CN109824795A - The extracting method of selenium-rich Moringa - Google Patents
The extracting method of selenium-rich Moringa Download PDFInfo
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Abstract
The invention discloses the extracting methods of selenium-rich Moringa, are related to Moringa deep process technology field.The extracting method is based on selenium-rich polysaccharide has good solubility in boiling water, nutritional ingredient is extracted again from the cultural method of selenium-rich Moringa, Polyose extraction purity and yield, waste residue starts with, screening experiment obtains raw material selection pretreatment, Freezing smashing, pressurised extraction, the process that filter residue extracts again, alcohol precipitation is lyophilized, it is scientific and reasonable, not only substantially increase recovery rate, the purity of selenium-rich polysaccharide, total Se content greatly improves simultaneously, a large amount of pterigospermin is extracted in waste residue, significantly improves the economic benefit of Moringa.
Description
Technical field
The present invention relates to Moringa deep process technology fields, and in particular to the extracting method of selenium-rich Moringa.
Background technique
Moringa is Moringaceae Moringa perennial plant, is the primary fast-growing tree in north India Himalayas southern foot
Kind, Drought hardiness is strong, and sandy loam is born in happiness.Root, stem, leaf, flower, seed, branch and the bark of Moringa nutritional ingredient rich in
And medicinal ingredient.Moringa Moringa flavones, polysaccharide compound, protein, amino acid and vitamin rich in etc., wherein
Amino acid can not be synthesized voluntarily comprising human body or synthesis rate is not able to satisfy the essential amino acid itself needed.
It is confirmed through research, protein content is 4 times of milk in leaf of Moringa and benevolence, and the content of Moringa general flavone reaches
6.11%, seed oil-containing 24.5-29.4%, total amino acid content reaches 20.49%, and type reaches 17 kinds.Especially contain 11 kinds
The essential amino acid of human body, Vitamin C content are 7 times of citrus, and vitamin A content is 4 times of carrot, and calcium is the 4 of milk
Times, potassium is 3 times of banana.Moringa polysaccharide is one of effective component important in Moringa, and the polyoses content of different tissues is with root
In at most, minimum in petiole, changes of contents range is 8.16~33.61%, has hypoglycemic, reducing blood lipid, anti-oxidant, disease-resistant
Poison, raising immunity and other effects, extraction and purification process also has received widespread attention and studies.
Research at present about polysaccharide component extraction process in Moringa is more, and Liang Peng et al. is original with Moringa cauline leaf dry powder
Material, extracts the plant polyose in Moringa using water as Extraction solvent, and it is real to have carried out external function to its extract
It tests, it was demonstrated that the inoxidizability of Moringa polysaccharide.Sun Ming et al. using phend-sulphuric acid inquired into Moringa leaf age, organ, the place of production,
The relationship of picking time, management level, direction etc. and Polysaccharides from Leaves of Moringa oleifera content.The extraction of preferable Moringa polysaccharide after study
Condition are as follows: with 15 times of solvent usages, under 90 DEG C of water bath conditions, extract 3 times, each 120min, with this condition, leaf of Moringa
Polyoses content is 25.51%.The patent of application number 201810321043.8 discloses a kind of preparation side of Moringa selenium-rich polysaccharide
Method, by the way that residue and filtrate will be obtained through alcohol extracting, ultrafiltration again after leaf of Moringa frozen drying, crushing, sieving, residue with go
It after ionized water, yeast selenium mixing, is handled through low-temperature circulating, centrifugation extraction, alcohol precipitation, filtering, that vacuum freeze-drying obtains Moringa selenium-rich is more
Sugar, this method significantly improve the combination of polysaccharide and yeast selenium and form stable selenium-rich polysaccharide, will not damage work under low temperature
Property.
Studies have found that having the following problems in polysaccharide extracting process in existing Moringa: 1, Moringa is in planting link
The middle filling for lacking Selenium-rich nutrient solution is applied, so that vane thickness, photosynthesis weaken, the selenium-rich polysaccharide contained in blade petiole is not
It is more；2, after conventional raw material high temperature drying, crushing, a large amount of polysaccharide just be lost with moisture evaporation in dry material, then pass through
It crosses the not high water of dissolubility to mention, so that the purity of polysaccharide and yield substantially reduce；3, containing big in the waste residue, waste liquid after extracting
The nutritional ingredients such as flavonoids, oil ben, the pterigospermin of amount, if the waste of resource will be will cause by directly toppling over, if can be into
One step is subject to extraction and application, will greatly improve the economic benefit of Moringa.
Summary of the invention
In order to solve the above technical problems, the purpose of the present invention is to provide a kind of extracting method of selenium-rich Moringa, bases
In selenium-rich polysaccharide there is good solubility in boiling water, from the cultural method of selenium-rich Moringa, Polyose extraction purity and yield, gives up
Nutritional ingredient is extracted start with again in slag, and screening experiment obtains raw material and pretreatment, Freezing smashing, pressurised extraction, filter residue is selected to mention again
It takes, the process of alcohol precipitation freeze-drying, it is scientific and reasonable, not only substantially increase recovery rate, the purity of selenium-rich polysaccharide, while total Se content
It greatly improves, a large amount of pterigospermin is extracted in waste residue, significantly improve the economic benefit of Moringa.
