CN114917617B - Cranberry grading extraction method - Google Patents
Cranberry grading extraction method Download PDFInfo
- Publication number
- CN114917617B CN114917617B CN202210610485.0A CN202210610485A CN114917617B CN 114917617 B CN114917617 B CN 114917617B CN 202210610485 A CN202210610485 A CN 202210610485A CN 114917617 B CN114917617 B CN 114917617B
- Authority
- CN
- China
- Prior art keywords
- cranberry
- extraction
- solution
- extract
- ultrafiltration membrane
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000000605 extraction Methods 0.000 title claims abstract description 82
- 235000012545 Vaccinium macrocarpon Nutrition 0.000 title claims abstract description 48
- 235000002118 Vaccinium oxycoccus Nutrition 0.000 title claims abstract description 48
- 235000004634 cranberry Nutrition 0.000 title claims abstract description 48
- 244000291414 Vaccinium oxycoccus Species 0.000 title description 2
- 240000001717 Vaccinium macrocarpon Species 0.000 claims abstract description 61
- 239000012528 membrane Substances 0.000 claims abstract description 51
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 45
- 235000020237 cranberry extract Nutrition 0.000 claims abstract description 28
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 235000021019 cranberries Nutrition 0.000 claims abstract description 15
- 239000000706 filtrate Substances 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000002390 rotary evaporation Methods 0.000 claims abstract description 7
- 238000006911 enzymatic reaction Methods 0.000 claims abstract description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 26
- 229920002125 Sokalan® Polymers 0.000 claims description 23
- 239000004584 polyacrylic acid Substances 0.000 claims description 23
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 21
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 21
- 229920001046 Nanocellulose Polymers 0.000 claims description 18
- 239000013078 crystal Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000004695 Polyether sulfone Substances 0.000 claims description 17
- 229920006393 polyether sulfone Polymers 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 238000002791 soaking Methods 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000000284 extract Substances 0.000 claims description 14
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 13
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- 239000002202 Polyethylene glycol Substances 0.000 claims description 12
- 229920001223 polyethylene glycol Polymers 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 12
- 238000005238 degreasing Methods 0.000 claims description 11
- 238000005374 membrane filtration Methods 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 230000004907 flux Effects 0.000 claims description 10
- 238000007710 freezing Methods 0.000 claims description 10
- 230000008014 freezing Effects 0.000 claims description 10
- 238000000926 separation method Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 8
- 238000005266 casting Methods 0.000 claims description 7
- 239000000287 crude extract Substances 0.000 claims description 7
- 239000003480 eluent Substances 0.000 claims description 7
- 238000004440 column chromatography Methods 0.000 claims description 6
- 238000004108 freeze drying Methods 0.000 claims description 6
- 239000003208 petroleum Substances 0.000 claims description 6
- 108010059892 Cellulase Proteins 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 5
- 229940106157 cellulase Drugs 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 5
- 238000007598 dipping method Methods 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000004898 kneading Methods 0.000 claims description 5
- 238000007790 scraping Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000009740 moulding (composite fabrication) Methods 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000005194 fractionation Methods 0.000 claims 1
- 239000004480 active ingredient Substances 0.000 abstract description 10
- 238000004090 dissolution Methods 0.000 abstract description 3
- 241000196324 Embryophyta Species 0.000 abstract description 2
- 238000007781 pre-processing Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 18
- 238000001514 detection method Methods 0.000 description 6
- 239000004410 anthocyanin Substances 0.000 description 4
- 229930002877 anthocyanin Natural products 0.000 description 4
- 235000010208 anthocyanin Nutrition 0.000 description 4
- 150000004636 anthocyanins Chemical class 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000010355 oscillation Effects 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 239000002352 surface water Substances 0.000 description 3
- PFTAWBLQPZVEMU-ZFWWWQNUSA-N (+)-epicatechin Natural products C1([C@@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-ZFWWWQNUSA-N 0.000 description 2
- PFTAWBLQPZVEMU-UKRRQHHQSA-N (-)-epicatechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-UKRRQHHQSA-N 0.000 description 2
- 108091003079 Bovine Serum Albumin Proteins 0.000 description 2
- 230000003064 anti-oxidating effect Effects 0.000 description 2
- 229940098773 bovine serum albumin Drugs 0.000 description 2
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 description 2
- 235000005487 catechin Nutrition 0.000 description 2
- 229950001002 cianidanol Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- LPTRNLNOHUVQMS-UHFFFAOYSA-N epicatechin Natural products Cc1cc(O)cc2OC(C(O)Cc12)c1ccc(O)c(O)c1 LPTRNLNOHUVQMS-UHFFFAOYSA-N 0.000 description 2
- 235000012734 epicatechin Nutrition 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- PFTAWBLQPZVEMU-DZGCQCFKSA-N (+)-catechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-DZGCQCFKSA-N 0.000 description 1
- 241000612182 Rexea solandri Species 0.000 description 1
- 241000208422 Rhododendron Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 125000004403 catechin group Chemical group 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 235000013325 dietary fiber Nutrition 0.000 description 1
- 208000010643 digestive system disease Diseases 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 208000019206 urinary tract infection Diseases 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0011—Casting solutions therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
-
- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Water Supply & Treatment (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a cranberry grading extraction method, and relates to the technical field of plant extraction. The invention relates to a cranberry grading extraction method, which specifically comprises the following steps of taking fresh cranberries, and preprocessing to obtain cranberry juice, pericarp and pulp; adding the pulp into the extraction solution, separating to obtain a filtrate, mixing the filtrate with cranberry juice, and filtering and separating by an ultrafiltration membrane to obtain a primary extraction solution; and (3) after the pericarp is subjected to enzymatic reaction, adding an extraction solution, performing ultrahigh pressure extraction, filtering to obtain a secondary extraction solution, combining the primary extraction solution and the secondary extraction solution, performing rotary evaporation to dryness to obtain a crude cranberry extract, and purifying the crude cranberry extract to obtain the cranberry extract. The invention discloses a cranberry grading extraction method, which aims at the characteristic of different properties of different positions of cranberries, and can effectively improve the dissolution rate of active ingredients in each position of the cranberries, thereby improving the content of the active ingredients in the cranberry extract obtained finally.
