CN113307892A - Tremella polysaccharide iron (III) compound and preparation method thereof - Google Patents
Tremella polysaccharide iron (III) compound and preparation method thereof Download PDFInfo
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- CN113307892A CN113307892A CN202110747861.6A CN202110747861A CN113307892A CN 113307892 A CN113307892 A CN 113307892A CN 202110747861 A CN202110747861 A CN 202110747861A CN 113307892 A CN113307892 A CN 113307892A
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- iron
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
Abstract
The invention discloses a tremella polysaccharide iron (III) compound and a preparation method thereof. The preparation method comprises the following steps: dissolving sodium citrate and tremella polysaccharide in deionized water, and stirring in a water bath at 50-80 ℃ to dissolve the sodium citrate and the tremella polysaccharide to form a mixed solution; adding an iron chloride solution and a sodium hydroxide solution into the mixed solution until the pH value of the mixed solution is 8.0-8.5 to form a reaction solution until insoluble substances appear in the reaction solution; and (3) continuing heating in a water bath at 50-80 ℃, stirring, stopping stirring, and separating and purifying insoluble substances to obtain the tremella polysaccharide iron (III) compound. The tremella polysaccharide iron compound prepared by the invention has high iron content.
Description
Technical Field
The invention relates to a tremella polysaccharide and iron (III) compound and a preparation method thereof, belonging to the technical field of biological medicines.
Background
Tremella fuciformis (also called Tremella fuciformis), which belongs to the order Tremellales and family Tremellaceae, is an edible fungus. The tremella polysaccharide is a main active ingredient, mainly comprises mannose, glucuronic acid, glucose, galactose, xylose and rhamnose, and has multiple physiological activities of resisting oxidation, resisting tumors, inhibiting inflammation and the like. The fermentation process can enrich the composition and molecular weight of the polysaccharide through medium composition and other factors. Compared with the traditional tremella polysaccharide extracted from sporocarp, the tremella polysaccharide obtained by fermentation has smaller molecular weight and stronger activity.
Iron is active as a cofactor for metabolic and immune functions and is critical to the normal function of the organism. Since iron is mainly present in blood, iron deficiency anemia is inevitably produced once a human body becomes iron deficient. The most common form of anemia is known as Iron Deficiency Anemia (IDA). According to the world health organization (world health organization) data, 43% of children worldwide are affected by anemia. In 2002, iron deficiency anemia affects 20 billion of people, especially 90% of children and pregnant women, and is considered to be a major cause of global disease burden. Iron deficiency anemia is ubiquitous nutritional deficiency anemia in China, affects a wide population and a high incidence rate, and seriously affects the health and the life quality of people. The oral iron supplement is the cheapest and most effective treatment method, but the side effect of the oral iron supplement is gastrointestinal tract disorder, such as nausea, heartburn or pain, constipation and diarrhea, meanwhile, the annual morbidity and mortality caused by accidental excessive use of iron salt are very obvious, the iron content of the current iron supplement is low, the dosage of a patient is large, the iron (III) is complexed with tremella polysaccharide image produced by liquid fermentation with good activity, and the iron content is high.
The current research on the tremella polysaccharide-iron complex generated by complexing liquid fermented tremella polysaccharide with iron ions is not reported yet.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the tremella polysaccharide iron (III) compound is prepared by fermenting tremella polysaccharide with good activity and iron (III) and is convenient to use in functional food, medicine and health care products, and the compound has good complexation and high iron content.
In order to solve the technical problems, the invention provides the following technical scheme:
a preparation method of a tremella polysaccharide iron (III) compound comprises the following steps:
step 1): dissolving sodium citrate and tremella polysaccharide in deionized water, and stirring in a water bath at 50-80 ℃ to dissolve the sodium citrate and the tremella polysaccharide to form a mixed solution;
step 2): adding an iron chloride solution and a sodium hydroxide solution into the mixed solution until the pH value of the mixed solution is 8.0-8.5 to form a reaction solution until insoluble substances appear in the reaction solution; and (3) continuing heating in a water bath at 50-80 ℃, stirring, stopping stirring, and separating and purifying insoluble substances to obtain the tremella polysaccharide iron (III) compound.
