CN114249666B - Extraction method of betaine in phoenix tree leaves - Google Patents
Extraction method of betaine in phoenix tree leaves Download PDFInfo
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- CN114249666B CN114249666B CN202210038287.1A CN202210038287A CN114249666B CN 114249666 B CN114249666 B CN 114249666B CN 202210038287 A CN202210038287 A CN 202210038287A CN 114249666 B CN114249666 B CN 114249666B
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- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 title claims abstract description 103
- 241001412225 Firmiana simplex Species 0.000 title claims abstract description 68
- 229960003237 betaine Drugs 0.000 title claims abstract description 59
- 238000000605 extraction Methods 0.000 title claims abstract description 11
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 title claims abstract 16
- 238000001179 sorption measurement Methods 0.000 claims abstract description 24
- 239000011347 resin Substances 0.000 claims abstract description 21
- 229920005989 resin Polymers 0.000 claims abstract description 21
- 238000001728 nano-filtration Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 23
- 108010059892 Cellulase Proteins 0.000 claims description 12
- 229940106157 cellulase Drugs 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 10
- 239000003480 eluent Substances 0.000 claims description 10
- 239000012528 membrane Substances 0.000 claims description 8
- 238000002390 rotary evaporation Methods 0.000 claims description 8
- 239000012141 concentrate Substances 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000010828 elution Methods 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000003306 harvesting Methods 0.000 claims description 6
- 238000004108 freeze drying Methods 0.000 claims description 4
- 238000001694 spray drying Methods 0.000 claims description 4
- 239000003463 adsorbent Substances 0.000 claims description 3
- 238000003287 bathing Methods 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 230000007071 enzymatic hydrolysis Effects 0.000 claims description 2
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 6
- 230000006378 damage Effects 0.000 abstract description 2
- 238000007781 pre-processing Methods 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 8
- 230000001276 controlling effect Effects 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 238000004128 high performance liquid chromatography Methods 0.000 description 4
- 241001412224 Firmiana Species 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 229940023579 anhydrous betaine Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 description 1
- 206010007247 Carbuncle Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- 208000015817 Infant Nutrition disease Diseases 0.000 description 1
- 206010042674 Swelling Diseases 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000001412 amines Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229940076810 beta sitosterol Drugs 0.000 description 1
- LGJMUZUPVCAVPU-UHFFFAOYSA-N beta-Sitostanol Natural products C1CC2CC(O)CCC2(C)C2C1C1CCC(C(C)CCC(CC)C(C)C)C1(C)CC2 LGJMUZUPVCAVPU-UHFFFAOYSA-N 0.000 description 1
- UMRPOGLIBDXFNK-ZYGITSNFSA-N beta-amyrin acetate Chemical compound C([C@H]1C2=CC[C@H]34)C(C)(C)CC[C@]1(C)CC[C@@]2(C)[C@]4(C)CC[C@@H]1[C@]3(C)CC[C@H](OC(=O)C)C1(C)C UMRPOGLIBDXFNK-ZYGITSNFSA-N 0.000 description 1
- PDNLMONKODEGSE-UHFFFAOYSA-N beta-amyrin acetate Natural products CC(=O)OC1CCC2(C)C(CCC3(C)C4(C)CCC5(C)CCC(C)(C)CC5C4=CCC23C)C1(C)C PDNLMONKODEGSE-UHFFFAOYSA-N 0.000 description 1
- NJKOMDUNNDKEAI-UHFFFAOYSA-N beta-sitosterol Natural products CCC(CCC(C)C1CCC2(C)C3CC=C4CC(O)CCC4C3CCC12C)C(C)C NJKOMDUNNDKEAI-UHFFFAOYSA-N 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 description 1
- 229940106681 chloroacetic acid Drugs 0.000 description 1
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 description 1
- 229960001231 choline Drugs 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000005548 dental material Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 208000001848 dysentery Diseases 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 235000015203 fruit juice Nutrition 0.000 description 1
- 208000014617 hemorrhoid Diseases 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000020939 nutritional additive Nutrition 0.000 description 1
- -1 printing and dyeing Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 description 1
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 description 1
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 description 1
- 235000005493 rutin Nutrition 0.000 description 1
- 229960004555 rutoside Drugs 0.000 description 1
- KZJWDPNRJALLNS-VJSFXXLFSA-N sitosterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CC[C@@H](CC)C(C)C)[C@@]1(C)CC2 KZJWDPNRJALLNS-VJSFXXLFSA-N 0.000 description 1
- 229950005143 sitosterol Drugs 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000008736 traumatic injury Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Cosmetics (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for extracting betaine from phoenix tree leaves, and belongs to the technical field of betaine extraction. The method comprises the following steps: preprocessing; performing enzymolysis treatment; nanofiltration and concentration are carried out; purifying with macroporous adsorption resin; and (5) drying treatment. The extraction method of betaine in the phoenix tree leaves adopts the phoenix tree leaves as raw materials to extract the betaine, the raw materials are widely available in sources and low in extraction cost; the continuous treatment of enzymolysis, nanofiltration and NKA-9 macroporous adsorption resin for preparing betaine has short time consumption, mild condition, small product damage and high betaine extraction rate up to 13.7%.