Description
Technical Field
The invention relates to the technical field of plant extraction, in particular to a cranberry grading extraction method.
Background
The cranberry is also called cranberry, is evergreen small shrub of the cranberry genus of the azalea family, the cranberry extract contains rich dietary fibers, vitamins, minerals, inorganic salts and the like, the rich procyanidine can avoid the damage of cells and maintain the health and the vitality of the cells due to the special antioxidation capability, the procyanidine is natural polyphenol existing in nature, and the main structure of the procyanidine is catechin, epicatechin or a polymer between the catechin and the epicatechin, has the effects of antioxidation and deferring human aging, can treat digestive system diseases and urinary tract infection, and has an auxiliary effect on the treatment of diabetes.
The existing cranberry extract is prepared by directly crushing whole cranberries and then integrally extracting, but because the cranberry extract has different material compositions of all parts, the fibrous content of the pericarps is high, the sugar content of pulp and juice is high, the existing integral extraction mode can lead to incomplete extraction of procyanidine in the pericarps, and a large amount of other material components are extracted from the pulp and the juice, so that the active ingredients in the cranberry extract are not high finally.
Disclosure of Invention
Aiming at the problems, the invention aims to disclose a cranberry grading extraction method, which aims at the characteristic that the cranberries have different properties at different positions, and can effectively improve the dissolution rate of active ingredients in each part of the cranberry, thereby improving the content of the active ingredients in the cranberry extract obtained finally.
Specifically, the cranberry grading extraction method provided by the invention specifically comprises the following steps:
The method specifically comprises the following steps:
pretreatment: taking fresh cranberries, removing seeds, and performing juice extraction treatment to obtain cranberry juice and residues;
Dipping and freezing: soaking the residue in water for 1-2h, fishing out and drying the surface moisture, freezing at-20 to-15 ℃ for 12-14h, taking out, standing at room temperature for 30-45min, and then kneading and separating to obtain peel and pulp;
Primary extraction: adding water into the pulp obtained by preparation, ball milling for 1-2h, taking out, adding the extraction solution, stirring and mixing for 30-45min, performing membrane filtration and separation to obtain filtrate, mixing the filtrate with cranberry juice, adding the extraction solution, stirring and mixing, and performing ultrafiltration membrane filtration and separation to obtain primary extraction solution;
and (3) secondary extraction: drying the separated pericarps, cutting, inoculating cellulase, performing enzymatic reaction, adding extraction solution after the reaction is completed, performing ultrahigh pressure extraction, and filtering to obtain secondary extract;
Degreasing: mixing the primary extract and the secondary extract, adding petroleum ether for degreasing treatment, and then carrying out rotary evaporation to dryness to obtain a cranberry crude extract;
Purifying: separating and purifying the crude cranberry extract by column chromatography to obtain eluent, concentrating, and freeze-drying to obtain cranberry extract.
Further, the extraction solution is prepared from an ethanol solution with the mass fraction of 70% and a citric acid solution with the mass fraction of 1%, and the volume ratio of the ethanol solution to the citric acid solution is (10-8): 1.
Further, the pressure of the ultrahigh pressure extraction is 400MPa, the pressure rising speed is 10MPa/min, the pressure maintaining time is 20min, and the temperature is 25 ℃.
Further, the pressure is 0.4-0.6MPa, the temperature is 25-35 ℃ and the membrane flux is 400-450L/h when the ultrafiltration membrane is used for filtering for one-time extraction.