Preferably, the ratio of the sodium citrate to the tremella polysaccharide to the deionized water in the step 2) is 1 g: 2 g: 100 mL.
Preferably, the concentration of the ferric trichloride solution in the step 2) is 2mol/L, and the mass fraction of sodium hydroxide in the sodium hydroxide solution is 20%.
Preferably, the separation and purification treatment in step 2) specifically comprises: centrifuging the reaction solution, and collecting a supernatant; adding ethanol into the supernatant, precipitating with ethanol, standing overnight, collecting precipitate, washing with anhydrous ethanol, diethyl ether and acetone, centrifuging, collecting precipitate, and vacuum drying to obtain Tremella polysaccharide iron (III) complex.
More preferably, the rotating speed of the centrifugation is 8000r/min and the time is 15 min.
More preferably, the ethanol is 95% by volume and is added in an amount of 2 times the volume of the supernatant.
More preferably, the vacuum drying conditions are-45 ℃ and 15.65 MPa.
Preferably, the tremella polysaccharide is extracted from tremella spore fermentation broth.
The invention also provides the tremella polysaccharide iron (III) compound prepared by the preparation method of the tremella polysaccharide iron (III) compound.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention adopts the polysaccharide extracted from the tremella spore fermentation liquor, has low raw material cost and stable quality, and almost has no toxic or side effect.
(2) The tremella polysaccharide and iron (III) have good complexing ability, and the polysaccharide iron (III) compound belongs to one of organic iron, and has better activity and lower side effect than inorganic iron.
(3) The preparation method disclosed by the invention is simple and easy to operate, high in experimental safety, easy for mass preparation and high in efficiency.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below.
The method for measuring the content of iron in the tremella polysaccharide iron (III) adopts a 1, 10-phenanthroline method, and comprises the following steps:
a. and (3) preparing a standard curve: taking 7 50mL measuring bottles, respectively adding 0.00mL, 1.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL and 10.00mL of standard iron use solution (10 mu g/mL), and respectively adding 1mL of hydroxylamine hydrochloride solution with mass concentration of 10%, 2.5mL of 1, 10-phenanthroline color developing solution and sodium acetate solution (1 mol. L)-1) Diluting the solution to a scale with distilled water by 5mL, shaking up, standing for 10-15 min, taking the reagent solution as a blank at 510nm, and measuring the absorbance by using an ultraviolet-visible spectrophotometer. A standard curve was prepared with the iron concentration (C) as the abscissa and the absorbance (A) as the ordinate. The standard curve equation is: 0.2114C-0.0035 and 0.9902 in terms of A, C and R2, wherein A is an absorbance value, C is a standard iron solution concentration (ul/mL), and R is2Is a correlation coefficient;
b. and (3) determining the iron content of the tremella polysaccharide iron: 10mg of dried tremella polysaccharide iron complex is accurately weighed and dispersed in 20mL of 1M HCl for 24h to break the complex, so that released iron can be dissolved. 1mL of the sample was added with 10% hydroxylamine hydrochloride by mass, 2.5mL of 10% 1, 10-phenanthroline by mass, and 5mL of sodium acetate trihydrate buffer (pH4.5), and after standing for 30 minutes, the absorbance value A was measured with an ultraviolet spectrophotometer at λ 510 nm. Calculating the iron content in the tremella polysaccharide-iron complex according to the standard curve;
the invention carries out the property determination of the tremella polysaccharide iron (III) solution, and the steps are as follows:
dispersing 10mg of dry tremella polysaccharide iron complex in 2mL of H respectively2O and 2mL of 1M HCl. The mixture was stirred at room temperature for 2h, and potassium ferrocyanide (K) was added dropwise to the tube4[Fe(CN)6]·3H2O), the solution was observed for changes in appearance, resulting in a dark blue precipitate.
