CN114249666A - Method for extracting betaine from phoenix tree leaves - Google Patents

Method for extracting betaine from phoenix tree leaves Download PDF

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Publication number
CN114249666A
CN114249666A CN202210038287.1A CN202210038287A CN114249666A CN 114249666 A CN114249666 A CN 114249666A CN 202210038287 A CN202210038287 A CN 202210038287A CN 114249666 A CN114249666 A CN 114249666A
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betaine
phoenix tree
temperature
extracting
tree leaves
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CN202210038287.1A
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CN114249666B (en
Inventor
闫捷
庞红威
陈虎虎
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Longdong University
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Longdong University
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C227/00Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
    • C07C227/38Separation; Purification; Stabilisation; Use of additives
    • C07C227/40Separation; Purification

Abstract

The invention discloses a method for extracting betaine from phoenix tree leaves, belonging to the technical field of betaine extraction. The method comprises the following steps: preprocessing; carrying out enzymolysis treatment; performing nanofiltration and concentration on the ground; purifying with macroporous adsorption resin; and fifthly, drying. The method for extracting the betaine in the phoenix tree leaves adopts the phoenix tree leaves as the raw materials to extract the betaine, the raw materials are wide and easily available, and the extraction cost is low; the time consumption for preparing the betaine by enzymolysis, nanofiltration and continuous treatment of NKA-9 macroporous adsorption resin is short, the conditions are mild, the product damage is small, and the extraction rate of the betaine can reach 13.7%.