Description
Technical Field
The invention belongs to the technical field of betaine extraction, and particularly relates to a method for extracting betaine from phoenix tree leaves.
Background
The Firmiana straminea leaf is the leaf of Firmiana straminea of Firmiana of Firmicaceae, and is distributed in most regions of the country. The phoenix tree leaf is used as a traditional Chinese medicine material and has the effects of dispelling wind and removing dampness, detoxifying and reducing swelling and reducing blood pressure. It is used for treating rheumatalgia, traumatic injury, carbuncle, sore, toxic swelling, hemorrhoid, infantile malnutrition, dysentery, and hypertension. The phoenix tree leaf contains betaine, choline, beta-amyrin acetate, beta-sitosterol, and 0.15% of rutin.
Betaine is also called trimethylglycine, and belongs to quaternary amine type alkaloids. The anhydrous betaine is a novel fine chemical and can be widely applied to the fields of food, medicine, daily chemicals, printing and dyeing, chemical industry and the like. Anhydrous betaine is a high-efficiency and high-quality nutritional additive; the pharmaceutical betaine can be used in medicine, cosmetics, food, fruit juice industry and dental materials; in addition, betaine can also be used in the fermentation industry; betaine can be extracted from the roots, stems, leaves and fruits of natural plants or chemically synthesized by adopting trimethylamine and chloroacetic acid as raw materials.
Although the phoenix tree leaves contain a large amount of betaine, no document for efficiently extracting betaine from the phoenix tree leaves is disclosed.
Disclosure of Invention
The invention aims to provide a method for extracting betaine from phoenix tree leaves, which takes phoenix tree leaves as a raw material, and comprises the steps of enzymolysis, nanofiltration concentration, macroporous adsorption resin purification treatment and drying to obtain high-purity betaine.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a method for extracting betaine from phoenix tree leaves comprises the following steps:
pretreatment of
Harvesting fresh phoenix tree leaves, cleaning, cutting into filaments, and freeze-drying to obtain a dried material;
enzymatic hydrolysis treatment of the ground
Adding the dried material into pure water with the mass of 5-10 times of that of the dried material, adjusting the pH value to 4.5-6.0, adding a cellulase solution at the temperature of 45-60 ℃, controlling the concentration of cellulase to be 5-10U/mL, carrying out enzymolysis for 3-5 h, then heating to 90-95 ℃ for treatment for 10-15min, cooling to 70-75 ℃, carrying out microwave treatment for 10-15min, and then heating to 80-85 ℃ for constant temperature treatment for 2-3 h to obtain an enzymolysis material;
nano-filtration concentration
Filtering the enzymolysis material by using 2-3 layers of gauze, collecting filtrate, and concentrating by using a nanofiltration membrane to obtain concentrated solution;
purifying with macroporous adsorbent resin
Adsorbing the concentrated solution by NKA-9 macroporous adsorption resin, eluting with deionized water, and eluting with 30% -80% ethanol to obtain eluate containing phoenix tree leaf betaine;
drying treatment for bathing
Performing vacuum rotary evaporation on the eluent containing the phoenix tree leaf betaine to obtain evaporation concentrate, and performing spray drying to obtain the phoenix tree leaf betaine.
