CN100362021C - Chinese yam polysaccharide-iron complex and its preparation process - Google Patents

Abstract

A yam polysaccharide and ferrum compound and a preparation process thereof belong to polysaccharide compound technology field. The yam polysaccharide and water-solubility citrate salt or tartrate are selected to dissolve in distilled water, then the water solution is heated and mixed and added with two-valence ferrum or three valence ferrum compound water solution, and then reacted for 0.5-2 hours; the reaction liquid is then cooled, and added with ethanol and is deposited, washed to obtain yam polysaccharide-ferrum compound; the mass ratio of the yam polysaccharide, water-solubility citrate salt or tartrate, two-valence ferrum or three valence ferrum compound is 1.5-8.5:3-6:3-10.5. In the obtained compound, the mass contents of the ferrum and yam polysaccharide are respectively between 20-40% and 10-50%. The solvabilities of the yam polysaccharide-two valence ferrum compound and the yam polysaccharide-three valence ferrum compound in 100 mL water under 25 DEG C are respectively 6-7 g and 10-12 g. The inventive product has excellent dissolving out property and stability, has neutral water solution and can replace the existing ferrum replenishing agent to replenish ferrum for human body.

Description

Chinese yam polysaccharide-iron complex and its preparation process

technical field

The invention belongs to the technical field of polysaccharide complexes, in particular to a yam polysaccharide-iron complex and a preparation process thereof.

Background technique

Polysaccharides are natural macromolecular substances from higher plants, animals, and microbial cells. They are high molecular polymers formed in biological life activities and are important components of living organisms. They become the most important three biological macromolecules together with proteins and nucleic acids. molecular. Polysaccharides have large molecular weight, high polarity, complex structure, and are not easy to form crystals, so there are great difficulties in separation, purification and structure identification. Studies by scholars at home and abroad have shown that polysaccharides can not only treat cancers where the body's immune system is severely damaged, but also treat a variety of immune deficiency diseases. As a drug, more importantly, it has minimal cytotoxicity. When treating tumors, it does not directly kill the growing tumor cells like ordinary chemotherapy drugs, but promotes cellular and humoral immune responses to inhibit and eliminate tumor cells, and has little effect on normal cells.

my country is rich in yam resources. Only Wuzhi, Wenxian, and Qinyang in Jiaozuo, Henan Province (formerly Huaiqing Prefecture, where the yam produced by Dioscorea opposita Thunb) produces more than one million tons of yam per year. At present, yam from the place of origin is still processed by traditional methods, and the process is complicated and labor-intensive. And the processing process must be fumigated with sulfur to sterilize and bleach, which may lead to excessive sulfur residues or produce harmful sulfides.

Contents of the invention

The object of the present invention is to provide a yam polysaccharide-iron complex and a preparation process thereof.

In order to achieve the above purpose, the present invention adopts the following technical scheme: yam polysaccharide-iron complex, wherein the mass content of iron is 20-40%, and the content of yam polysaccharide is between 10-50%.

It is a yam polysaccharide-ferrous iron complex with a solubility of 6-7 grams in 100 milliliters of water at 25°C.

It is a yam polysaccharide-ferric iron complex with a solubility of 10-12 grams in 100 milliliters of water at 25°C.

The preparation process of yam polysaccharide-iron complex is to dissolve yam polysaccharide and water-soluble citrate or tartrate in distilled water, add the aqueous solution of divalent iron or ferric iron compound dropwise under heating and stirring in a water bath, and then react after the dropwise addition 0.5-2 hours; cooling, adding ethanol to the reaction solution for alcohol precipitation and washing to obtain the yam polysaccharide-iron complex; the mass ratio of yam polysaccharide to water-soluble citrate or tartrate, divalent iron or ferric iron compound is 1.5-8.5: 3-6: 3-10.5.

The citrate is trisodium citrate or tripotassium citrate, the tartrate is sodium tartrate or potassium tartrate, and the iron compound is ferric chloride or ammonium ferrous sulfate.

Citrate is trisodium citrate and tartrate is sodium tartrate.

The polysaccharide concentration is 1-5g/250ml, the trisodium citrate concentration is 0.1-0.3mol/l, the ferric chloride concentration is 0.2-0.6mol/l, and the pH of the reaction solution is 7-8.

The polysaccharide concentration is 1-5g/250ml, the sodium tartrate concentration is 0.1-0.3mol/l, the ferrous ammonium sulfate concentration is 0.2-0.6mol/l, and the pH of the reaction solution is 7-8.

The filter residue obtained by alcohol precipitation is washed successively with 95% ethanol, absolute ethanol, acetone and ether, and vacuum-dried or freeze-dried to obtain a powdery yam polysaccharide-iron complex.

The present invention utilizes yam with abundant resources for the first time, and reacts yam polysaccharide from yam with divalent iron or ferric iron water-soluble salt to prepare yam polysaccharide-iron complex (complex). The mass content of iron is between 20-40% and the mass content of polysaccharide is between 10-50% as measured by atomic absorption, o-phenanthroline spectrophotometry and sulfuric acid phenol color spectrophotometry. At 25°C, the solubility of the yam polysaccharide-ferrous iron complex in 100 milliliters of water is 6-7 grams, and the solubility of the yam polysaccharide-ferric iron complex in 100 milliliters of water is 10-12 grams. The dissolution performance and stability of yam polysaccharide-iron complex are good, and its aqueous solution is neutral, which is close to the pH value of human body fluid. It can replace the existing iron supplements (ferrous sulfate, ferrous succinate, ferrous gluconate, etc.) to supplement iron to the human body, and can avoid the gastrointestinal stimulating side effects of the existing iron supplements on the human body. During the reaction, iron ions and citrate ions form a complex iron citrate, and under alkaline conditions, ferric citrate is converted into citrate polymeric iron, and yam polysaccharide interacts with polymeric iron on the surface of the polymeric iron core with its sugar chains. Generate a stable yam polysaccharide-citric acid-polymeric iron complex, that is, yam polysaccharide-iron complex. In the preparation process of the present invention, the raw materials are easy to obtain, the process steps are few, and the three wastes are not generated.