Description

Method for extracting betaine from phoenix tree leaves
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
Folium Firmianae is the leaf of Firmiana simplex belonging to the genus Firmiana of the family Firmiana, and is distributed in most parts of the country. The phoenix tree leaf is used as a traditional Chinese medicine and has the effects of dispelling wind and removing dampness, detoxifying and reducing swelling and reducing blood pressure. It is used to treat rheumatic arthralgia, traumatic injury, carbuncle, sore, toxic swelling, hemorrhoid, infantile malnutrition, dysentery, and hypertension. The folium Firmianae contains betaine, choline, beta-balsamic alcohol acetate, beta-sitosterol, trisnane and 0.15% of rutin.
Betaine, also known as trimethylglycine, belongs to quaternary amine 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. The anhydrous betaine is a high-efficiency and high-quality nutritional additive; the pharmaceutical grade 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 root, stem, leaf and fruit of natural plant or chemically synthesized from trimethylamine and chloroacetic acid.
The phoenix tree leaves contain a large amount of betaine, but at present, few documents which use the phoenix tree leaves as raw materials for efficiently extracting the betaine are disclosed.
Disclosure of Invention
The invention aims to provide a method for extracting betaine from phoenix tree leaves.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for extracting betaine from folium Firmianae comprises the following steps:
pretreatment
Collecting fresh folium Firmianae, cleaning, cutting into filaments, and freeze drying to obtain dried material;
the enzymolysis treatment is carried out
Adding the dried material into pure water with the mass being 5-10 times of that of the dried material, adjusting the pH value to 4.5-6.0 and the temperature to 45-60 ℃, adding a cellulase solution, controlling the concentration of cellulase to be 5-10U/mL, carrying out enzymolysis reaction for 3-5 h, heating to 90-95 ℃, treating for 10-15min, cooling to 70-75 ℃, carrying out microwave treatment for 10-15min, heating to 80-85 ℃, and carrying out constant-temperature treatment for 2-3 h to obtain an enzymolysis material;
concentrating by nanofiltration
Filtering the enzymolysis material by using 2-3 layers of gauze, collecting filtrate, and concentrating by using a nanofiltration membrane to obtain concentrated solution;
fourth step of macroporous adsorbent resin purification
Adsorbing the concentrated solution with NKA-9 macroporous adsorbent resin, eluting with deionized water, and eluting with 30-80% ethanol to obtain eluate containing betaine of folium Firmianae;
drying treatment
Vacuum rotary evaporating the eluate containing firmiana leaf betaine to obtain concentrated solution, and spray drying to obtain firmiana leaf betaine.
Further, the freeze drying is to pre-cool the phoenix tree leaf filament to-40 to-60 ℃, to sublimate and dry for 8-20h until the temperature of the phoenix tree leaf filament is 0-10 ℃, and to analyze and dry for 10-20h until the temperature of the phoenix tree leaf filament is 20-30 ℃.
Furthermore, the microwave power adopted by the microwave treatment is 450-500W.
Furthermore, the molecular weight cut-off of the nanofiltration membrane is 200-1000 Da.
Further, the NKA-9 macroporous adsorption resin has a diameter-height 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 method for extracting the betaine in the phoenix tree leaves adopts the phoenix tree leaves as the raw materials to extract the betaine, the raw materials are wide and easily available, and the extraction cost is low; the time consumption for preparing the betaine by enzymolysis, nanofiltration and continuous treatment of NKA-9 macroporous adsorption resin is short, the conditions are mild, the product damage is small, and the extraction rate of the betaine can reach 13.7%.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail by the following examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
Collecting fresh phoenix tree leaf, cleaning, cutting into 2mm wide filament, taking 5.0kg of phoenix tree leaf filament, pre-cooling to-40 ℃, sublimation drying for 10h until the temperature of the phoenix tree leaf filament is 4 ℃, desorption drying for 12h until the temperature of the phoenix tree leaf filament is 20 ℃, adding the obtained dried material into pure water with the mass of 5 times of that of the phoenix tree leaf filament, adjusting the pH value to 4.6, adding cellulase solution at 45 ℃, controlling the concentration of cellulase to be 6U/mL, carrying out enzymolysis reaction for 4.5h, then heating to 90 ℃ for treatment for 15min, then cooling to 70 ℃, treating for 15min by adopting 450W microwaves, then heating to 80 ℃ for constant temperature treatment for 3h, filtering the obtained enzymolysis material by adopting 2 layers of gauze, collecting filtrate, concentrating the filtrate by using a nanofiltration membrane with the molecular weight cutoff of 20Da, adsorbing the obtained concentrated solution by NKA-9 macroporous adsorption resin, eluting by using deionized water, then eluting by using 30% ethanol to obtain eluent containing the phoenix tree leaf betaine, the ratio of the diameter to the height of the NKA-9 macroporous adsorption resin is 1: 8, the adsorption time is 4h, and the elution volume of 30 percent ethanol is 4 times of the volume of NKA-9 macroporous adsorption resin; vacuum rotary evaporation is carried out on the eluent containing the phoenix tree leaf betaine, the vacuum degree is 0.02MPa, the temperature is 60 ℃, the obtained evaporation concentrated solution is spray-dried, the air inlet temperature is 180 ℃, and the material outlet temperature is 80 ℃, so that 1.027kg of phoenix tree leaf betaine powder is obtained.
The obtained firmiana leaf betaine powder is yellow in appearance, and the content of betaine in the firmiana leaf betaine powder is 10.8% through high performance liquid chromatography detection.
Example 2
Collecting fresh phoenix tree leaf, cleaning, cutting into 2mm wide filament, taking 5kg of phoenix tree leaf filament, pre-cooling to-60 ℃, sublimation drying for 18h until the temperature of the phoenix tree leaf filament is 0 ℃, desorption drying for 15h until the temperature of the phoenix tree leaf filament is 25 ℃, adding the obtained dried material into pure water with the mass of 8 times of that of the dried material, adjusting the pH value to 5.5, adding cellulase solution at the temperature of 55 ℃, controlling the concentration of the cellulase to be 6U/mL, carrying out enzymolysis reaction for 4h, then heating to 95 ℃, treating for 12min, cooling to 75 ℃, treating for 12min by using 500W microwaves, then heating to 85 ℃, carrying out constant temperature treatment for 3h, filtering the obtained enzymolysis material by using 3 layers of gauze, collecting filtrate, concentrating the filtrate by using a nanofiltration membrane with the molecular weight cutoff of 500Da, adsorbing the obtained concentrated solution by NKA-9 macroporous adsorption resin, eluting by using deionized water, eluting by using 50% ethanol to obtain an eluent containing the phoenix tree leaf betaine, the ratio of the diameter to the height of the NKA-9 macroporous adsorption resin is 1: 8, the adsorption time is 5h, and the 50-ethanol elution volume is 8 times of the volume of the NKA-9 macroporous adsorption resin; vacuum rotary evaporation is carried out on the eluent containing the phoenix tree leaf betaine, the vacuum degree is 0.05MPa, the temperature is 50 ℃, the obtained evaporation concentrated solution is spray-dried, the air inlet temperature is 200 ℃, and the discharging temperature is 85 ℃, so that 1.112kg of phoenix tree leaf betaine powder is obtained.
The obtained firmiana leaf betaine powder is yellow in appearance, and the content of betaine in the firmiana leaf betaine powder is 13.2% through high performance liquid chromatography detection.
Example 3
Collecting fresh phoenix tree leaf, cleaning, cutting into 2mm wide filament, taking 10kg of phoenix tree leaf filament, pre-cooling to-50 ℃, sublimation drying for 15h until the temperature of the phoenix tree leaf filament is 4 ℃, desorption drying for 20h until the temperature of the phoenix tree leaf filament is 30 ℃, adding the obtained dried material into pure water with the mass of 7 times of that of the dried material, adjusting the pH value to 4.8 and the temperature to 50 ℃, adding cellulase solution, controlling the concentration of cellulase to be 8U/mL, carrying out enzymolysis reaction for 5h, then heating to 95 ℃, treating for 12min, cooling to 70 ℃, treating for 15min by using 500W microwaves, then heating to 85 ℃, carrying out constant temperature treatment for 3h, filtering the obtained enzymolysis material by using 2 layers of gauze, collecting filtrate, concentrating the filtrate by using a nanofiltration membrane with the molecular weight cutoff of 200Da, adsorbing the obtained concentrated solution by NKA-9 macroporous adsorption resin, eluting by using deionized water, then eluting by using 80% ethanol to obtain the elution containing the phoenix tree leaf betaine, the ratio of the diameter to the height of the NKA-9 macroporous adsorption resin is 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; vacuum rotary evaporation is carried out on the eluent containing the phoenix tree leaf betaine, the vacuum degree is 0.05MPa, the temperature is 60 ℃, the obtained evaporation concentrated solution is spray-dried, the air inlet temperature is 210 ℃, and the discharging temperature is 90 ℃, so that 2.403kg of phoenix tree leaf sweet powder is obtained.
The obtained firmiana leaf betaine powder is light yellow in appearance, and the content of betaine in the firmiana leaf betaine powder is 13.7% through high performance liquid chromatography detection.
Example 4
Collecting fresh phoenix tree leaf, cleaning, cutting into filament with width of 3mm, taking 15kg of phoenix tree leaf filament, pre-cooling to-40 ℃, sublimation drying for 8h until the temperature of the phoenix tree leaf filament is 10 ℃, desorption drying for 20h until the temperature of the phoenix tree leaf filament is 20 ℃, adding the obtained dried material into pure water with the mass of 5 times of that of the dried material, adjusting the pH value to 4.5, adding cellulase solution at the temperature of 60 ℃, controlling the concentration of the cellulase to be 5U/mL, carrying out enzymolysis reaction for 3h, then heating to 90 ℃, treating for 15min, cooling to 70 ℃, treating for 15min by using 500W microwaves, then heating to 85 ℃, carrying out constant temperature treatment for 2h, filtering the obtained enzymolysis material by using 3 layers of gauze, collecting filtrate, concentrating the filtrate by using a nanofiltration membrane with molecular weight of 1000Da, adsorbing the obtained concentrated solution by NKA-9 macroporous adsorption resin, eluting by using deionized water, then eluting by using 30% ethanol to obtain eluent containing the phoenix tree leaf betaine, the ratio of the diameter to the height of the NKA-9 macroporous adsorption resin is 1: 12, the adsorption time is 3h, and the elution volume of 50 percent ethanol is 10 times of the volume of NKA-9 macroporous adsorption resin; vacuum rotary evaporation is carried out on the eluent containing the phoenix tree leaf betaine, the vacuum degree is 0.05MPa, the temperature is 40 ℃, the obtained evaporation concentrated solution is spray-dried, the air inlet temperature is 195 ℃, and the discharging temperature is 85 ℃, so that 3.326kg of phoenix tree leaf betaine powder is obtained.
The obtained firmiana leaf betaine powder in the embodiment is yellow brown in appearance, and the content of betaine in the firmiana leaf betaine powder is 12.1% by high performance liquid chromatography detection.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (6)

