CN106279461B - A kind of selenizing maca polysaccharide and its preparation method and application - Google Patents
A kind of selenizing maca polysaccharide and its preparation method and application Download PDFInfo
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Abstract
A kind of selenizing maca polysaccharide and its preparation method and application.The preparation method includes that (1) maca polysaccharide is added in aqueous acid, dissolution, and selenizing agent is added, and heating reaction obtains selenylation reaction liquid；(2) selenylation reaction liquid cooling obtained by step (1) but, is then separated by solid-liquid separation, collects supernatant, cleans；(3) supernatant obtained by step (2) is concentrated, it is dry, obtain selenizing maca polysaccharide.The selenizing maca polysaccharide of method preparation of the invention has the double effects of maca polysaccharide and organic selenium concurrently, improves the added value of maca polysaccharide, is more conducive to be absorbed by organisms utilization, product shows higher bioactivity, has broad application prospects.
Description
Technical field
The present invention relate to a kind of chemical synthesis process more particularly to a kind of selenizing modification maca polysaccharide and preparation method thereof and
Purposes belongs to the field of deep of maca polysaccharide.
Background technique
Selenium is the essential trace elements of the human body, is the main active of glutathione peroxidase, can directly or
Internal oxygen radical is removed indirectly, inhibits lipid oxidation or peroxidating, the pathogenic effects of blocking activity oxygen and free radical, protection is carefully
Born of the same parents safeguard the stability of cell membrane from the damage of peroxide, to the growth of animal, breeding, immune, anti-infective, resisting stress
Etc. play an important role.Investigation shows that China has 2/3rds or more regional half populations to be in selenium deficiency, low selenium band,
Minimum requirements amount is not achieved in the selenium amount taken in by ordinary meal, so that disease incidence related with selenium deficiency greatly improves.
Strengthen the effective way that selenium is Selenium Supplement in food.The selenium hardening agent in China includes inorganic selenium and organic selenium two
Kind, inorganic selenium mainly has sodium selenite and sodium selenate, and organic selenium mainly has selenoprotein, Se-enriched yeast, selenide of carragheen, selenium more
Sugar, selenoaminoacid, seleno nucleic acid etc..Although inorganic selenium selenium content is high and cheap, absorption is undesirable, and biological effectiveness is low,
It is more toxic, thus is strictly limited its usage amount.It is strong as the nutrition of selenium that developed country has not had to simple inorganic salt form
Agent, currently, the developed countries such as Japan, U.S. have forbidden adding the inorganic seleniums such as sodium selenite in food.And organic selenium is then
It is highly-safe, it is not susceptible to be poisoned, be easily absorbed by the body utilization, and selenium-supply is high-efficient, and bioactivity is high.Therefore, preparation safety,
Efficient organic selenium compounds are an important contents of selenium chemical research.
Selenium polysaccharide is the organic selenium compounds that selenium is bonded with active polysaccharide, has function of both polysaccharide and selenium, toxicity concurrently
It is substantially reduced with side effect, therefore shows more effective physiological activity, can be used as a kind of selemium nutrition safely, effectively, healthy
Source.The activity of selenium polysaccharide is higher than selenium and polysaccharide, is more advantageous to and is absorbed by organisms utilization, develops and uses and cause the wide of the world
General concern.It is demonstrated experimentally that selenium polysaccharide has anti-metal poisoning, anti-oxidant, inhibiting tumor cell and virus, immunological regulation, anti-aging etc.
Pharmacological action.With being constantly progressive for society, people's lives level is gradually increased, and is increasingly paid close attention to the health of itself, this
Just urgently need more selenium polysaccharide launch.
Currently, there are mainly two types of the preparation methods of selenium polysaccharide, i.e. biological concentration method and chemical synthesis.Biological concentration legal system
The standby period is long, and condition should not control, and it is difficult to produce feasibility in enormous quantities.In the chemical production processes of selenium polysaccharide, it is common to use pyrrole
The toxic organic solvents such as pyridine, benzene, thionyl chloride, to influence application of the selenizing polysaccharide in food.
