizes 60 mesh sieves, takes 3Kg myrica ruba marc powder;
B. adding 81L volume ratio is 50% ethanolic solution, 630W microwave power lixiviate 12min, and filter and obtain filtrate 1., remaining 3.3Kg filter residue is for subsequent use;
C. in the filter residue of step b, add 105L43 DEG C of hot water, 170.1g cellulase, 113.4g pectase, enzymolysis 63min, 95 DEG C of process 10min carry out going out enzyme immediately, and filter and obtain filtrate 2., remaining 3.6Kg filter residue is for subsequent use;
D. in the filter residue of step c, add 61L48 DEG C of hot water extraction 55min, filter and obtain filtrate 3.;
E. merge 1. 2. 3. filtrate, 3200rpm is centrifugal, uses DA-201 macroreticular resin to carry out purifying after suction filtration;
F. concentrate the sample after macroporous resin purification with Rotary Evaporators, thickening temperature and pressure are respectively 52 DEG C, 0.075MPa, until flow out without ethanol, with being placed on 24h in 50 DEG C of drying boxes, obtain 51g bayberry polyphenol, its yield is 1.7%.
Embodiment 3: a kind of method extracting bayberry polyphenol from myrica ruba marc of the present invention, comprises the following steps:
A. myrica ruba marc is dried to moisture under 45 DEG C of conditions is 15%, pulverizes 60 mesh sieves, takes 5Kg myrica ruba marc powder;
B. adding 150L volume ratio is 50% ethanolic solution, 650W microwave power lixiviate 15min, and filter and obtain filtrate 1., remaining 5.5Kg filter residue is for subsequent use;
C. in the filter residue of step b, add 192.5L45 DEG C of hot water, 346.5g cellulase, 231g pectase, enzymolysis 65min, 95 DEG C of process 10min carry out going out enzyme immediately, and filter and obtain filtrate 2., remaining 6Kg filter residue is for subsequent use;
D. in the filter residue of step c, add 120L50 DEG C of hot water extraction 60min, filter and obtain filtrate 3.;
E. merge 1. 2. 3. filtrate, 3500rpm is centrifugal, uses DA-201 macroreticular resin to carry out purifying after suction filtration;
F. concentrate the sample after macroporous resin purification with Rotary Evaporators, thickening temperature and pressure are respectively 55 DEG C, 0.08MPa, until flow out without ethanol, with being placed on 24h in 50 DEG C of drying boxes, obtain 90g bayberry polyphenol, its yield is 1.8%.
Claims (8)
1. from myrica ruba marc, extract a method for bayberry polyphenol, it is characterized in that comprising the following steps:
A. myrica ruba marc is dried, and pulverizes 60 mesh sieves;
B. add the ethanolic solution of 50% volume ratio, microwave digestion, filter and obtain filtrate 1., filter residue is for subsequent use;
C. in the filter residue of step b, add 40-45 DEG C of hot water and cellulase, pectase, enzymolysis 60-65min, 95 DEG C of process 10min carry out going out enzyme immediately, and filter and obtain filtrate 2., filter residue is for subsequent use;
D. in the filter residue of step c, add 45-50 DEG C of hot water extraction 50-60min, filter and obtain filtrate 3.;
E. merge 1. 2. 3. filtrate, after centrifugal, suction filtration, use DA-201 macroreticular resin to carry out purifying;
F. with Rotary Evaporators, the sample after macroporous resin purification being concentrated, until flow out without ethanol, with being placed on 24h in 50 DEG C of drying boxes, obtaining bayberry polyphenol.
2. a kind of method extracting bayberry polyphenol from myrica ruba marc according to claim 1, is characterized in that: the myrica ruba marc bake out temperature described in step a is 40-45 DEG C, dry to the moisture in myrica ruba marc be 10-15%.
3. a kind of method extracting bayberry polyphenol from myrica ruba marc according to claim 1, is characterized in that: the ethanolic solution addition described in step b is 25-30 times of myrica ruba marc after drying, and microwave power is 600-650W, and the microwave time is 10-15min.
4. a kind of method extracting bayberry polyphenol from myrica ruba marc according to claim 1, it is characterized in that: the hot water addition described in step c is 30-35 times of step b filter residue, the total addition level of cellulase and pectase is the 0.25-0.3% of hot water addition, and the adding proportion of cellulase and pectase is 1.5:1.
5. a kind of method extracting bayberry polyphenol from myrica ruba marc according to claim 1, is characterized in that: the hot water addition described in steps d is 15-20 times of step c filter residue.
6. a kind of method extracting bayberry polyphenol from myrica ruba marc according to claim 1, is characterized in that: the centrifugation rate described in step e is 3000-3500rpm.
7. a kind of method extracting bayberry polyphenol from myrica ruba marc according to claim 1, is characterized in that: the thickening temperature described in step f and pressure are respectively 50-55 DEG C, 0.07-0.08MPa.
8. a kind of method extracting bayberry polyphenol from myrica ruba marc according to claim 1, is characterized in that comprising the following steps:
A. myrica ruba marc is dried to moisture under 40-45 DEG C of condition is 10-15%, pulverizes 60 mesh sieves;
B. add the ethanolic solution of myrica ruba marc 25-30 50% volume ratio doubly after drying, 600-650W microwave power lixiviate 10-15min, filter and obtain filtrate 1., filter residue is for subsequent use;
C. in the filter residue of step b, add 30-35 40-45 DEG C of hot water doubly, account for the cellulase of hot water addition 0.25-0.3%, pectase, the adding proportion of cellulase and pectase is preferably 1.5:1, enzymolysis 60-65min, 95 DEG C of process 10min carry out going out enzyme immediately, 2. filtration obtains filtrate, and filter residue is for subsequent use;
D. in the filter residue of step c, add 15-20 45-50 DEG C of hot water extraction 50-60min doubly, filter and obtain filtrate 3.;
E. merge 1. 2. 3. filtrate, 3000-3500rpm is centrifugal, uses DA-201 macroreticular resin to carry out purifying after suction filtration;
F. concentrate the sample after macroporous resin purification with Rotary Evaporators, thickening temperature and pressure are respectively 50-55 DEG C, 0.07-0.08MPa, until flow out without ethanol, with being placed on 24h in 50 DEG C of drying boxes, obtain bayberry polyphenol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510826878.5A CN105476025A (en) | 2015-11-24 | 2015-11-24 | Method for extracting waxberry polyphenol from waxberry fruit residues |
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| CN201510826878.5A CN105476025A (en) | 2015-11-24 | 2015-11-24 | Method for extracting waxberry polyphenol from waxberry fruit residues |
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| CN105476025A true CN105476025A (en) | 2016-04-13 |
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| CN201510826878.5A Pending CN105476025A (en) | 2015-11-24 | 2015-11-24 | Method for extracting waxberry polyphenol from waxberry fruit residues |
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Application publication date: 20160413 |