Further, the ultrafiltration membrane for one-time extraction is prepared by a wet method with polyethersulfone, polyacrylic acid, nanocellulose crystal, nano calcium carbonate and polyethylene glycol as raw materials and N, N-dimethylformamide as a solvent.
According to the ultrafiltration membrane, the polyether sulfone is used as a main substrate, the polyacrylic acid and the nanocellulose crystal are used as additives, on one hand, the polyacrylic acid and the nanocellulose crystal have good hydrophilicity, the hydrophilicity of the substrate can be improved to a certain extent by adding the polyacrylic acid and the nanocellulose crystal into the substrate, so that the anti-pollution performance of the ultrafiltration membrane is improved, and meanwhile, under the synergistic effect of the polyacrylic acid and the nanocellulose crystal, the acid resistance of a base material can be improved to a certain extent, so that the subsequent preparation process is facilitated, and meanwhile, the tolerance to an extraction solution can be improved in the use process, and the service life is prolonged; the added nano calcium carbonate and polyethylene glycol are used as pore-forming agents, and the nano calcium carbonate is dissolved out through acid treatment in the preparation process of the ultrafiltration membrane, so that the pore diameter of the ultrafiltration membrane obtained by preparation can be effectively improved, the membrane flux is improved, and the treatment capacity of the ultrafiltration membrane is improved.
Further, the ultrafiltration membrane comprises, by weight, 80-85 parts of polyethersulfone serving as a raw material, 4-6 parts of polyacrylic acid, 3-5 parts of nanocellulose crystal, 0.5-1 part of nano calcium carbonate and 1-3 parts of polyethylene glycol.
Further, the ultrafiltration membrane comprises the following raw materials of 82 parts by weight of polyethersulfone, 5 parts by weight of polyacrylic acid, 4 parts by weight of nano cellulose crystal, 0.8 part by weight of nano calcium carbonate and 2 parts by weight of polyethylene glycol.
Further, the preparation method of the ultrafiltration membrane comprises the following steps: adding polyacrylic acid into N, N-dimethylformamide, stirring until the polyacrylic acid is completely dissolved, adding nano cellulose crystal, nano calcium carbonate and polyethylene glycol, performing ultrasonic vibration dispersion, adding polyethersulfone, heating to 60-70 ℃, continuously stirring for 2-3 hours to obtain a casting solution, standing for defoaming for 6 hours, scraping a film, cooling and forming, soaking in a hydrochloric acid solution with the pH value of 2-3 for 30-45 minutes, taking out, washing, soaking in distilled water for 2-3d, and drying to obtain the modified polyethersulfone ultrafiltration membrane.
Further, the temperature of the casting film liquid for standing and defoaming is 25-28 ℃ and the humidity is 20-30%.
The invention has the beneficial effects that:
1. The invention discloses a cranberry grading extraction method, which aims at the characteristic that cranberries are different in properties at different positions, and respectively treats pericarps, pulps and juices, and extracts the pericarps, the pulps and the juices, so that the dissolution rate of active ingredients in each position of the cranberry can be effectively improved, the utilization rate of the cranberry is improved, and the content of the active ingredients in the cranberry extract obtained finally is further improved.
2. The cranberry grading extraction method improves the ultrafiltration membrane used, has higher hydrophilicity and pollution resistance, can reduce the influence of impurities such as protein in cranberry juice and pulp extracts on the ultrafiltration membrane, and prolongs the service life of the ultrafiltration membrane.
Detailed Description
The present invention will be described in detail with reference to the following specific examples:
According to the cranberry classifying and extracting method, each part of the cranberry is separated, and then the cranberries are respectively processed and classified and extracted according to the characteristics of each part, so that the extraction rate of active ingredients in the cranberry can be effectively improved, the content of the active ingredients in the cranberry extract obtained finally is further improved, and the biological activity of the cranberry extract is improved, and the method comprises the following steps of:
Example 1
Preparation of ultrafiltration membranes
Adding 5 parts of polyacrylic acid into 100 parts of N, N-dimethylformamide, stirring until the polyacrylic acid is completely dissolved, adding 4 parts of nano cellulose crystal, 0.8 part of nano calcium carbonate and 2 parts of polyethylene glycol, dispersing by ultrasonic oscillation, adding 82 parts of polyethersulfone, heating to 70 ℃, continuously stirring for 2 hours to obtain a casting solution, standing and defoaming for 6 hours at the temperature of 28 ℃ and the humidity of 25%, scraping the film, cooling and forming, then soaking in hydrochloric acid solution with the pH of 2-3 for 45 minutes, fishing out, washing, soaking in distilled water for 2 days, and drying to obtain the modified polyethersulfone ultrafiltration membrane.