Further, the freeze drying is to pre-cool the phoenix tree leaf filaments to-40 to-60 ℃, sublimate and dry for 8-20 hours until the temperature of the phoenix tree leaf filaments is 0-10 ℃, and analyze and dry for 10-20 hours until the temperature of the phoenix tree leaf filaments is 20-30 ℃.
Further, the microwave power adopted by the microwave treatment is 450-500W.
Further, the molecular weight cut-off of the nanofiltration membrane is 200-1000 Da.
Further, the NKA-9 macroporous adsorbent resin has an aspect ratio of 1: 8-12, the adsorption time is 3-5 h, and the elution volume of 30% -80% ethanol is 4-10 times of the volume of NKA-9 macroporous adsorption resin.
Further, the vacuum degree of the vacuum rotary evaporation is 0.02-0.05 MPa, and the temperature is 40-60 ℃; the air inlet temperature of spray drying is 180-210 ℃, and the discharging temperature is 80-90 ℃.
The beneficial technical effects of the invention are as follows: the extraction method of betaine in the phoenix tree leaves adopts the phoenix tree leaves as raw materials to extract the betaine, the raw materials are widely available in sources and low in extraction cost; the continuous treatment of enzymolysis, nanofiltration and NKA-9 macroporous adsorption resin for preparing betaine has short time consumption, mild condition, small product damage and high betaine extraction rate up to 13.7%.
Detailed Description
The present invention will be further described in detail with reference to the following examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
Harvesting fresh phoenix tree leaves, cleaning, cutting into filaments with the width of 2mm, pre-cooling 5.0kg of phoenix tree leaf filaments to-40 ℃, sublimating and drying for 10h until the temperature of the phoenix tree leaf filaments is 4 ℃, analyzing and drying for 12h until the temperature of the phoenix tree leaf filaments is 20 ℃, adding the obtained dried material into pure water with the mass of 5 times of the dried material, regulating the pH value to 4.6, adjusting the temperature to 45 ℃, adding a cellulase solution, controlling the concentration of the cellulase to be 6U/mL, carrying out enzymolysis for 4.5h, then heating to 90 ℃ for 15min, cooling to 70 ℃, carrying out microwave treatment for 15min by 450W, then heating to 80 ℃ for constant temperature for 3h, filtering the obtained enzymolysis material by using 2 layers of gauze, collecting filtrate, concentrating the obtained concentrate by using nanofiltration membrane with the interception molecular weight of 20Da, adsorbing by using NKA-9 macroporous adsorption resin, eluting by deionized water, eluting by using 30% ethanol to obtain eluent containing phoenix tree leaf betaine, and carrying out the diameter ratio of NKA-9 macroporous adsorption resin 1:8, the adsorption time is 4 hours, and the elution volume of 30% ethanol is 4 times of the volume of NKA-9 macroporous adsorption resin; performing vacuum rotary evaporation on the eluent containing the phoenix tree leaf betaine, wherein the vacuum degree is 0.02MPa, the temperature is 60 ℃, and the obtained evaporation concentrate is spray-dried, the air inlet temperature is 180 ℃, and the discharge temperature is 80 ℃, so as to obtain 1.027kg of phoenix tree leaf betaine powder.
The phoenix tree leaf betaine obtained in the embodiment is yellow in appearance, and the betaine content in the phoenix tree leaf betaine powder is 10.8% through high performance liquid chromatography detection.