The purpose of the present invention can be achieved through the following technical solutions:
The present invention provides a kind of extracting methods of selenium-rich Moringa, comprising the following steps:
(1) raw material selection, pretreatment: the tender leaf blade of the selenium-rich Moringa of selection Selenium-rich nutrient solution culture, petiole position,
Vacuum oscillation removes surface dirt particle, after tender leaf blade, petiole surface spraying are mingled with the high speed aqueous vapor of diatomite, continues
Leaf nutrition agent is sprayed, the microwave drying heat conditioning of 50~60s is carried out under the conditions of 75~82 DEG C；
In raw material selection of the invention, after culture is applied in Selenium-rich nutrient solution filling, trace elements of selenium can be with the amino in blade
Sour organic complex forms macromolecule functional group, the directly synthesis of the nutriments such as participation protein, polysaccharide, is not necessarily to photosynthetic conversion
Effect is suitable as the extraction raw material of selenium-rich polysaccharide so selenium element Percentage bound and utilization rate are high.In the process of vacuum oscillation
In, the dust granule of blade, petiole surface can be removed quickly, and high speed aqueous vapor is due to good flow velocity and gasification journey
Degree is mingled with the diatomite of good specific surface area, adsorptivity, can wrap up the colloid substance and oil for taking away blade, petiole surface
Shape impurity.A small amount of aqueous vapor remains in blade, petiole surface, but prolonged high temperature drying be easily destroyed again Moringa flavones,
The nutritional ingredients such as polysaccharide.It is screened by a large amount of experiment condition, finds the microwave drying for carrying out 50~60s at 75~82 DEG C
Heat conditioning after, blade, intrapetiolar nutritional ingredient detection substantially there is no variation, and moisture content be reduced to 1% hereinafter, tool
There is good drying effect.
(2) Freezing smashing: tender leaf blade, petiole after heat conditioning are put into confined chamber, are passed through low-temperature circulating nitrogen, when
After the volume of low temperature nitrogen reaches the 60~70% of closed building volume, impeller 20~30min of rotating shredder, by tender leaf blade, leaf
Handle is crushed to 200~300 targeted fine powders；
Moringa blade, petiole are able to carry out the abundant freezing of cell in the atmosphere of low-temperature circulating nitrogen, form cell
Ice shelf, while using liquid nitrogen be used as abrasive media, realize ultralow temperature crush, reduce hot steam crushing when energy consumption with
Nutrient loss is converted into selenium-rich polysaccharide by flow regime solidifying on the basis of ensureing the grinding partial size of blade, petiole
The water-soluble water that carries out of solid fraction state, later use polysaccharide mentions, and farthest improves recovery rate.
(3) pressurised extraction: fine powder is passed through in extractor, is passed through the purified water of 3 times of amounts, is warming up to 85~93 DEG C,
2h is extracted under 0.1MPa, extracting solution is passed through centrifugal chamber and is separated by solid-liquid separation, and nanofiltration membrane obtains the first supernatant；Continue to add
The purified water for entering 1 times of amount, is warming up to 95~100 DEG C, boosts to 0.12MPa, extracts 1h, and extracting solution is passed through centrifugal chamber and is consolidated
Liquid separation, nanofiltration membrane obtain the second supernatant；The purified water for continuously adding 1 times of amount is warming up to 102~105 DEG C, boosting
To 0.13MPa, 30min is extracted, extracting solution is passed through centrifugal chamber and is separated by solid-liquid separation, and nanofiltration membrane obtains third supernatant；It closes
And collect extraction process generates three times supernatant and filter residue；
During pressurised extraction, the solubility based on selenium-rich polysaccharide in water is substantially better than dissolution in ethanol
Degree, the solubility in boiling water is better than the solubility in warm water, in the solubility being higher than under 1 atmospheric pressure better than normal
The solubility of pressure.Therefore, inventor screens through a large number of experiments, in conjunction with saving water resource and improving recovery rate, to pressurization
Water consumption, pressure, temperature in extraction process have carried out a large amount of screening comparative experiments, and the three above-mentioned stages of discovery progress add
Pressure is extracted, 3 times of amount water of first stage, 85~93 DEG C, extract 2h under the conditions of 0.1MPa, second stage is in 1 times of amount water, 95~100
DEG C, extract 1h under the conditions of 0.12MPa, the phase III extracts 30min under the conditions of 1 times of amount water, 102~105 DEG C, 0.13MPa,
In merging the supernatant detection collected, Moringa selenium-rich polyoses content and total Se content are above other comparison conditions, explanation
Preferably process conditions are obtained.
(4) filter residue extracts again: after filter residue is mixed with deionized water, yeast selenium according to 10:30:0.01, at 40~50 DEG C
After preheating 10min, then it is placed in circular treatment in -5~0 DEG C of microwave environment, be centrifugated, nanofiltration membrane is extracted again
Supernatant；
Inventor has found in merging filter residue research process during to pressurised extraction, in addition to containing a large amount of Moringa
Outside the nutritional ingredients such as flavones, oil ben, or contain a small amount of polysaccharide component.Yeast selenium as good organic selenium source,
In microwave water environment, small part selenium-rich polysaccharide remaining in filter residue can be combined and be assembled, formed water-soluble good
Assemble chemicals, is dissolved in supernatant, improves the recovery rate of selenium-rich polysaccharide.