The cranberry is extracted in a grading way by utilizing the prepared ultrafiltration membrane, and the method specifically comprises the following steps:
pretreatment: taking 1kg of fresh cranberry, removing seeds, and performing juice extraction treatment to obtain cranberry juice and residues;
dipping and freezing: soaking the residue in water for 1 hr, taking out, drying surface water, freezing at-15deg.C for 12 hr, taking out, standing at room temperature for 45min, and kneading to separate to obtain pericarp and pulp;
Primary extraction: preparing an ethanol solution with the mass fraction of 70% and a citric acid solution with the mass fraction of 1% according to the volume ratio of 10:1 to obtain an extraction solution,
Adding 1L of water into the pulp obtained by preparation, ball milling for 2 hours, taking out and adding 2L of extraction solution, stirring and mixing for 45 minutes, performing membrane filtration and separation to obtain filtrate, mixing the filtrate and cranberry juice, adding 1L of extraction solution, stirring and mixing, and performing ultrafiltration membrane filtration and separation under the conditions that the pressure is 0.5MPa, the temperature is 35 ℃ and the membrane flux is 420L/h to obtain primary extraction solution;
And (3) secondary extraction: drying the separated pericarps, cutting, inoculating and adding 0.01kg of cellulase, preserving heat at 55 ℃ for enzymatic reaction, adding 1L of extraction solution after the reaction is completed, performing ultrahigh pressure extraction under the conditions of 400MPa of pressure, 10MPa/min of pressure rise speed, 20min of pressure maintaining time and 25 ℃ of temperature, and filtering to obtain secondary extraction solution;
degreasing: mixing the primary extract and the secondary extract, adding 2L petroleum ether for degreasing treatment, and then carrying out rotary evaporation to dryness to obtain a cranberry crude extract;
Purifying: separating and purifying crude cranberry extract by using the existing column chromatography to obtain eluent, concentrating, and freeze-drying to obtain cranberry extract.
Through detection, the anthocyanin yield in the cranberry extract is 1.29%.
Example two
Preparation of ultrafiltration membranes
Adding 6 parts of polyacrylic acid into 100 parts of N, N-dimethylformamide, stirring until the polyacrylic acid is completely dissolved, adding 3 parts of nano cellulose crystal, 1 part of nano calcium carbonate and 1 part of polyethylene glycol, dispersing by ultrasonic oscillation, adding 80 parts of polyethersulfone, heating to 65 ℃, continuously stirring for 3 hours to obtain a casting solution, standing and defoaming for 6 hours at the temperature of 25 ℃ and the humidity of 20%, scraping the film, cooling and forming, soaking in a hydrochloric acid solution with the pH of 2-3 for 30 minutes, fishing out, washing, soaking in distilled water for 3 days, and drying to obtain the modified polyethersulfone ultrafiltration membrane.
The cranberry is extracted in a grading way by utilizing the prepared ultrafiltration membrane, and the method specifically comprises the following steps:
pretreatment: taking 1.5kg of fresh cranberry, removing seeds, and performing juice extraction treatment to obtain cranberry juice and residues;
Dipping and freezing: soaking the residue in water for 1 hr, taking out, drying surface water, freezing at-20deg.C for 13 hr, taking out, standing at room temperature for 30min, and kneading to separate to obtain pericarp and pulp;
primary extraction: preparing an ethanol solution with the mass fraction of 70% and a citric acid solution with the mass fraction of 1% according to the volume ratio of 9:1 to obtain an extraction solution,
Adding 2L of water into the pulp obtained by preparation, ball milling for 1h, taking out, adding 4L of extraction solution, stirring and mixing for 40min, performing membrane filtration and separation to obtain filtrate, mixing the filtrate and cranberry juice, adding 1L of extraction solution, stirring and mixing, and performing ultrafiltration membrane filtration and separation under the conditions that the pressure is 0.4MPa, the temperature is 30 ℃ and the membrane flux is 450L/h to obtain primary extraction solution;
And (3) secondary extraction: drying the separated pericarps, cutting, inoculating and adding 0.01kg of cellulase, preserving heat at 50 ℃ for enzymatic reaction, adding 2L of extraction solution after the reaction is completed, performing ultrahigh pressure extraction under the conditions of 400MPa of pressure, 10MPa/min of pressure rise speed, 20min of pressure maintaining time and 25 ℃ of temperature, and filtering to obtain secondary extraction solution;
degreasing: mixing the primary extract and the secondary extract, adding 2L petroleum ether for degreasing treatment, and then carrying out rotary evaporation to dryness to obtain a cranberry crude extract;
Purifying: separating and purifying crude cranberry extract by using the existing column chromatography to obtain eluent, concentrating, and freeze-drying to obtain cranberry extract.
Through detection, the anthocyanin yield in the cranberry extract is 1.19%.