Example 2
Harvesting fresh phoenix tree leaves, cleaning, cutting into filaments with the width of 2mm, pre-cooling 5kg of phoenix tree leaf filaments to-60 ℃, sublimating and drying for 18h until the temperature of the phoenix tree leaf filaments is 0 ℃, analyzing and drying for 15h until the temperature of the phoenix tree leaf filaments is 25 ℃, adding the obtained dried material into pure water with the mass of 8 times of the dried material, adjusting the pH value to 5.5, adjusting the temperature to 55 ℃, adding a cellulase solution, controlling the concentration of the cellulase to be 6U/mL, carrying out enzymolysis for 4h, then heating to 95 ℃ for 12min, cooling to 75 ℃, carrying out microwave treatment for 12min by 500W, then heating to 85 ℃ for constant temperature for 3h, filtering the obtained enzymolysis material by using 3 layers of gauze, collecting filtrate, concentrating the obtained concentrated solution by using nanofiltration membrane with the interception molecular weight of 500Da, eluting by deionized water firstly, eluting by using 50% ethanol, and obtaining eluent containing phoenix tree leaf betaine, wherein the diameter ratio of NKA-9 macroporous adsorption resin is 1:8, the adsorption time is 5h, and the volume of 50 ethanol elution is 8 times of the volume of NKA-9 macroporous adsorption resin; performing vacuum rotary evaporation on the eluent containing the phoenix tree leaf betaine, wherein the vacuum degree is 0.05MPa, the temperature is 50 ℃, and the obtained evaporation concentrate is spray-dried, the air inlet temperature is 200 ℃, the discharge temperature is 85 ℃, so as to obtain 1.112kg of phoenix tree leaf betaine powder.
The phoenix tree leaf betaine obtained in the embodiment is yellow in appearance, and the betaine content in the phoenix tree leaf betaine powder is 13.2% through high performance liquid chromatography detection.
Example 3
Harvesting fresh phoenix tree leaves, cleaning, cutting into filaments with the width of 2mm, pre-cooling 10kg of phoenix tree leaf filaments to-50 ℃, sublimating and drying for 15h to the temperature of the phoenix tree leaf filaments to 4 ℃, analyzing and drying for 20h to the temperature of the phoenix tree leaf filaments to 30 ℃, adding the obtained dried material into pure water with the mass of 7 times of the dried material, adjusting the pH to 4.8, the temperature to 50 ℃, adding a cellulase solution, controlling the concentration of the cellulase to 8U/mL, carrying out enzymolysis for 5h, then heating to 95 ℃ for 12min, cooling to 70 ℃, carrying out microwave treatment for 15min by 500W, then heating to 85 ℃ for constant temperature for 3h, filtering the obtained enzymolysis material by using 2 layers of gauze, collecting filtrate, concentrating the obtained concentrated solution by using nanofiltration membrane with the interception molecular weight of 200Da, eluting by deionized water firstly, eluting by using 80% ethanol to obtain eluent containing phoenix tree leaf betaine, and carrying out the diameter-to ratio of NKA-9 macroporous adsorption resin 1:8, the adsorption time is 5h, and the elution volume of 80% ethanol is 8 times of the volume of NKA-9 macroporous adsorption resin; performing vacuum rotary evaporation on the eluent containing the phoenix tree leaf betaine, wherein the vacuum degree is 0.05MPa, the temperature is 60 ℃, and the obtained evaporation concentrate is spray-dried, the air inlet temperature is 210 ℃, the discharge temperature is 90 ℃, so as to obtain 2.403kg of phoenix tree leaf sweet powder.
The phoenix tree leaf betaine obtained in the embodiment is light yellow in appearance, and the betaine content in the phoenix tree leaf betaine powder is 13.7% through high performance liquid chromatography detection.