(5) alcohol precipitation is lyophilized: supernatant is extracted in supernatant that the extraction process three times of step (3) generates and step (4) again
Liquid mixing, is slowly added dropwise dehydrated alcohol, is stirred with 20-40r/min, and liquid bottom generates precipitating, when bottom precipitation is not further added by
When, stop the dropwise addition of dehydrated alcohol, ultrafiltration membrance filter, reduced pressure, freeze-drying, crushing obtain Moringa selenium-rich polysaccharide.
Selenium-rich polysaccharide has a good dissolubility in water, and other nutrition such as Moringa flavones, oil ben, pterigospermin at
Dissolubility is excellent point in alcoholic solvent, and the present invention utilizes the principle of similar compatibility, using high concentration ethanol by the richness in supernatant
Selenium polysaccharide extracts, while freeze-drying will not destroy the chemical structure of selenium-rich polysaccharide, farthest guarantees selenium-rich polysaccharide
Purity.
As a further solution of the present invention, step (1) Selenium-rich nutrient solution the preparation method is as follows: selection it is organic
Selenium converts the water of 200kg as selenium raw material, 100mg organic selenium, and the yeast selenium of 20mg is added, and is stirred continuously completely molten to organic selenium
Solution；Method using Selenium-rich nutrient solution culture selenium-rich Moringa is as follows: after the field planting of Moringa seedling, according to the amount of daily every plant of 10-20mg
It is sprayed；Later every 3-5 days, the amount of every plant of 30-60mg is sprayed；Picking first 1 month, every 3-5 days to blade,
Petiole is sprayed, and is advisable with moistened surface.
Selenium-rich nutrient solution of the invention, organic selenium cooperate yeast selenium, and water is as solvent, the Selenium-rich nutrient solution being prepared,
It acts not only as daily irrigation to use, while selenium element needed for organic selenium supplement Moringa, promotes the synthesis of selenium-rich polysaccharide；
Yeast selenium further participates in the optical effect of Moringa as selenium agent is drawn, promotes its photosynthesis and selenium rich of egg white matter, richness
The synthesis of selenium polysaccharide.Selenium-rich nutrient solution culture selenium-rich Moringa is inventor by largely attempting and testing obtained preferable training
The scheme of supporting to the amount of spraying and sprays the stringent control of position progress in the different phase of Moringa growth, promotes selenium-rich nutritive substance
Synthesis.
As a further solution of the present invention, step (1) the leaf nutrition agent preparation method the following steps are included:
1) fresh aloe leaf is chosen, peeling is cleaned, shape of cutting into chunks is put into wall-breaking machine, and aloe leaf quality is added
1.2-1.5 times of clear water, broken wall are beaten to obtain slurries, and asparagus juice is obtained by filtration；
2) fresh rosemary cauline leaf is chosen, peeling is cleaned, distillate is collected in 100-120 DEG C of distillation, and 4-8 DEG C of refrigeration is standby
With；It is spare that seaweed, pollen pini, chitosan wear into powdery respectively；
3) asparagus juice, distillate, seaweed, pollen pini, chitosan, honey are mixed according to mass ratio 2:1:1:2:0.2:0.5
After closing uniformly, pulp is stirred rapidly, nanofiltration membrane obtains the leaf nutrition agent.
Aloe leaf broken wall is beaten to obtain asparagus juice, the preparation distillation of rosemary cauline leaf by leaf nutrition agent of the invention
Liquid, then obtained with seaweed, pollen pini, chitosan, honey mixing, drying, asparagus juice reed rich in mentioned component
Luxuriant growth acid, lignin, saponin, aloin, containing ingredients such as diosmin, Rosmarinic acids in rosemary distillate, chitosan,
Under the adhesive effect of honey, several ingredients can be well bonded to together, and water-soluble polysaccharide is molten in increase Moringa blade
Out-degree.
As a further solution of the present invention, step (4) the microwave environment circular treatment is specifically in 600-800MHz
30s is handled, 800-1000MHz handles 20s, and 1000-1200MHz handles 10s, circular treatment 3-5 times.
As a further solution of the present invention, the step (3) filter residue that extraction process generates three times and step (4)
Mixed filter residue is obtained after extracting filter residue mixing again, carries out the extraction of pterigospermin, specific steps are as follows:
1) mixed filter residue is crushed, is stirred evenly, put into subcritical abstraction kettle, be added the ethyl alcohol of 80vt%, adjust solid-to-liquid ratio to
1:10 is extracted 3 times, extraction time 30min under the conditions of 0.08~0.1MPa of vacuum degree, 100~120 DEG C of temperature；
2) extracting solution is concentrated under reduced pressure, and cocoanut active charcoal absorption is added, reuses petroleum ether-acetic acid second of volume proportion 3:1
The elution of ester mixed solution, obtains medicinal extract, and medicinal extract is eluted using eluent gradient, merges eluent, is concentrated under reduced pressure and removes elution
Agent is recrystallized using ethyl alcohol in 0-5 DEG C.
It after the present invention mixes the filter residue generated in pressurised extraction and filter residue again extraction process, is extracted, is screened by ethyl alcohol
Preferably solid-to-liquid ratio, vacuum degree, temperature condition out, and pass through the cocoanut active charcoal of good specific surface area, adsorption rate and carry out Moringa
The absorption of element, the gradient elution of dual-solvent system can be monitored by TLC selects highly concentrated eluent section, improves pterigospermin
Purity and yield.