Example III
Preparation of ultrafiltration membranes
Adding 4 parts of polyacrylic acid into 100 parts of N, N-dimethylformamide, stirring until the polyacrylic acid is completely dissolved, adding 5 parts of nano cellulose crystal, 0.5 part of nano calcium carbonate and 3 parts of polyethylene glycol, dispersing by ultrasonic oscillation, adding 85 parts of polyethersulfone, heating to 70 ℃, continuously stirring for 2 hours to obtain a casting solution, standing and defoaming for 6 hours at the temperature of 26 ℃ and the humidity of 30%, scraping the film, cooling and forming, then soaking in hydrochloric acid solution with the pH of 2-3 for 45 minutes, fishing out, washing, soaking in distilled water for 3 days, and drying to obtain the modified polyethersulfone ultrafiltration membrane.
The cranberry is extracted in a grading way by utilizing the prepared ultrafiltration membrane, and the method specifically comprises the following steps:
pretreatment: taking 2kg of fresh cranberries, removing seeds, and performing juice extraction treatment to obtain cranberry juice and residues;
dipping and freezing: soaking the residue in water for 2 hr, taking out, drying surface water, freezing at-15deg.C for 14 hr, taking out, standing at room temperature for 40min, and kneading to separate to obtain pericarp and pulp;
Primary extraction: preparing an ethanol solution with the mass fraction of 70% and a citric acid solution with the mass fraction of 1% according to the volume ratio of 8:1 to obtain an extraction solution,
Adding 3L of water into the prepared pulp, ball milling for 2 hours, taking out and adding 5L of extraction solution, stirring and mixing for 30 minutes, performing membrane filtration and separation to obtain filtrate, mixing the filtrate and cranberry juice, adding 2L of extraction solution, stirring and mixing, and performing ultrafiltration membrane filtration and separation under the conditions that the pressure is 0.6MPa, the temperature is 25 ℃ and the membrane flux is 400L/h to obtain primary extraction solution;
and (3) secondary extraction: drying the separated pericarps, cutting, inoculating and adding 0.02kg of cellulase, preserving heat at 55 ℃ for enzymatic reaction, adding 3L of extraction solution after the reaction is completed, performing ultrahigh pressure extraction under the conditions of 400MPa of pressure, 10MPa/min of pressure rise speed, 20min of pressure maintaining time and 25 ℃ of temperature, and filtering to obtain secondary extraction solution;
degreasing: mixing the primary extract and the secondary extract, adding 3L petroleum ether for degreasing treatment, and then carrying out rotary evaporation to dryness to obtain a cranberry crude extract;
Purifying: separating and purifying crude cranberry extract by using the existing column chromatography to obtain eluent, concentrating, and freeze-drying to obtain cranberry extract.
Through detection, the anthocyanin yield in the cranberry extract is 1.25%.
Comparative example one
The difference between this comparative example and example I is that polyacrylic acid was not added to the ultrafiltration membrane raw material of this comparative example.
Comparative example two
The difference between this comparative example and example I is that no nanocellulose crystal was added to the ultrafiltration membrane material of this comparative example.
Comparative example three
The difference between the present comparative example and the first example is that polyacrylic acid and nanocellulose crystals are not added to the ultrafiltration membrane raw material of the present comparative example.
Comparative example four
Compared with the first embodiment, the comparative example is different in that the cranberry of the comparative example is directly crushed when being extracted, then the same extraction solution of the comparative example is added for extraction, stirring and mixing are carried out for 2 hours, membrane filtration is carried out to obtain an extraction solution, petroleum ether is added into the extraction solution for degreasing treatment, then the cranberry crude extract is obtained by rotary evaporation, the cranberry crude extract is separated and purified by adopting the existing column chromatography, and the cranberry extract is obtained by freeze drying after eluent concentration. Through detection, the anthocyanin yield in the cranberry extract is 0.96%.
The ultrafiltration membranes prepared in the first to third examples, the comparative examples and the third examples are tested for hydrophilicity and pollution resistance,
Hydrophilicity was measured using a HAKE JGW-360a contact angle tester for static contact angles of the films. After natural air drying, the ultrafiltration membrane is used as test liquid, 5 positions are randomly taken for measurement, and the average value is taken as the final contact angle.
The pollution resistance detection adopts a bovine serum albumin solution with the concentration of 150mg/L as a feed, the pure water flux of the membrane is measured under the conditions of 0.1MPa and room temperature, the prepared bovine serum albumin solution is poured into the membrane to perform continuous ultrafiltration experiments for 1h, the polluted membrane is backwashed for 10min by deionized water, the pure water flux of the backwashed membrane is measured, the loss of the membrane flux is calculated, and the detection result is shown in the table 1:
TABLE 1 Ultrafiltration Membrane Performance test results
| Detecting items | Example 1 | Example two | Example III | Comparative example one | Comparative example two | Comparative example three |
| Contact angle | 65.9° | 67.4° | 66.3° | 79.1° | 75.5° | 86.4° |
| Amount of membrane flux loss | 18％ | 15％ | 19％ | 36％ | 32％ | 52％ |
As can be seen from the data in the table, the ultrafiltration membrane can effectively improve the hydrophilicity and pollution resistance of the ultrafiltration membrane by adding polyacrylic acid and nanocellulose crystals, so that the service life of the ultrafiltration membrane is prolonged, and meanwhile, as can be seen from the first embodiment and the fourth comparative embodiment, the content of active ingredients in the cranberry extract obtained finally can be improved by classifying the cranberries and respectively treating different parts.