Example 1
A preparation method of a tremella polysaccharide-iron compound comprises the following specific steps:
step 1, dissolving sodium citrate and tremella polysaccharide in deionized water, and uniformly stirring to form a mixed solution. Stirring in water bath at 50 deg.C to dissolve;
step 2, adding a ferric chloride solution and a sodium hydroxide solution into the mixed solution until the pH value of the mixed solution is 8.0 to form a reaction solution;
and 3, continuing heating in a water bath until the reaction solution generates reddish brown insoluble substances, stirring for about 1h, and separating and purifying the mixture after stopping stirring to obtain the tremella polysaccharide-iron complex.
The preparation method of the tremella polysaccharide-iron complex comprises the following steps of, by mass, 1: 2, the deionized water is 100 mL.
The preparation method of the tremella polysaccharide-iron complex comprises the step of preparing a ferric trichloride solution, wherein the concentration of the ferric trichloride solution is 2 mol/L.
The preparation method of the tremella polysaccharide-iron complex comprises the step of preparing a sodium hydroxide solution, wherein the mass fraction of sodium hydroxide in the sodium hydroxide solution is 20%.
The preparation method of the tremella polysaccharide-iron complex is characterized in that the reaction temperature and the environment are 50 ℃ water bath environment.
The preparation method of the tremella polysaccharide-iron complex comprises the following steps of separating and purifying the mixture to obtain the tremella polysaccharide-iron complex: centrifuging the mixture at 8000r/min for 15min, and collecting supernatant; adding 2 times volume of 95 vol% ethanol into the supernatant, precipitating with ethanol, standing overnight, collecting precipitate, washing with anhydrous ethanol, diethyl ether and acetone, centrifuging at 8000r/min for 15min, collecting precipitate, and vacuum drying to obtain fermented Tremella polysaccharide-iron complex.
The preparation method of the tremella polysaccharide-iron complex comprises the step of drying the tremella polysaccharide-iron complex under vacuum at-45 ℃ and 15.65 MPa.
The tremella polysaccharide is extracted from tremella spore fermentation liquor.
The content of the iron element in the obtained tremella polysaccharide iron (III) is 22.97%.
The property measurement shows that the appearance of the aqueous solution is not changed, and the potassium ferrocyanide is added into the tremella polysaccharide iron complex in the hydrochloric acid solution, so that dark blue precipitation appears. The tremella polysaccharide-iron complex is shown to contain no free iron ions, and the polysaccharide and the iron are combined together through a bond, rather than being simply physically mixed together.
Example 2
A method of preparing a tremella polysaccharide-iron complex, similar to example 1, except that:
in the step 1, the sodium citrate and the tremella polysaccharide are dissolved in deionized water to form a mixed solution. The mixture was stirred in a water bath at 60 ℃ to dissolve the mixture.
The content of the iron element in the obtained tremella polysaccharide iron (III) is 21.74%.
The property measurement shows that the appearance of the aqueous solution is not changed, and the potassium ferrocyanide is added into the tremella polysaccharide iron complex in the hydrochloric acid solution, so that dark blue precipitation appears. The tremella polysaccharide-iron complex is shown to contain no free iron ions, and the polysaccharide and the iron are combined together through a bond, rather than being simply physically mixed together.
Example 3
A method of preparing a tremella polysaccharide-iron complex, similar to example 1, except that:
in the step 1, the sodium citrate and the tremella polysaccharide are dissolved in deionized water to form a mixed solution. The mixture was stirred in a water bath at 70 ℃ to dissolve the mixture.
And 2, adding an iron chloride solution and a sodium hydroxide solution into the mixed solution until the pH value of the mixed solution is 8.3 to form a reaction solution.
The content of the iron element in the obtained tremella polysaccharide iron (III) is 18.62%.
The property measurement shows that the appearance of the aqueous solution is not changed, and the potassium ferrocyanide is added into the tremella polysaccharide iron complex in the hydrochloric acid solution, so that dark blue precipitation appears. The tremella polysaccharide-iron complex is shown to contain no free iron ions, and the polysaccharide and the iron are combined together through a bond, rather than being simply physically mixed together.
Example 4
A method of preparing a tremella polysaccharide-iron complex, similar to example 1, except that:
in the step 1, the sodium citrate and the tremella polysaccharide are dissolved in deionized water to form a mixed solution. The mixture was stirred in a water bath at 80 ℃ to dissolve the mixture.