As a further solution of the present invention, the eluant, eluent is ethyl alcohol-petroleum ether system or dichloromethane-petroleum ether
System, two kinds of solvents carry out gradient elution according to the proportion of 1:5,1:4,1:3,1:2.
Beneficial effects of the present invention:
1, the extracting method of selenium-rich Moringa of the invention has good solubility based on selenium-rich polysaccharide in boiling water, from
The cultural method of selenium-rich Moringa, Polyose extraction purity and yield, nutritional ingredient is extracted start with again in waste residue, and screening experiment obtains original
Material selection pretreatment, Freezing smashing, pressurised extraction, the process that filter residue extracts again, alcohol precipitation is lyophilized, it is scientific and reasonable, not only mention significantly
The high recovery rate of selenium-rich polysaccharide, purity, while total Se content greatly improves, and a large amount of pterigospermin is extracted in waste residue, shows
Write the economic benefit for improving Moringa.
2, raw material selection and pretreatment process in, Selenium-rich nutrient solution filling apply culture after, trace elements of selenium can in blade
Amino acid organic complex form macromolecule functional group, the directly synthesis of participation protein, the nutriments such as polysaccharide, no light requirement
Transformation is closed, so selenium element Percentage bound and utilization rate are high, is suitable as the extraction raw material of selenium-rich polysaccharide；In vacuum oscillation
During, high speed aqueous vapor is mingled with the diatomite of good specific surface area, adsorptivity, can wrap up and take away blade, petiole table
The colloid substance and oily impurity in face.
3, it in pressurised extraction process, screens through a large number of experiments, in conjunction with saving water resource and improving recovery rate, to adding
Water consumption, pressure, temperature in pressure extraction process have carried out a large amount of screening comparative experiments, and discovery carries out the three above-mentioned stages
Pressurised extraction, 3 times of amount water of first stage, 85~93 DEG C, extract 2h under the conditions of 0.1MPa, second stage 1 times of amount water, 95~
100 DEG C, extract 1h under the conditions of 0.12MPa, the phase III extracts under the conditions of 1 times of amount water, 102~105 DEG C, 0.13MPa
30min, in merging the supernatant detection collected, Moringa selenium-rich polyoses content and total Se content are above other comparison conditions,
Illustrate to have obtained preferably process conditions.
4, in Selenium-rich nutrient solution preparation, organic selenium cooperates yeast selenium, and water is as solvent, the Selenium-rich nutrient solution being prepared,
It acts not only as daily irrigation to use, while selenium element needed for organic selenium supplement Moringa, promotes the synthesis of selenium-rich polysaccharide；
Yeast selenium further participates in the optical effect of Moringa as selenium agent is drawn, promotes its photosynthesis and selenium rich of egg white matter, richness
The synthesis of selenium polysaccharide.
5, it after the filter residue mixing that pressurised extraction and filter residue generate in extraction process again, is extracted, is filtered out more excellent by ethyl alcohol
Solid-to-liquid ratio, vacuum degree, temperature condition, and pass through the cocoanut active charcoal of good specific surface area, adsorption rate carry out pterigospermin suction
Attached, the gradient elution of dual-solvent system can be monitored by TLC selects highly concentrated eluent section, improves the purity of pterigospermin
And yield.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution in the embodiment of the present invention is clearly and completely retouched
It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention
In embodiment, all other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, shall fall within the protection scope of the present invention.
Embodiment 1
The extracting method of the present embodiment selenium-rich Moringa, comprising the following steps:
(1) raw material selection, pretreatment: the tender leaf blade of the selenium-rich Moringa of selection Selenium-rich nutrient solution culture, petiole position,
Vacuum oscillation removes surface dirt particle, after tender leaf blade, petiole surface spraying are mingled with the high speed aqueous vapor of diatomite, continues
Leaf nutrition agent is sprayed, the microwave drying heat conditioning of 50s is carried out under the conditions of 80 DEG C；Wherein, the preparation method of Selenium-rich nutrient solution
It is as follows: to select organic selenium as selenium raw material, 100mg organic selenium converts the water of 200kg, and the yeast selenium of 20mg is added, is stirred continuously
It is completely dissolved to organic selenium；Method using Selenium-rich nutrient solution culture selenium-rich Moringa is as follows: after the field planting of Moringa seedling, according to daily
The amount of every plant of 10-20mg is sprayed；Later every 3-5 days, the amount of every plant of 30-60mg is sprayed；First 1 month of picking, often
Blade, petiole are sprayed every 3-5 days, are advisable with moistened surface.
The preparation method of leaf nutrition agent the following steps are included:
1) fresh aloe leaf is chosen, peeling is cleaned, shape of cutting into chunks is put into wall-breaking machine, and aloe leaf quality is added
1.2-1.5 times of clear water, broken wall are beaten to obtain slurries, and asparagus juice is obtained by filtration；
2) fresh rosemary cauline leaf is chosen, peeling is cleaned, distillate is collected in 100-120 DEG C of distillation, and 4-8 DEG C of refrigeration is standby
With；It is spare that seaweed, pollen pini, chitosan wear into powdery respectively；3) by asparagus juice, distillate, seaweed, pollen pini, chitosan,
Honey after mixing, stirs rapidly pulp according to mass ratio 2:1:1:2:0.2:0.5, and nanofiltration membrane obtains the blade
Nutritional agents.