1. A method for extracting betaine from phoenix tree leaves is characterized by comprising the following steps:
pretreatment
Collecting fresh folium Firmianae, cleaning, cutting into filaments, and freeze drying to obtain dried material;
the enzymolysis treatment is carried out
Adding the dried material into pure water with the mass being 5-10 times of that of the dried material, adjusting the pH value to 4.5-6.0 and the temperature to 45-60 ℃, adding a cellulase solution, controlling the concentration of cellulase to be 5-10U/mL, carrying out enzymolysis reaction for 3-5 h, heating to 90-95 ℃, treating for 10-15min, cooling to 70-75 ℃, carrying out microwave treatment for 10-15min, heating to 80-85 ℃, and carrying out constant-temperature treatment for 2-3 h to obtain an enzymolysis material;
concentrating by nanofiltration
Filtering the enzymolysis material by using 2-3 layers of gauze, collecting filtrate, and concentrating by using a nanofiltration membrane to obtain concentrated solution;
fourth step of macroporous adsorbent resin purification
Adsorbing the concentrated solution with NKA-9 macroporous adsorbent resin, eluting with deionized water, and eluting with 30-80% ethanol to obtain eluate containing betaine of folium Firmianae;
drying treatment
Vacuum rotary evaporating the eluate containing firmiana leaf betaine to obtain concentrated solution, and spray drying to obtain firmiana leaf betaine.
2. The method for extracting betaine from phoenix tree leaves as claimed in claim 1, wherein: the freeze drying is to pre-cool the phoenix tree leaf filament to-40 to-60 ℃, to sublimate and dry for 8-20h until the temperature of the phoenix tree leaf filament is 0-10 ℃, and to analyze and dry for 10-20h until the temperature of the phoenix tree leaf filament is 20-30 ℃.
3. The method for extracting betaine from phoenix tree leaves as claimed in claim 1, wherein: the microwave power adopted by the microwave treatment is 450-500W.
4. The method for extracting betaine from phoenix tree leaves as claimed in 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 as claimed in claim 1, wherein: the ratio of the diameter to the height 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 as claimed in 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 ℃.
CN202210038287.1A 2022-01-13 2022-01-13 Extraction method of betaine in phoenix tree leaves Active CN114249666B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112624934A (en) * 2020-12-08 2021-04-09 武汉美味源生物工程有限公司 Method for extracting natural betaine from beet molasses

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CN112624934A (en) * 2020-12-08 2021-04-09 武汉美味源生物工程有限公司 Method for extracting natural betaine from beet molasses

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112624934A (en) * 2020-12-08 2021-04-09 武汉美味源生物工程有限公司 Method for extracting natural betaine from beet molasses

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