The above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered by the scope of the claims of the present invention. The technology, shape, and construction parts of the present invention, which are not described in detail, are known in the art.
Claims (7)
1. The cranberry grading extraction method is characterized by comprising the following steps of:
pretreatment: taking fresh cranberries, removing seeds, and performing juice extraction treatment to obtain cranberry juice and residues;
Dipping and freezing: soaking the residue in water for 1-2h, fishing out and drying the surface moisture, freezing at-20 to-15 ℃ for 12-14h, taking out, standing at room temperature for 30-45min, and then kneading and separating to obtain peel and pulp;
Primary extraction: adding water into the pulp obtained by preparation, ball milling for 1-2h, taking out, adding the extraction solution, stirring and mixing for 30-45min, performing membrane filtration and separation to obtain filtrate, mixing the filtrate with cranberry juice, adding the extraction solution, stirring and mixing, and performing ultrafiltration membrane filtration and separation to obtain primary extraction solution;
and (3) secondary extraction: drying the separated pericarps, cutting, inoculating cellulase, performing enzymatic reaction, adding extraction solution after the reaction is completed, performing ultrahigh pressure extraction, and filtering to obtain secondary extract;
Degreasing: mixing the primary extract and the secondary extract, adding petroleum ether for degreasing treatment, and then carrying out rotary evaporation to dryness to obtain a cranberry crude extract;
Purifying: separating and purifying the crude cranberry extract by adopting a column chromatography method to obtain an eluent, concentrating the eluent, and freeze-drying to obtain the cranberry extract;
The ultrafiltration membrane for one-time extraction is prepared by a wet method by taking polyethersulfone, polyacrylic acid, nano cellulose crystal, nano calcium carbonate and polyethylene glycol as raw materials and taking N, N-dimethylformamide as a solvent;
The preparation method of the ultrafiltration membrane comprises the following steps: adding polyacrylic acid into N, N-dimethylformamide, stirring until the polyacrylic acid is completely dissolved, adding nano cellulose crystal, nano calcium carbonate and polyethylene glycol, performing ultrasonic vibration dispersion, adding polyethersulfone, heating to 60-70 ℃, continuously stirring for 2-3 hours to obtain a casting solution, standing for defoaming for 6 hours, scraping a film, cooling and forming, soaking in a hydrochloric acid solution with the pH value of 2-3 for 30-45 minutes, taking out, washing, soaking in distilled water for 2-3d, and drying to obtain the modified polyethersulfone ultrafiltration membrane.
2. The method for classifying and extracting cranberries according to claim 1, wherein the extracting solution is prepared from an ethanol solution with a mass fraction of 70% and a citric acid solution with a mass fraction of 1%, and the volume ratio of the ethanol solution to the citric acid solution is (10-8): 1.
3. The method for classifying and extracting cranberries according to claim 1, wherein the pressure of the ultra-high pressure extraction is 400MPa, the pressure increasing speed is 10MPa/min, the dwell time is 20min, and the temperature is 25 ℃.
4. A method for classifying and extracting cranberries according to claim 3, wherein the pressure is 0.4-0.6MPa, the temperature is 25-35 ℃ and the membrane flux is 400-450L/h when the ultrafiltration membrane is used for one-time extraction.
5. The cranberry fractional extraction method according to claim 1, wherein the ultrafiltration membrane comprises, by weight, 80-85 parts of polyether sulfone serving as a raw material, 4-6 parts of polyacrylic acid, 3-5 parts of nanocellulose crystal, 0.5-1 part of nano calcium carbonate and 1-3 parts of polyethylene glycol.
6. The cranberry fractionation method according to claim 5, wherein the ultrafiltration membrane comprises the following raw materials of polyethersulfone 82 parts, polyacrylic acid 5 parts, nanocellulose crystal 4 parts, nano calcium carbonate 0.8 part, and polyethylene glycol 2 parts by weight.