(2) Freezing smashing: tender leaf blade, petiole after heat conditioning are put into confined chamber, are passed through low-temperature circulating nitrogen, when
After the volume of low temperature nitrogen reaches the 64% of closed building volume, tender leaf blade, petiole are crushed to by impeller rotating shredder 26min
200~300 targeted fine powders；
(3) pressurised extraction: fine powder is passed through in extractor, is passed through the purified water of 3 times of amounts, 90 DEG C is warming up to, in 0.1MPa
Lower extraction 2h, extracting solution are passed through centrifugal chamber and are separated by solid-liquid separation, and nanofiltration membrane obtains the first supernatant；Continuously add 1 times of amount
Purified water, be warming up to 98 DEG C, boost to 0.12MPa, extract 1h, extracting solution is passed through centrifugal chamber and is separated by solid-liquid separation, nanofiltration membrane
The second supernatant is obtained by filtration；The purified water for continuously adding 1 times of amount, is warming up to 103 DEG C, boosts to 0.13MPa, extracts
30min, extracting solution are passed through centrifugal chamber and are separated by solid-liquid separation, and nanofiltration membrane obtains third supernatant；Merge to collect and extract three times
The supernatant and filter residue that process generates；
(4) filter residue extracts again: after filter residue is mixed with deionized water, yeast selenium according to 10:30:0.01, preheating at 46 DEG C
After 10min, then it is placed in -3 DEG C of microwave environment circular treatment, centrifuge separation, nanofiltration membrane is extracted supernatant and again again
Extract filter residue；Wherein, microwave environment circular treatment is specifically to handle 30s in 600-800MHz, and 800-1000MHz handles 20s,
1000-1200MHz handles 10s, circular treatment 3-5 times.
(5) alcohol precipitation is lyophilized: supernatant is extracted in supernatant that the extraction process three times of step (3) generates and step (4) again
Liquid mixing, is slowly added dropwise dehydrated alcohol, is stirred with 20-40r/min, and liquid bottom generates precipitating, when bottom precipitation is not further added by
When, stop the dropwise addition of dehydrated alcohol, ultrafiltration membrance filter, reduced pressure, freeze-drying, crushing obtain Moringa selenium-rich polysaccharide.
Step (3) filter residue that extraction process generates three times obtains mixing filter with extracting again for step (4) after filter residue mixes
Slag carries out the extraction of pterigospermin, specific steps are as follows:
1) mixed filter residue is crushed, is stirred evenly, put into subcritical abstraction kettle, be added the ethyl alcohol of 80vt%, adjust solid-to-liquid ratio to
1:10 is extracted 3 times, extraction time 30min under the conditions of 0.08~0.1MPa of vacuum degree, 100~120 DEG C of temperature；
2) extracting solution is concentrated under reduced pressure, and cocoanut active charcoal absorption is added, reuses petroleum ether-acetic acid second of volume proportion 3:1
The elution of ester mixed solution, obtains medicinal extract, and medicinal extract is eluted using eluent gradient, merges eluent, is concentrated under reduced pressure and removes elution
Agent is recrystallized using ethyl alcohol in 0-5 DEG C.Wherein, eluant, eluent is ethyl alcohol-petroleum ether system or dichloromethane-petroleum ether body
System, two kinds of solvents carry out gradient elution according to the proportion of 1:5,1:4,1:3,1:2.
Embodiment 2
The extracting method of the present embodiment selenium-rich Moringa, comprising the following steps:
(1) raw material selection, pretreatment: the tender leaf blade of the selenium-rich Moringa of selection Selenium-rich nutrient solution culture, petiole position,
Vacuum oscillation removes surface dirt particle, after tender leaf blade, petiole surface spraying are mingled with the high speed aqueous vapor of diatomite, continues
Leaf nutrition agent is sprayed, the microwave drying heat conditioning of 56s is carried out under the conditions of 78 DEG C；Wherein, the preparation method of Selenium-rich nutrient solution
It is same as Example 1；Method using Selenium-rich nutrient solution culture selenium-rich Moringa is same as Example 1.The system of leaf nutrition agent
Preparation Method is same as Example 1.
(2) Freezing smashing: tender leaf blade, petiole after heat conditioning are put into confined chamber, are passed through low-temperature circulating nitrogen, when
After the volume of low temperature nitrogen reaches the 70% of closed building volume, tender leaf blade, petiole are crushed to by impeller rotating shredder 30min
200~300 targeted fine powders；
(3) pressurised extraction: fine powder is passed through in extractor, is passed through the purified water of 3 times of amounts, 93 DEG C is warming up to, in 0.1MPa
Lower extraction 2h, extracting solution are passed through centrifugal chamber and are separated by solid-liquid separation, and nanofiltration membrane obtains the first supernatant；Continuously add 1 times of amount
Purified water, be warming up to 100 DEG C, boost to 0.12MPa, extract 1h, extracting solution is passed through centrifugal chamber and is separated by solid-liquid separation, nanofiltration
The second supernatant is obtained by filtration in film；The purified water for continuously adding 1 times of amount, is warming up to 104 DEG C, boosts to 0.13MPa, extracts
30min, extracting solution are passed through centrifugal chamber and are separated by solid-liquid separation, and nanofiltration membrane obtains third supernatant；Merge to collect and extract three times
The supernatant and filter residue that process generates；
(4) filter residue extracts again: after filter residue is mixed with deionized water, yeast selenium according to 10:30:0.01, preheating at 50 DEG C
After 10min, then it is placed in 0 DEG C of microwave environment circular treatment, centrifuge separation, nanofiltration membrane is extracted supernatant and again again
Extract filter residue；Wherein, microwave environment circular treatment is specifically to handle 30s in 600-800MHz, and 800-1000MHz handles 20s,
1000-1200MHz handles 10s, circular treatment 3-5 times.