Detailed ways

Embodiment 1, yam polysaccharide-iron complex preparation process, get yam polysaccharide aqueous solution (3.0012g/250ml) 14ml, trisodium citrate aqueous solution (0.1388mol/l) 5ml, add FeCl dropwise at 1ml/min _Aqueous solution (0.4382 mol/l) 5ml, adjust the pH of the reaction solution between 7-8 with NaOH aqueous solution (3mol/l), react under heating in a water bath at 70°C for 1 hour, cool, and centrifuge. Add 4 times the amount (volume) of 95% ethanol to the supernatant, let it stand in the refrigerator, filter, and wash the filter residue with 95% ethanol, absolute ethanol, acetone, and anhydrous ether successively, and vacuum-dry to obtain a brown-red powder, which is yam polysaccharide - Ferric complex. The mass content of the yam polysaccharide is 48.3%, the mass content of ferric iron is 21.8%, and the solubility of the compound in 100 ml of water at 25°C is 10.8 grams.

Embodiment 2, in the present embodiment, yam polysaccharide aqueous solution (1.9586g/250ml) consumption 20ml, trisodium citrate replace with sodium tartrate, sodium tartrate aqueous solution (0.1392mol/l) consumption 5ml, FeCl _aqueous solution (0.5477mol/l ) consumption 4ml, other with embodiment 1. The obtained yam polysaccharide-ferric iron complex has a mass content of yam polysaccharide of 46.2%, a mass content of ferric iron of 32.1%, and the solubility of the compound in 100 ml of water at 25° C. is 11.2 grams.

Embodiment 3, in the present embodiment, yam polysaccharide aqueous solution (1.9586g/250ml) consumption 20ml, trisodium citrate replace with sodium tartrate, sodium tartrate aqueous solution (0.1392mol/l) consumption 5ml, FeCl _aqueous solution (0.5477mol/l ) in an amount of 4ml, the pH of the solution was adjusted to 7-8 with an aqueous solution of sodium carbonate, the reaction temperature was 90° C., and the reaction time was 2 hours. Others are the same as embodiment 1. The obtained yam polysaccharide-ferric iron compound has a mass content of 37.2% of yam polysaccharide and 20.7% of ferric iron, and the solubility of the compound in 100 ml of water at 25°C is 11.4 grams.

Example 4. In this example, the dosage of yam polysaccharide aqueous solution (1.9586g/250ml) is 20ml, the dosage of trisodium citrate aqueous solution (0.1392mol/l) is 5ml, and the aqueous solution of FeCl ₃ uses (NH ₄ ) ₂ Fe(SO ₄ ) ₂ Aqueous solution replacement, (NH ₄ ) ₂ Fe(SO ₄ ) ₂ aqueous solution (0.5033mol/l) dosage 10ml, solution pH adjusted to 7-8 with NaOH aqueous solution, reaction temperature 80°C, reaction time 2 hours. Others are the same as embodiment 1. In the obtained yam polysaccharide-ferrous iron complex, the mass content of the yam polysaccharide is 18.6%, the mass content of the ferrous iron is 23.6%, and the solubility of the compound in 100 ml of water at a temperature of 25°C is 6.6 grams.

Claims (5)

1. Chinese yam polysaccharide-iron complexes is characterized in that, wherein the mass content of iron is 20-40%, and Chinese yam polysaccharide content is between 10-50%; Wherein 25 ℃ of Chinese yam polysaccharide-iron (III) mixtures solubleness in water is per 100 ml water 10-12 gram; 25 ℃ of Chinese yam polysaccharide-iron (II) mixtures solubleness in water is per 100 ml water 6-7 gram.

2. the preparation technology of the described Chinese yam polysaccharide-iron complexes of claim 1, it is characterized in that, getting Chinese yam polysaccharide and water-soluble citrate or tartrate is dissolved in the distilled water, heating in water bath, stirring drip the aqueous solution of ferrous iron or ferric compound down, dropwise, continue reaction 0.5-2 hour; Cooling adds ethanol alcohol precipitation, washing in the reaction solution, get Chinese yam polysaccharide-iron complexes; Chinese yam polysaccharide and water-soluble citrate or tartrate, ferrous iron or ferric mass ratio are 1.5-8.5: 3-6: 3-10.5.

3. preparation technology as claimed in claim 2 is characterized in that, Citrate trianion is trisodium citrate or citric acid tri potassium, and tartrate is sodium tartrate or soluble tartrate, and the compound of iron is iron(ic) chloride or ferrous ammonium sulphate.

4. preparation technology as claimed in claim 3 is characterized in that, polysaccharide concentration is 1-5g/250ml, the concentration of trisodium citrate is 0.1-0.3mol/l, the concentration of iron(ic) chloride is 0.2-0.6mol/l, and the concentration of ferrous ammonium sulphate is 0.2-0.6mol/l, reaction solution pH=7-8.

5. as claim 2,3 or 4 described preparation technologies, it is characterized in that alcohol precipitation gained filter residue with 95% ethanol, dehydrated alcohol, acetone, ether washing, gets powdery Chinese yam polysaccharide-iron complexes through vacuum-drying or lyophilize successively.