Maca is a kind of Cruciferae Lepidium plant with high nutritive value and pharmacology value, and maca polysaccharide is Ma
One of effective component of coffee.Modern pharmacology research confirms that maca polysaccharide has various biological activity, wherein with anti-oxidant, anti-
Aging and anti-fatigue active research are more.Chen Yanqing (carboxymethyl maca polysaccharide preparation and Study of Antioxidation, Chinese food addition
Agent, 2010,2:94-96) maca polysaccharide has carried out carboxy methylation modification, and maca polysaccharide is to hydroxy radical after finding carboxy methylation
Scavenging activity improves 2 times.CN103739729A discloses a kind of Indigowoad root selenium polysaccharide and preparation method thereof, in selenylation reaction
Barium chloride is added as catalyst, but barium ions is a kind of toxic substance, influences its safety.
Different method of modifying is different to the activity influence of polysaccharide, and the selenium after the selenizing of maca polysaccharide modification and modification
There is not been reported for the research of change maca polysaccharide.
Summary of the invention
In view of the deficiencies of the prior art, an object of the present invention is to provide a kind of preparation method of selenizing maca polysaccharide,
The pharmacological function of selenium and maca polysaccharide is set to be optimized integration, activity is apparently higher than selenium or maca polysaccharide, and is conducive to by body
It is absorbed and utilized.
In order to achieve the above object, the present invention adopts the following technical scheme:
A kind of preparation method of selenizing maca polysaccharide, includes the following steps:
(1) maca polysaccharide is added in aqueous acid, dissolution, selenizing agent is added, heating reaction obtains selenylation reaction liquid；
(2) selenylation reaction liquid cooling obtained by step (1) but, is then separated by solid-liquid separation, collects supernatant, cleans；
(3) supernatant obtained by step (2) is concentrated, it is dry, obtain selenizing maca polysaccharide.
The present invention carries out catalysis reaction using acid solution, greatly reduces the residual of later period heavy metal barium ions, makes to be made
Product it is safer.
Preferably, aqueous acid described in step (1) is nitric acid solution, sulfuric acid solution, phosphoric acid solution, perchloric acid is molten
The combination of one or more of liquid.
Preferably, volumetric concentration sour in the aqueous acid be 0.5-5%, for example, 1%, 1.5%, 2%, 2.5%,
3%, 3.5%, 4%, 4.5% etc., preferably 0.5-2%.
Preferably, the selenizing agent is sodium selenite and/or selenous acid.
Preferably, the mass ratio of the selenizing agent and maca polysaccharide be 1:5-30, for example, 1:7,1:9,1:12,1:15,
1:19,1:22,1:26,1:29 etc..
Preferably, the temperature of the heating reaction is 30-90 DEG C, for example, 35 DEG C, 39 DEG C, 43 DEG C, 48 DEG C, 55 DEG C, 60
DEG C, 66 DEG C, 71 DEG C, 78 DEG C, 84 DEG C, 88 DEG C etc., time 1-9h, for example, 1.5h, 3h, 5h, 7h, 8.5h etc..
Preferably, cooling temperature described in step (2) is 10-35 DEG C.
Preferably, the removal of impurities is dialysis and/or film filtering.It can be by the residual of selenizing agent using dialysis and/or film filtering
It reduces, obtained selenizing maca polysaccharide has more safety；Simultaneously compared with the prior art in common alcohol precipitating method more save
Process, reduces costs.
Preferably, step (3) can also be following process: 3-5 times of volume of concentrate being added after supernatant is concentrated
Dehydrated alcohol is precipitated, and separation by drying precipitate, obtains selenizing maca polysaccharide.Wherein separation can be used commonly used in the art
Technological means, such as centrifugation, filtering.
Preferably, the drying in step (3) is vacuum drying and/or freeze-drying.