(5) alcohol precipitation is lyophilized: supernatant is extracted in supernatant that the extraction process three times of step (3) generates and step (4) again
Liquid mixing, is slowly added dropwise dehydrated alcohol, is stirred with 20-40r/min, and liquid bottom generates precipitating, when bottom precipitation is not further added by
When, stop the dropwise addition of dehydrated alcohol, ultrafiltration membrance filter, reduced pressure, freeze-drying, crushing obtain Moringa selenium-rich polysaccharide.
Step (3) filter residue that extraction process generates three times obtains mixing filter with extracting again for step (4) after filter residue mixes
Slag, carries out the extraction of pterigospermin, and concrete operation step is same as Example 1.
Embodiment 3
The extracting method of the present embodiment selenium-rich Moringa, comprising the following steps:
(1) raw material selection, pretreatment: the tender leaf blade of the selenium-rich Moringa of selection Selenium-rich nutrient solution culture, petiole position,
Vacuum oscillation removes surface dirt particle, after tender leaf blade, petiole surface spraying are mingled with the high speed aqueous vapor of diatomite, continues
Leaf nutrition agent is sprayed, the microwave drying heat conditioning of 50s is carried out under the conditions of 82 DEG C；Wherein, the preparation method of Selenium-rich nutrient solution
It is same as Example 1；Method using Selenium-rich nutrient solution culture selenium-rich Moringa is same as Example 1.The system of leaf nutrition agent
Preparation Method is same as Example 1.
(2) Freezing smashing: tender leaf blade, petiole after heat conditioning are put into confined chamber, are passed through low-temperature circulating nitrogen, when
After the volume of low temperature nitrogen reaches the 62% of closed building volume, tender leaf blade, petiole are crushed to by impeller rotating shredder 30min
200~300 targeted fine powders；
(3) pressurised extraction: fine powder is passed through in extractor, is passed through the purified water of 3 times of amounts, 87 DEG C is warming up to, in 0.1MPa
Lower extraction 2h, extracting solution are passed through centrifugal chamber and are separated by solid-liquid separation, and nanofiltration membrane obtains the first supernatant；Continuously add 1 times of amount
Purified water, be warming up to 98 DEG C, boost to 0.12MPa, extract 1h, extracting solution is passed through centrifugal chamber and is separated by solid-liquid separation, nanofiltration membrane
The second supernatant is obtained by filtration；The purified water for continuously adding 1 times of amount, is warming up to 105 DEG C, boosts to 0.13MPa, extracts
30min, extracting solution are passed through centrifugal chamber and are separated by solid-liquid separation, and nanofiltration membrane obtains third supernatant；Merge to collect and extract three times
The supernatant and filter residue that process generates；
(4) filter residue extracts again: after filter residue is mixed with deionized water, yeast selenium according to 10:30:0.01, preheating at 50 DEG C
After 10min, then it is placed in -2 DEG C of microwave environment circular treatment, centrifuge separation, nanofiltration membrane is extracted supernatant and again again
Extract filter residue；Wherein, microwave environment circular treatment is specifically to handle 30s in 600-800MHz, and 800-1000MHz handles 20s,
1000-1200MHz handles 10s, circular treatment 3-5 times.
(5) alcohol precipitation is lyophilized: supernatant is extracted in supernatant that the extraction process three times of step (3) generates and step (4) again
Liquid mixing, is slowly added dropwise dehydrated alcohol, is stirred with 20-40r/min, and liquid bottom generates precipitating, when bottom precipitation is not further added by
When, stop the dropwise addition of dehydrated alcohol, ultrafiltration membrance filter, reduced pressure, freeze-drying, crushing obtain Moringa selenium-rich polysaccharide.
Step (3) filter residue that extraction process generates three times obtains mixing filter with extracting again for step (4) after filter residue mixes
Slag, carries out the extraction of pterigospermin, and concrete operation step is same as Example 1.
Comparative example 1
Compared with Example 1, fine powder is passed through in extractor by this comparative example in step (3), is passed through the purifying of 4 times of amounts
Water is warming up to 90 DEG C, and 2h is extracted at 0.1MPa, and extracting solution is passed through centrifugal chamber and is separated by solid-liquid separation, and nanofiltration membrane obtains
One supernatant；The purified waters for continuously adding 2 times of amounts, are warming up to 98 DEG C, boost to 0.12MPa, extract 1h, extracting solution be passed through from
Ventricle is separated by solid-liquid separation, and nanofiltration membrane obtains the second supernatant；The purified water for continuously adding 4 times of amounts, is warming up to 103 DEG C,
0.13MPa is boosted to, 30min is extracted, extracting solution is passed through centrifugal chamber and is separated by solid-liquid separation, and nanofiltration membrane obtains third supernatant
Liquid；Merge the supernatant and filter residue for collecting that extraction process generates three times.