Example 4
Harvesting fresh phoenix tree leaves, cleaning, cutting into filaments with the width of 3mm, pre-cooling 15kg of phoenix tree leaf filaments to-40 ℃, sublimating and drying for 8h to the temperature of the phoenix tree leaf filaments to 10 ℃, analyzing and drying for 20h to the temperature of the phoenix tree leaf filaments to 20 ℃, adding the obtained dried material into pure water with the mass of 5 times of the dried material, regulating the pH to 4.5, the temperature to 60 ℃, adding a cellulase solution, controlling the concentration of the cellulase to be 5U/mL, carrying out enzymolysis for 3h, then heating to 90 ℃ for 15min, cooling to 70 ℃, carrying out microwave treatment for 15min by 500W, then heating to 85 ℃ for constant temperature for 2h, filtering the obtained enzymolysis material by using 3 layers of gauze, collecting filtrate, concentrating the obtained concentrated solution by using nanofiltration membrane with the interception molecular weight of 1000Da, eluting by deionized water firstly, eluting by using 30% ethanol to obtain eluent containing phoenix tree leaf betaine, and carrying out the diameter-to ratio of NKA-9 macroporous adsorption resin 1:12, the adsorption time is 3h, and the elution volume of 50% ethanol is 10 times of the volume of NKA-9 macroporous adsorption resin; performing vacuum rotary evaporation on the eluent containing the phoenix tree leaf betaine, wherein the vacuum degree is 0.05MPa, the temperature is 40 ℃, and the obtained evaporation concentrate is spray-dried, the air inlet temperature is 195 ℃, the discharge temperature is 85 ℃, so as to obtain 3.326kg of phoenix tree leaf betaine powder.
The phoenix tree leaf betaine obtained in the embodiment has yellow brown appearance, and the betaine content in the phoenix tree leaf betaine powder is 12.1% through high performance liquid chromatography detection.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (6)
1. The extraction method of betaine in phoenix tree leaves is characterized by comprising the following steps:
pretreatment of
Harvesting fresh phoenix tree leaves, cleaning, cutting into filaments, and freeze-drying to obtain a dried material;
enzymatic hydrolysis treatment of the ground
Adding the dried material into pure water with the mass of 5-10 times of that of the dried material, adjusting the pH value to 4.5-6.0, adding a cellulase solution at the temperature of 45-60 ℃, controlling the concentration of cellulase to be 5-10U/mL, carrying out enzymolysis for 3-5 h, then heating to 90-95 ℃ for treatment for 10-15min, cooling to 70-75 ℃, carrying out microwave treatment for 10-15min, and then heating to 80-85 ℃ for constant temperature treatment for 2-3 h to obtain an enzymolysis material;
nano-filtration concentration
Filtering the enzymolysis material by using 2-3 layers of gauze, collecting filtrate, and concentrating by using a nanofiltration membrane to obtain concentrated solution;
purifying with macroporous adsorbent resin
Adsorbing the concentrated solution by NKA-9 macroporous adsorption resin, eluting with deionized water, and eluting with 30% -80% ethanol to obtain eluate containing phoenix tree leaf betaine;
drying treatment for bathing
Performing vacuum rotary evaporation on the eluent containing the phoenix tree leaf betaine to obtain evaporation concentrate, and performing spray drying to obtain the phoenix tree leaf betaine.
2. The method for extracting betaine from phoenix tree leaves according to claim 1, wherein: the freeze drying is to pre-cool the Chinese parasol leaf filaments to-40 to-60 ℃ and sublimate and dry for 8-20 hours until the temperature of the Chinese parasol leaf filaments is 0-10 ℃ and analyze and dry for 10-20 hours until the temperature of the Chinese parasol leaf filaments is 20-30 ℃.
3. The method for extracting betaine from phoenix tree leaves according to claim 1, wherein: the microwave power adopted by the microwave treatment is 450-500W.
4. The method for extracting betaine from phoenix tree leaves according to claim 1, wherein: the molecular weight cut-off of the nanofiltration membrane is 200-1000 Da.
5. The method for extracting betaine from phoenix tree leaves according to claim 1, wherein: the diameter-height ratio of the NKA-9 macroporous adsorption resin is 1: 8-12, the adsorption time is 3-5 h, and the elution volume of 30% -80% ethanol is 4-10 times of the volume of NKA-9 macroporous adsorption resin.
6. The method for extracting betaine from phoenix tree leaves according to claim 1, wherein: the vacuum degree of the vacuum rotary evaporation is 0.02-0.05 MPa, and the temperature is 40-60 ℃; the air inlet temperature of spray drying is 180-210 ℃, and the discharging temperature is 80-90 ℃.
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| JP2010207208A (en) * | 2009-02-10 | 2010-09-24 | Eisai Food Chemical Kk | Antibacterial agent containing mallotus japonicus extract |
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