The selenium content of the obtained selenizing maca polysaccharide of the present invention is 1-10 μ g/mg.Resulting selenizing maca polysaccharide is being protected
On the basis of demonstrate,proving its bioactivity, the content of selenium is greatly reduced, advantageously reduces production cost, while it is more to improve selenizing maca
The safety of sugar.
An object of the present invention, which also resides in, provides the selenizing maca polysaccharide of preparation method preparation of the present invention.The present invention
The antioxidant activity of the selenizing maca polysaccharide of preparation is higher than maca polysaccharide.
An object of the present invention, which also resides in, provides selenizing maca polysaccharide of the invention in anti-oxidant and selenium supplement
Using.
It preferably, can be using selenizing maca polysaccharide as phases such as adjuvant treatment aging, tumour, immunity degradation or skin diseases
Close the raw material of drug, health food and cosmetics.
Preferably, ordinary food, health food and feed can be used for using selenizing maca polysaccharide as organic selenium supplement
In raw material.
Compared with prior art, the present invention having following technical advantage:
(1) selenium is introduced into the sugar unit of maca polysaccharide by the present invention, is prepared selenizing maca polysaccharide, is effectively reduced sub- selenium
The toxicity of acid groups obtains selenizing maca polysaccharide soluble easily in water, improves the selenium content of polysaccharide, has to free radical significant clear
Except effect, it is more conducive to be absorbed by organisms utilization.
(2) present invention can be reduced the residual of selenizing agent, obtained selenizing maca by the method for dialysis or film filtering
Polysaccharide has more safety.
(3) any organic solvent is not used in the present invention, is avoided pollution-free to environment and product.Selenylation reaction condition can
Control, production equipment is of less demanding, and production cost is low, is easy to realize industrial production.
(4) selenizing maca polysaccharide prepared by the present invention can be used as efficient, less toxic organic selenium supplement application to food, guarantor
In strong product and feed, selenium element necessary to human body or animal is provided.In addition, selenizing maca polysaccharide has good anti-oxidant work
Property, the exploitation of corresponding cosmetics is had far-reaching significance.
Detailed description of the invention
Fig. 1 is the infrared spectrogram of maca polysaccharide；
Fig. 2 is the infrared spectrogram of selenizing maca polysaccharide prepared by embodiment 1.
Specific embodiment
Of the invention for ease of understanding, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is used only for helping to understand the present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1: the preparation of selenizing maca polysaccharide
(1) nitric acid solution that 0.5g maca polysaccharide is added 0.5% is dissolved, 0.1g sodium selenite is added, 30 DEG C add
Thermal response 9h obtains selenylation reaction liquid；
(2) selenylation reaction liquid is cooled to 20 DEG C, centrifugation collects supernatant, dialyses；
(3) solution in bag filter is concentrated, is dried in vacuo, obtain 0.1g selenizing maca polysaccharide, selenium content is 10 μ
g/mg。
Embodiment 2: the preparation of selenizing maca polysaccharide
(1) sulfuric acid solution that 10g maca polysaccharide is added 2% is dissolved, 1g selenous acid, 90 DEG C of heating reactions is added
1h obtains selenylation reaction liquid；
(2) selenylation reaction liquid is cooled to 10 DEG C, centrifugation is collected supernatant, is added in ultrafiltration membrane, and film filtering is carried out；
(3) solution in ultrafiltration membrane is concentrated, is freeze-dried, obtain 2.8g selenizing maca polysaccharide, selenium content is 1 μ
g/mg。
Embodiment 3: the preparation of selenizing maca polysaccharide
(1) phosphoric acid solution that 5g maca polysaccharide is added 5% is dissolved, 0.33g sodium selenite is added, 60 DEG C of heating are anti-
5h is answered, selenylation reaction liquid is obtained；
(2) selenylation reaction liquid is cooled to 35 DEG C, centrifugation collects supernatant, dialyses；
(3) solution in bag filter is concentrated, is freeze-dried, obtain 1.5g selenizing maca polysaccharide, selenium content is 5 μ
g/mg。
Embodiment 4: the preparation of selenizing maca polysaccharide
(1) perchloric acid solution that 20g maca polysaccharide is added 3.5% is dissolved, 1g selenous acid is added, 45 DEG C of heating are anti-
3h is answered, selenylation reaction liquid is obtained；
(2) selenylation reaction liquid is cooled to 15 DEG C, supernatant is collected in centrifugation, and ultrafiltration membrane is first added and is filtered, adds
Nanofiltration membrane is filtered；
(3) solution in nanofiltration is concentrated, is dried in vacuo, obtain 5g selenizing maca polysaccharide, selenium content is 3 μ g/mg.