Comparative example 2
Compared with Example 1, fine powder is passed through in extractor by this comparative example in step (3), is passed through the purifying of 3 times of amounts
Water is warming up to 80 DEG C, and 2h is extracted at 0.1MPa, and extracting solution is passed through centrifugal chamber and is separated by solid-liquid separation, and nanofiltration membrane obtains
One supernatant；The purified water for continuously adding 1 times of amount, is warming up to 90 DEG C, boosts to 0.12MPa, extracts 1h, extracting solution be passed through from
Ventricle is separated by solid-liquid separation, and nanofiltration membrane obtains the second supernatant；The purified water for continuously adding 1 times of amount, is warming up to 98 DEG C,
0.13MPa is boosted to, 30min is extracted, extracting solution is passed through centrifugal chamber and is separated by solid-liquid separation, and nanofiltration membrane obtains third supernatant
Liquid；Merge the supernatant and filter residue for collecting that extraction process generates three times.
Comparative example 3
Compared with Example 1, fine powder is passed through in extractor by this comparative example in step (3), is passed through the purifying of 3 times of amounts
Water is warming up to 90 DEG C, and 2h is extracted at 0.09MPa, and extracting solution is passed through centrifugal chamber and is separated by solid-liquid separation, and nanofiltration membrane obtains
First supernatant；The purified water for continuously adding 1 times of amount, is warming up to 98 DEG C, boosts to 0.10MPa, extracts 1h, and extracting solution is passed through
Centrifugal chamber is separated by solid-liquid separation, and nanofiltration membrane obtains the second supernatant；The purified water for continuously adding 1 times of amount, is warming up to 103
DEG C, 0.11MPa is boosted to, 30min is extracted, extracting solution is passed through centrifugal chamber and is separated by solid-liquid separation, and nanofiltration membrane obtains in third
Clear liquid；Merge the supernatant and filter residue for collecting that extraction process generates three times.
Comparative example 4
Compared with Example 1, this comparative example cancellation step (4) filter residue extracts again, and alcohol precipitation freeze-drying directly uses step (3)
The supernatant of preparation is operated.
Supernatant detection
Above-described embodiment 1-3, comparative example 1-4 step (3) are merged and collect the supernatant that extraction process generates three times, is subtracted
Moringa selenium-rich polyoses content is tested using spectrophotometer after pressure concentration, obtains Moringa selenium-rich polysaccharide extract rate and Moringa selenium-rich
Purity of polysaccharide is analyzed total in the Moringa selenium-rich polysaccharide extracted using efficient liquid phase-Hydride Generation-atomic Fluorescence Spectrometry
Se content and organic selenium content.Concrete outcome is shown in Table 1:
1. supernatant testing result of table
As can be seen from the above table, in the supernatant that the embodiment of the present invention is prepared by pressurised extraction, contain higher concentration
Selenium-rich polysaccharide, organic selenium, total selenium illustrate that this method is suitable for the industrialization extraction production of selenium-rich polysaccharide.
Finished product detection
To the Moringa selenium-rich polysaccharide finished product of above-described embodiment 1-3, comparative example 1-4 preparation, tested using spectrophotometer peppery
The wooden selenium-rich polyoses content obtains Moringa selenium-rich polysaccharide extract rate and Moringa selenium-rich purity of polysaccharide, utilizes efficient liquid phase-hydride
The total Se content and organic selenium content in Moringa selenium-rich polysaccharide that Generation-Atomic Fluorescence Spectrometry analysis is extracted.Concrete outcome
It is shown in Table 2:
2. finished product detection result of table
As can be seen from the above table, the selenium-rich polysaccharide finished product of preparation of the embodiment of the present invention, either recovery rate, purity, organic
Se content, total Se content are above comparative example.Comparative example 1-3 on amount of water, temperature, pressure parameter due to carrying out respectively
Screening, is unable to reach the extraction effect of embodiment.Comparative example 4 is mentioned again due to the filter residue not generated to step (3)
It takes, so that remaining a large amount of selenium-rich polysaccharide in filter residue, reduces the economic benefit of Moringa blade, petiole.
In the description of this specification, the description meaning of reference term " one embodiment ", " example ", " specific example " etc.
Refer to that particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one reality of the invention
It applies in example or example.In the present specification, schematic expression of the above terms are not necessarily referring to identical embodiment or show
Example.Moreover, particular features, structures, materials, or characteristics described can be in any one or more embodiment or examples
In can be combined in any suitable manner.
Above content is only citing made for the present invention and explanation, affiliated those skilled in the art are to institute
The specific embodiment of description does various modifications or additions or is substituted in a similar manner, without departing from invention or
Person beyond the scope defined by this claim, is within the scope of protection of the invention.