7. The method for classifying and extracting cranberries according to claim 1, wherein the temperature of the casting solution for standing and defoaming is 25-28 ℃ and the humidity is 20-30%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210610485.0A CN114917617B (en) | 2022-05-31 | 2022-05-31 | Cranberry grading extraction method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210610485.0A CN114917617B (en) | 2022-05-31 | 2022-05-31 | Cranberry grading extraction method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114917617A CN114917617A (en) | 2022-08-19 |
| CN114917617B true CN114917617B (en) | 2024-06-11 |
Family
ID=82812827
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210610485.0A Active CN114917617B (en) | 2022-05-31 | 2022-05-31 | Cranberry grading extraction method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114917617B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115553440B (en) * | 2022-09-15 | 2024-07-05 | 福州康嘉欣辰生物科技有限公司 | Cranberry powder and preparation method thereof |
| CN116370517B (en) * | 2023-02-28 | 2024-04-16 | 苏州农业职业技术学院 | Extraction method for extracting flavonoid substances from cranberries |
Citations (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1297699A (en) * | 2000-12-01 | 2001-06-06 | 傅敏恭 | Comprehensive utilization process of extracting effective components from tomato |
| CN1485324A (en) * | 2002-09-28 | 2004-03-31 | 河北神兴沙棘研究院 | Method of membrane separation technique for producing seabuckthorn flavone |
| CN101239962A (en) * | 2007-02-07 | 2008-08-13 | 上海华珠生物科技有限公司 | Method for extracting proanthocyanidins from cranberry |
| CN102218273A (en) * | 2010-04-16 | 2011-10-19 | 中国科学院大连化学物理研究所 | Preparation method for hydrophilic ultrafiltration membrane |
| CN102626595A (en) * | 2012-04-13 | 2012-08-08 | 清华大学 | Formula for industrial high-strength anti-pollution ultrafiltration flat plate membrane and preparation method thereof |
| CN102942549A (en) * | 2012-11-27 | 2013-02-27 | 长沙哈根生物科技有限公司 | Method for extracting blueberry anthocyanin with good stability |
| CN103252176A (en) * | 2013-05-13 | 2013-08-21 | 浙江理工大学 | Method for preparing modified polyether sulfone hollow fiber membrane |
| CN103480278A (en) * | 2013-09-06 | 2014-01-01 | 烟台绿水赋膜材料有限公司 | Preparation method and application of anti-pollution hydrophilic separating membrane |
| CN103570664A (en) * | 2013-11-13 | 2014-02-12 | 长沙蓝威生物制品有限公司 | Method of extracting procyanidine from huckleberries |
| CN103704665A (en) * | 2014-01-01 | 2014-04-09 | 宜昌土老憨风味食品有限公司 | Brewing method for citrus soy sauce |
| CN104605284A (en) * | 2015-02-13 | 2015-05-13 | 宁波杰顺生物科技有限公司 | Preparation method for cranberry pomace polyphenol extract |
| CN106036648A (en) * | 2016-06-12 | 2016-10-26 | 宁夏薯味仙食品科技开发有限公司 | Method for preparing potato nutrition porridge and method for preparing potato nutrition powder |
| CN106380458A (en) * | 2016-08-30 | 2017-02-08 | 福建光泽圣祥源酒业有限公司 | Method for extracting anthocyanidin in blueberry |
| CN107880148A (en) * | 2017-12-29 | 2018-04-06 | 广东省肇庆市质量计量监督检测所 | A kind of extracting method of Pachyrhizua angulatus polysaccharide |
| CN108936109A (en) * | 2018-07-02 | 2018-12-07 | 界首市百乐泉纯净水厂 | A kind of passion fruit modulation soda water |
| CN109645198A (en) * | 2018-12-06 | 2019-04-19 | 广东省农业科学院蚕业与农产品加工研究所 | A kind of preparation method of the passion fruit preserved fruit rich in anthocyanidin |
| CN110981682A (en) * | 2019-12-19 | 2020-04-10 | 董秀华 | Lycopene extraction element |
| CN111377898A (en) * | 2018-12-29 | 2020-07-07 | 宁波杰顺生物科技有限公司 | Preparation process of cranberry extract procyanidine |
| CN112314945A (en) * | 2020-10-29 | 2021-02-05 | 安徽卡伦拜瑞健康科技有限公司 | Method for preparing high-activity cranberry extract by sectional extraction method |
-
2022
- 2022-05-31 CN CN202210610485.0A patent/CN114917617B/en active Active
Patent Citations (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1297699A (en) * | 2000-12-01 | 2001-06-06 | 傅敏恭 | Comprehensive utilization process of extracting effective components from tomato |
| CN1485324A (en) * | 2002-09-28 | 2004-03-31 | 河北神兴沙棘研究院 | Method of membrane separation technique for producing seabuckthorn flavone |
| CN101239962A (en) * | 2007-02-07 | 2008-08-13 | 上海华珠生物科技有限公司 | Method for extracting proanthocyanidins from cranberry |
| CN102218273A (en) * | 2010-04-16 | 2011-10-19 | 中国科学院大连化学物理研究所 | Preparation method for hydrophilic ultrafiltration membrane |
| CN102626595A (en) * | 2012-04-13 | 2012-08-08 | 清华大学 | Formula for industrial high-strength anti-pollution ultrafiltration flat plate membrane and preparation method thereof |