Embodiment 5: the preparation of selenizing maca polysaccharide
(1) nitric acid solution that 100g maca polysaccharide is added 4% is dissolved, 4g sodium selenite is added, 75 DEG C of heating are anti-
7h is answered, selenylation reaction liquid is obtained；
(2) selenylation reaction liquid is cooled to 25 DEG C, centrifugation collects supernatant, dialyses；
(3) solution in bag filter is concentrated, is dried in vacuo, obtain 26g selenizing maca polysaccharide, selenium content is 8 μ g/
mg。
Embodiment 6: the preparation of selenizing maca polysaccharide
(1) phosphoric acid solution that 1g maca polysaccharide is added 0.5% is dissolved, 0.04g sodium selenite, 80 DEG C of heating is added
8h is reacted, selenylation reaction liquid is obtained；
(2) selenylation reaction liquid is cooled to 18 DEG C, centrifugation collects supernatant, dialyses；
(3) solution in bag filter is concentrated, is dried in vacuo, obtain 0.22g selenizing maca polysaccharide, selenium content is 6 μ
g/mg。
Embodiment 7: the verifying of selenizing maca polysaccharide
The selenizing maca polysaccharide for taking maca polysaccharide and embodiment 1 to prepare respectively is a little, carries out after addition KBr tabletting infrared
Scanning, Fig. 1 and Fig. 2 are respectively the infrared spectrogram of maca polysaccharide and selenizing maca polysaccharide.
Fig. 2 and Fig. 1 are compared, it can be seen that selenizing maca polysaccharide is in 400-4000cm-1The infrared spectroscopy of range with
Maca polysaccharide is closely similar, shows that it still remains the structure of polysaccharide, i.e., in 3200-3600cm-1There is a broad peak, is polysaccharide
The stretching vibration of upper-OH, in 2900cm-1There is the stretching vibration peak that C-H is weaker, in 1600-1700cm-1There is C=O absorption peak,
Fig. 2 is in 808cm-1And 668cm-1There is the vibration absorption peak of Se=O key and selenic acid ester (Se-O-C) respectively in place, and in Fig. 1 then
No, show that the selenizing of maca polysaccharide is modified successfully.
Embodiment 8: the reducing power measurement of selenizing maca polysaccharide
The reducing power of selenizing maca polysaccharide and maca polysaccharide the results are shown in Table 1.Sample with reproducibility, can be by ferric iron
It is converted into ferrous iron, the latter has stronger absorption in 700nm, and therefore, reducing power is stronger, and light absorption value is higher.As it can be seen that with selenium
The raising for changing maca polysaccharide concentration, the absorption value detail at 700nm improve, good linear relationship are presented, illustrates selenizing
Maca reproducibility with higher.
1 selenizing maca polysaccharide reducing power experimental result of table
Embodiment 9: selenizing maca polysaccharide removes the experiment of DPPH free radical
The removing DPPH free radical of selenizing maca polysaccharide and maca polysaccharide the results are shown in Table 2.It is more with the maca of same concentrations
Sugar is compared, and selenizing maca polysaccharide significantly improves the clearance rate of DPPH free radical, and it is preferable clear to illustrate that selenizing maca polysaccharide has
Except the activity of DPPH free radical.