Claims (6)
1. the extracting method of selenium-rich Moringa, which comprises the following steps:
(1) raw material selection, pretreatment: the tender leaf blade of the selenium-rich Moringa of selection Selenium-rich nutrient solution culture, petiole position, vacuum vibration
It swings and removes surface dirt particle, after tender leaf blade, petiole surface spraying are mingled with the high speed aqueous vapor of diatomite, continue to spray blade
Nutritional agents carries out the microwave drying heat conditioning of 50~60s under the conditions of 75~82 DEG C；
(2) Freezing smashing: tender leaf blade, petiole after heat conditioning are put into confined chamber, are passed through low-temperature circulating nitrogen, are worked as cryogenic nitrogen
After the volume of gas reaches the 60~70% of closed building volume, impeller 20~30min of rotating shredder crushes tender leaf blade, petiole
To 200~300 targeted fine powders；
(3) pressurised extraction: fine powder is passed through in extractor, is passed through the purified water of 3 times of amounts, 85~93 DEG C is warming up to, in 0.1MPa
Lower extraction 2h, extracting solution are passed through centrifugal chamber and are separated by solid-liquid separation, and nanofiltration membrane obtains the first supernatant；Continuously add 1 times of amount
Purified water, be warming up to 95~100 DEG C, boost to 0.12MPa, extract 1h, extracting solution is passed through centrifugal chamber and is separated by solid-liquid separation, received
Membrane filtration obtains the second supernatant；The purified water for continuously adding 1 times of amount, is warming up to 102~105 DEG C, boosts to 0.13MPa,
30min is extracted, extracting solution is passed through centrifugal chamber and is separated by solid-liquid separation, and nanofiltration membrane obtains third supernatant；Merge and collects three times
The supernatant and filter residue that extraction process generates；
(4) filter residue extracts again: after filter residue is mixed with deionized water, yeast selenium according to 10:30:0.01, preheating at 40~50 DEG C
After 10min, then be placed in -5~0 DEG C of microwave environment circular treatment, centrifuge separation, nanofiltration membrane extracted again supernatant and
Filter residue is extracted again；
(5) alcohol precipitation is lyophilized: the supernatant that extracts again of supernatant and step (4) that the extraction process three times of step (3) generates is mixed
It closes, dehydrated alcohol is slowly added dropwise, is stirred with 20-40r/min, liquid bottom generates precipitating, when bottom precipitation is not further added by, stops
The only dropwise addition of dehydrated alcohol, ultrafiltration membrance filter, reduced pressure, freeze-drying, crushing obtain Moringa selenium-rich polysaccharide.
2. the extracting method of selenium-rich Moringa according to claim 1, which is characterized in that step (1) Selenium-rich nutrient solution
The preparation method is as follows: selecting organic selenium as selenium raw material, 100mg organic selenium converts the water of 200kg, the yeast selenium of 20mg is added,
It is stirred continuously to organic selenium and is completely dissolved；Method using Selenium-rich nutrient solution culture selenium-rich Moringa is as follows: after the field planting of Moringa seedling, pressing
It is sprayed according to the amount of daily every plant of 10-20mg；Later every 3-5 days, the amount of every plant of 30-60mg is sprayed；Pick first 1
Month, blade, petiole are sprayed every 3-5 days, are advisable with moistened surface.
3. the extracting method of selenium-rich Moringa according to claim 1, which is characterized in that step (1) the leaf nutrition agent
Preparation method the following steps are included:
1) fresh aloe leaf is chosen, peeling is cleaned, shape of cutting into chunks is put into wall-breaking machine, and aloe leaf quality 1.2- is added
1.5 times of clear water, broken wall are beaten to obtain slurries, and asparagus juice is obtained by filtration；
2) fresh rosemary cauline leaf is chosen, peeling is cleaned, distillate is collected in 100-120 DEG C of distillation, and 4-8 DEG C of refrigeration is spare；Sea
It is spare that algae, pollen pini, chitosan wear into powdery respectively；
3) asparagus juice, distillate, seaweed, pollen pini, chitosan, honey are mixed according to mass ratio 2:1:1:2:0.2:0.5 equal
After even, pulp is stirred rapidly, and nanofiltration membrane obtains the leaf nutrition agent.
4. the extracting method of selenium-rich Moringa according to claim 1, which is characterized in that step (4) microwave environment follows
Ring processing is specifically at 600-800MHz processing 30s, 800-1000MHz processing 20s, 1000-1200MHz processing 10s, circulation
Reason 3-5 times.
5. the extracting method of selenium-rich Moringa according to claim 1, which is characterized in that the step (3) was extracted three times
The filter residue that journey generates obtains mixed filter residue with being extracted after filter residue mixes again for step (4), carries out the extraction of pterigospermin, concrete operations
Steps are as follows:
1) mixed filter residue is crushed, is stirred evenly, put into subcritical abstraction kettle, be added the ethyl alcohol of 80vt%, adjust solid-to-liquid ratio to 1:10,
It is extracted 3 times under the conditions of 0.08~0.1MPa of vacuum degree, 100~120 DEG C of temperature, extraction time 30min；
2) extracting solution is concentrated under reduced pressure, and cocoanut active charcoal absorption is added, and the petroleum ether-ethyl acetate for reusing volume proportion 3:1 is mixed
Solution elution is closed, medicinal extract is obtained, medicinal extract is eluted using eluent gradient, merges eluent, is concentrated under reduced pressure and is removed eluant, eluent, is used
Ethyl alcohol is recrystallized in 0-5 DEG C.
6. the extracting method of selenium-rich Moringa according to claim 5, which is characterized in that the eluant, eluent is ethyl alcohol-petroleum
Ether system or dichloromethane-petroleum ether system, two kinds of solvents carry out gradient elution according to the proportion of 1:5,1:4,1:3,1:2.
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| CN116622002A (en) * | 2023-06-12 | 2023-08-22 | 湖南绿蔓生物科技股份有限公司 | Preparation method of moringa oleifera leaf extract |
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