The content of the iron element in the obtained tremella polysaccharide iron (III) is 20.07 percent.
The property measurement shows that the appearance of the aqueous solution is not changed, and the potassium ferrocyanide is added into the tremella polysaccharide iron complex in the hydrochloric acid solution, so that dark blue precipitation appears. The tremella polysaccharide-iron complex is shown to contain no free iron ions, and the polysaccharide and the iron are combined together through a bond, rather than being simply physically mixed together.
Claims (9)
1. A preparation method of a tremella polysaccharide iron (III) compound is characterized by comprising the following steps:
step 1): dissolving sodium citrate and tremella polysaccharide in deionized water, and stirring in a water bath at 50-80 ℃ to dissolve the sodium citrate and the tremella polysaccharide to form a mixed solution;
step 2): adding an iron chloride solution and a sodium hydroxide solution into the mixed solution until the pH value of the mixed solution is 8.0-8.5 to form a reaction solution until insoluble substances appear in the reaction solution; and (3) continuing heating in a water bath at 50-80 ℃, stirring, stopping stirring, and separating and purifying insoluble substances to obtain the tremella polysaccharide iron (III) compound.
2. The method for preparing the iron (iii) tremella polysaccharide complex as claimed in claim 1, wherein the ratio of sodium citrate, tremella polysaccharide and deionized water in step 2) is 1 g: 2 g: 100 mL.
3. The method for preparing the tremella polysaccharide iron (III) complex as claimed in claim 1, wherein the concentration of the ferric trichloride solution in step 2) is 2mol/L, and the mass fraction of sodium hydroxide in the sodium hydroxide solution is 20%.
4. The method for preparing the tremella polysaccharide iron (iii) complex as claimed in claim 1, wherein the separation and purification process in step 2) is specifically: centrifuging the reaction solution, and collecting a supernatant; adding ethanol into the supernatant, precipitating with ethanol, standing overnight, collecting precipitate, washing with anhydrous ethanol, diethyl ether and acetone, centrifuging, collecting precipitate, and vacuum drying to obtain Tremella polysaccharide iron (III) complex.
5. The method for preparing the iron (III) complex tremella polysaccharide according to claim 4, wherein the rotation speed of the centrifugation is 8000r/min and the time is 15 min.
6. The method for preparing the iron (III) complex tremella polysaccharide according to claim 4, wherein the ethanol is added in a concentration of 95 vol% and in an amount of 2 times the volume of the supernatant.
7. The method for preparing the iron (III) complex tremella polysaccharide as claimed in claim 4, wherein the vacuum drying condition is-45 ℃ and 15.65 MPa.
8. The method for preparing the iron (III) complex tremella polysaccharide according to any one of claims 1 to 7, wherein the tremella polysaccharide is extracted from tremella spore fermentation broth.
9. The iron (III) tremella polysaccharide complex obtained by the method of any one of claims 1 to 8.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115819638A (en) * | 2022-12-28 | 2023-03-21 | 广东药科大学 | Preparation method of tremella polysaccharides with different molecular weights |
| CN116041559A (en) * | 2022-09-28 | 2023-05-02 | 广州大学 | Auricularia polytricha polysaccharide-iron compound with enhanced oxidation resistance and preparation method thereof |
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| CN108914580A (en) * | 2018-05-31 | 2018-11-30 | 佛山市陵谐环保科技有限公司 | A kind of preparation method of functionalization skin care fiber |
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| CN108914580A (en) * | 2018-05-31 | 2018-11-30 | 佛山市陵谐环保科技有限公司 | A kind of preparation method of functionalization skin care fiber |
Non-Patent Citations (2)
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| 余华等: "通江银耳多糖和胶质成分及其铁复合物的合成", 《成都大学学报(自然科学版)》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116041559A (en) * | 2022-09-28 | 2023-05-02 | 广州大学 | Auricularia polytricha polysaccharide-iron compound with enhanced oxidation resistance and preparation method thereof |
| CN115819638A (en) * | 2022-12-28 | 2023-03-21 | 广东药科大学 | Preparation method of tremella polysaccharides with different molecular weights |
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