2 selenizing maca polysaccharide of table removes DPPH experimental result
Embodiment 10: selenizing maca polysaccharide removes the experiment of ABTS free radical
The removing ABTS free radical of selenizing maca polysaccharide and maca polysaccharide the results are shown in Table 3.It is more with the maca of same concentrations
Sugar is compared, and selenizing maca polysaccharide significantly improves the clearance rate of ABTS free radical, and when concentration is 0.5mg/ml, selenizing maca is more
Sugar reaches 60.78% to the clearance rate of ABTS free radical, is 1.8 times of selenizing polysaccharide, and it is preferable to illustrate that selenizing maca polysaccharide has
Removing ABTS free radical activity.
3 selenizing maca polysaccharide of table removes ABTS experimental result
Embodiment 11: the anti-tumor experiment of selenizing maca polysaccharide
The selenizing maca polysaccharide that maca polysaccharide and embodiment 3 obtain is made into the solution of 6mg/ml respectively, using mtt assay into
Row anti-tumor activity, two kinds of polysaccharide the results are shown in Table 4 to the inhibiting rate of different tumour cells, compared with maca polysaccharide, selenizing maca
Polysaccharide significantly improves the inhibiting rate of different tumour cells.
4 selenizing maca polysaccharide anti-tumor experiment result of table
Embodiment 12: selenizing maca polysaccharide improves immunity experiment
The selenizing maca polysaccharide that embodiment 5 is obtained carries out improving immunity experiment, is taken and is recommended according to the population of tested material
Dosage sets low, middle and high dose groups, respectively 500,1500,4500mg/kgbw, while setting 1 control group.It is examined using mtt assay
The mouse lymphocyte for surveying ConA induction is proliferated transformation function, and ear swelling method detects the delayed allergy of mouse, as a result sees
Table 5.
5 selenizing maca polysaccharide of table improves immunity result
| Group | Dosage (mg/kgbw) | Lymphopoiesis ability (OD) | Left and right auricle weight difference |
| Control group | -- | 0.27±0.06 | 10.76±3.11 |
| Low dosage | 500 | 0.32±0.04 | 11.07±4.02 |
| Middle dosage | 1500 | 0.35±0.08 | 13.62±3.76 |
| High dose | 4500 | 0.46±0.03* | 18.35±2.53* |
*: compared with the control group, significant difference, P < 0.05.
As shown in Table 5, compared with the control group, the mouse lymphocyte proliferative capacity of selenizing maca polysaccharide high dose group induction
It is remarkably reinforced；The degree of the difference reflection delayed allergy of left and right auricle weight, the weight difference of given the test agent high dose group
Value is apparently higher than control group, it is possible to determine that this experimental result is positive, i.e., there is selenizing maca polysaccharide preferable improve to be immunized
Power effect.
Embodiment 13: application of the selenizing maca polysaccharide in food
Maca pressed candy is made in the selenizing maca polysaccharide that embodiment 1 obtains, is formulated are as follows: selenizing maca polysaccharide 50g, Ma
Coffee powder 900g, xylitol 50g play the role of Selenium Supplement.
Embodiment 14: application of the selenizing maca polysaccharide in health food
Maca capsule is made in the selenizing maca polysaccharide that embodiment 2 obtains, is formulated are as follows: selenizing maca polysaccharide 100g, maca
Extract 800g, dextrin 50g, microcrystalline cellulose 50g play the role of strengthen immunity.
Its application method are as follows: after mixing by selenizing maca polysaccharide and health food, according to health food before mixing
Application method uses, and compared with the health food for being not added with selenizing maca polysaccharide, free radical scavenging activity improves 16.11%, plays
Remove the effect of free radical, anti-aging, Selenium Supplement.
Embodiment 15: application of the selenizing maca polysaccharide in feed
The selenizing maca polysaccharide that embodiment 6 obtains is applied in feed, in terms of the gross mass of feed, selenizing maca polysaccharide
Account for the 1-5% of total feed quality, application method are as follows: after mixing by selenizing maca polysaccharide and feed, according to making for feed
With method feeding piglet, compared with the control group, the piglet for eating selenizing maca polysaccharide improves weight gain 10.56%.
The Applicant declares that the present invention is explained by the above embodiments detailed process equipment and process flow of the invention,
But the present invention is not limited to the above detailed process equipment and process flow, that is, it is above-mentioned detailed not mean that the present invention must rely on
Process equipment and process flow could be implemented.It should be clear to those skilled in the art, any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within of the invention
Within protection scope and the open scope.
Claims (13)
1. a kind of preparation method of selenizing maca polysaccharide, includes the following steps:
(1) maca polysaccharide is added in aqueous acid, dissolution, selenizing agent is added, heating reaction obtains selenylation reaction liquid；
(2) selenylation reaction liquid cooling obtained by step (1) but, is then separated by solid-liquid separation, collects supernatant, cleans；
(3) supernatant obtained by step (2) is concentrated, it is dry, obtain selenizing maca polysaccharide；
Selenizing agent described in step (1) is sodium selenite and/or selenous acid；
The mass ratio of selenizing agent described in step (1) and maca polysaccharide is 1:5-30.
2. preparation method according to claim 1, which is characterized in that aqueous acid described in step (1) is that nitric acid is molten
The combination of one or more of liquid, sulfuric acid solution, phosphoric acid solution, perchloric acid solution.
3. preparation method according to claim 2, which is characterized in that sour volumetric concentration is 0.5- in the aqueous acid
5%.
4. preparation method according to claim 3, which is characterized in that sour volumetric concentration is 0.5- in the aqueous acid
2%.
5. preparation method according to claim 1, which is characterized in that the temperature for heating reaction described in step (1) is 30-
90 DEG C, time 1-9h.
6. preparation method according to claim 1, which is characterized in that cooling temperature described in step (2) is 10-35 DEG C.
7. preparation method according to claim 1, which is characterized in that removal of impurities described in step (2) is dialysis and/or film mistake
Filter.
8. preparation method according to claim 1, which is characterized in that step (3) further includes following process: supernatant is dense
The dehydrated alcohol that 3-5 times of volume of concentrate is added after contracting is precipitated, and is separated, by drying precipitate, is obtained selenizing maca polysaccharide.
9. preparation method according to claim 1, which is characterized in that drying in step (3) is vacuum drying and/or cold
It is lyophilized dry.
10. a kind of selenizing maca polysaccharide of the preparation of preparation method described in claim 1.
11. selenizing maca polysaccharide described in any one of claim 10 is preparing the purposes in antioxidant and selenium supplement.
12. purposes described in claim 11, which is characterized in that the selenizing maca polysaccharide is as preparation adjuvant treatment aging medicine
The raw material of object, the raw material of adjuvant therapy of tumors drug, the raw material for assisting in the treatment of immunity degradation drug, adjuvant treatment skin disease phase
Close raw material, the raw material of health food or the raw material of cosmetics of drug.
13. purposes described in claim 11 or 12, which is characterized in that the selenizing maca polysaccharide is used as organic selenium supplement
Raw material in ordinary food, health food and feed.
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| CN107011458B (en) * | 2017-06-06 | 2018-10-09 | 淮阴师范学院 | Selenizing lotus root polysaccharide and its preparation method and application |
| CN108200990A (en) * | 2017-12-06 | 2018-06-26 | 芜湖市欣然食品有限公司 | A kind of preparation method for consolidating lipid-loweringing selenizing bitter leaves tea polysaccharide meal replacement powder |
| CN108456258B (en) * | 2018-04-24 | 2020-07-03 | 重庆工业职业技术学院 | Preparation method of dendrobium officinale selenium polysaccharide |
| CN108314746B (en) * | 2018-04-24 | 2020-06-30 | 重庆工业职业技术学院 | Dendrobium officinale selenium polysaccharide |
| CN109912726B (en) * | 2018-09-29 | 2021-05-04 | 北方民族大学 | Phellinus linteus polysaccharide derivative, preparation method and application thereof |
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