| CN102942549A (en) * | 2012-11-27 | 2013-02-27 | 长沙哈根生物科技有限公司 | Method for extracting blueberry anthocyanin with good stability |
| CN103252176A (en) * | 2013-05-13 | 2013-08-21 | 浙江理工大学 | Method for preparing modified polyether sulfone hollow fiber membrane |
| CN103480278A (en) * | 2013-09-06 | 2014-01-01 | 烟台绿水赋膜材料有限公司 | Preparation method and application of anti-pollution hydrophilic separating membrane |
| CN103570664A (en) * | 2013-11-13 | 2014-02-12 | 长沙蓝威生物制品有限公司 | Method of extracting procyanidine from huckleberries |
| CN103704665A (en) * | 2014-01-01 | 2014-04-09 | 宜昌土老憨风味食品有限公司 | Brewing method for citrus soy sauce |
| CN104605284A (en) * | 2015-02-13 | 2015-05-13 | 宁波杰顺生物科技有限公司 | Preparation method for cranberry pomace polyphenol extract |
| CN106036648A (en) * | 2016-06-12 | 2016-10-26 | 宁夏薯味仙食品科技开发有限公司 | Method for preparing potato nutrition porridge and method for preparing potato nutrition powder |
| CN106380458A (en) * | 2016-08-30 | 2017-02-08 | 福建光泽圣祥源酒业有限公司 | Method for extracting anthocyanidin in blueberry |
| CN107880148A (en) * | 2017-12-29 | 2018-04-06 | 广东省肇庆市质量计量监督检测所 | A kind of extracting method of Pachyrhizua angulatus polysaccharide |
| CN108936109A (en) * | 2018-07-02 | 2018-12-07 | 界首市百乐泉纯净水厂 | A kind of passion fruit modulation soda water |
| CN109645198A (en) * | 2018-12-06 | 2019-04-19 | 广东省农业科学院蚕业与农产品加工研究所 | A kind of preparation method of the passion fruit preserved fruit rich in anthocyanidin |
| CN111377898A (en) * | 2018-12-29 | 2020-07-07 | 宁波杰顺生物科技有限公司 | Preparation process of cranberry extract procyanidine |
| CN110981682A (en) * | 2019-12-19 | 2020-04-10 | 董秀华 | Lycopene extraction element |
| CN112314945A (en) * | 2020-10-29 | 2021-02-05 | 安徽卡伦拜瑞健康科技有限公司 | Method for preparing high-activity cranberry extract by sectional extraction method |
Non-Patent Citations (2)
| Title |
|---|
| 温庆志，罗明良.压裂酸化新技术与污染控制.东营：中国石油大学出版社,2009,第180-181页. * |
| 纳米纤维素晶体对超滤膜亲水性能的提升研究;白朗明;梁恒;贾瑞宝;瞿芳术;丁安;李圭白;;给水排水(第12期);第30-35页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114917617A (en) | 2022-08-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114917617B (en) | Cranberry grading extraction method | |
| CN103980347A (en) | Antihypertensive peptide of swim bladder of large yellow croaker and preparation method and use thereof | |
| CN111440218A (en) | Preparation method of plant polyphenol | |
| CN107446978A (en) | A kind of stem of noble dendrobium small-molecular peptides and preparation method thereof | |
| CN107582581A (en) | A kind of extracting method of moringa oleifera leaf extractive | |
| CN104250286B (en) | Navodon septentrionalis fish-skin antioxidant collagen peptide and preparation method and use thereof | |
| CN114196721B (en) | Sea buckthorn bioactive peptide and preparation method thereof | |
| CN110885730A (en) | Production method of Chinese wolfberry fruit wine | |
| CN110496179B (en) | Method for extracting antioxidant substances from betel nut fruits and application | |
| CN113151388B (en) | Sea cucumber peptide with antioxidant and DPP-IV (dipeptidyl peptidase IV) inhibiting functions and preparation method thereof | |
| CN109385414B (en) | Purification method of bromelain | |
| CN102784193A (en) | Method for preparing hedysarum polybotrys extract by adopting coupling technology | |
| CN107349239A (en) | A kind of extracting method of mango leaf polyphenol | |
| CN112210022B (en) | Preparation method of low-methoxyl hawthorn pectin | |
| CN111617636B (en) | Plant extraction and purification process | |
| CN110483634B (en) | Purification method of soybean trypsin inhibitor crude extract | |
| CN114107265B (en) | Process for extracting bromelain | |
| CN110964767A (en) | Method for extracting aster polysaccharide and aster polypeptide | |
| CN117327205B (en) | Method for extracting heparin from pig lungs | |
| CN111410704A (en) | Latex coagulant containing pineapple plant extract | |
| CN110787210A (en) | Method for preparing desmodium styracifolium total glycosides based on membrane separation technology | |
| CN114365853B (en) | Method for preparing antioxidant dietary fibers in citrus peel residues | |
| CN114150033B (en) | Preparation method of rice bran antioxidant peptide compound treated by peak alpha amylase | |
| CN117683075A (en) | Hu sheep small molecular peptide separation and purification method | |
| CN116370517B (en) | Extraction method for extracting flavonoid substances from cranberries |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |