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CN100362021C - Chinese yam polysaccharide and ferrum compound and preparation process - Google Patents

Chinese yam polysaccharide and ferrum compound and preparation process Download PDF

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Publication number
CN100362021C
CN100362021C CNB031592910A CN03159291A CN100362021C CN 100362021 C CN100362021 C CN 100362021C CN B031592910 A CNB031592910 A CN B031592910A CN 03159291 A CN03159291 A CN 03159291A CN 100362021 C CN100362021 C CN 100362021C
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China
Prior art keywords
chinese yam
yam polysaccharide
iron
water
polysaccharide
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CNB031592910A
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Chinese (zh)
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CN1572802A (en
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刘绣华
李明静
赵东保
姜芳婷
宋爱新
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Bao Tong (Jiaozuo) Pharmaceutical Co., Ltd.
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Henan University
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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 complexes and preparation technology thereof
Technical field
The invention belongs to the polysaccharide compound technical field, particularly a kind of Chinese yam polysaccharide-iron complexes and preparation technology thereof.
Background technology
Polysaccharide is from the natural macromolecular material in higher plant, animal, the microorganism cells, it is the high molecular polymer that forms in the biological vital movement, be the important component part of Living organism, with protein, nucleic acid and become most important three kinds of biomacromolecules.Polysaccharide molecular weight is big, polarity is big, complex structure, be difficult for to form crystallization, has very big difficulty aspect separation and purification and structure evaluation.Chinese scholars studies show that polysaccharide not only can be treated the cancer that body immune system is subjected to major injury, can treat the damaged disease of panimmunity again.As medicine, the more important thing is that its cytotoxicity is minimum.During tumour, it directly kills the tumour cell of growing unlike general chemotherapeutics in treatment, thereby but promote cell and humoral immune reaction to reach to suppress and the effect of elimination tumour cell, very little to normal impact cell.
China's Chinese yam aboundresources, only the Wuzhi of Henan Province's JIAOZUO AREA, Wen County, Qinyang (celebrating mansion, old genus bosom, the rapid-result RHIIZOMA DIOSCOREAE frOm Henan of China Dioscorea of the institute Chinese yam that produces opposita Thunb) annual output Chinese yam is healed 1,000,000 tons.Place of production Chinese yam still adopts traditional method to concoct process complexity, labor intensive at present.And concocting process will be bleached with sterilization with sulfur fumigation, may cause sulphur residual too high or produce harmful sulfide.
Summary of the invention
The object of the invention is to provide a kind of Chinese yam polysaccharide-iron complexes and preparation technology thereof.
For reaching above-mentioned purpose, the present invention adopts following technical scheme: Chinese yam polysaccharide-iron complexes, and wherein the mass content of iron is 20-40%, Chinese yam polysaccharide content is between 10-50%.
It is Chinese yam polysaccharide-ferrous iron mixture, 25 ℃ in 100 ml waters solubleness be 6-7 gram.
It is Chinese yam polysaccharide-ferric iron mixture, 25 ℃ in 100 ml waters solubleness be 10-12 gram.
Chinese yam polysaccharide-iron complexes preparation technology is got Chinese yam polysaccharide and water-soluble citrate or tartrate and is dissolved in the distilled water, and heating in water bath, stirring drip the aqueous solution of ferrous iron or ferric compound down, dropwise and react 0.5-2 hour again; Cooling adds ethanol alcohol precipitation, washing in the reaction solution, get Chinese yam polysaccharide-iron complexes; The mass ratio of Chinese yam polysaccharide and water-soluble citrate or tartrate, ferrous iron or ferric compound is 1.5-8.5: 3-6: 3-10.5.
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.
Citrate trianion is a trisodium citrate, and tartrate is a sodium tartrate.
Polysaccharide concentration is 1-5g/250ml, and trisodium citrate concentration is 0.1-0.3mol/l, and the concentration of iron(ic) chloride is 0.2-0.6mol/l, reaction solution PH=7-8.
Polysaccharide concentration is 1-5g/250ml, and sodium tartrate concentration is 0.1-0.3mol/l, and the concentration of ferrous ammonium sulphate is 0.2-0.6mol/l, reaction solution PH=7-8.
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.
The present invention utilizes resourceful Chinese yam first, from the Chinese yam polysaccharide in the Chinese yam and ferrous iron or the reaction of ferric water-soluble salt, makes Chinese yam polysaccharide-iron complexes (complex compound).Utilize mass content that atomic absorption, phenanthroline spectrophotometry and sulfuric acid phenol colour developing spectrophotometry goes out iron wherein between 20-40%, the mass content of polysaccharide is between 10-50%.Under 25 ℃ of temperature, the Chinese yam polysaccharide-solubleness of ferrous iron mixture in 100 ml waters is the 6-7 gram, and the Chinese yam polysaccharide-solubleness of ferric iron mixture in 100 ml waters is the 10-12 gram.Chinese yam polysaccharide-iron complexes dissolving out capability and stability better, and its aqueous solution is neutral, near the human body fluid pH value.Alternative existing benefit chalybeate (ferrous sulfate, the acid of coral amber are ferrous, Ferrous Gluconate etc.) to compensating iron for human, can avoid using existing stimulation side effect of mending chalybeate to the human intestines and stomach.In the reaction process, iron ion and citrate ion form the complex compound ironic citrate, ironic citrate is converted into citric acid polymerization iron under alkaline condition, Chinese yam polysaccharide is with the surperficial and polymerization iron phase mutual effect at polymerization iron nuclear of its sugar chain, generate stable Chinese yam polysaccharide-citric acid-polymerization iron complexes, i.e. Chinese yam polysaccharide-iron complexes.Preparation technology among the present invention, raw material is easy to get, and processing step is few, and the no three wastes produce.
Embodiment
Embodiment 1, Chinese yam polysaccharide-iron complexes preparation technology are got the Chinese yam polysaccharide aqueous solution (3.0012g/250ml) 14ml, trisodium citrate aqueous solution (0.1388mol/l) 5ml, press 1ml/ minute speed and drip FeCl 3The aqueous solution (0.4382mol/l) 5ml adjusts between the reaction solution PH=7-8 with the NaOH aqueous solution (3mol/l), and 70 ℃ of heating in water bath reacted 1 hour down, cooling, centrifugation.Add 95% ethanol of 4 times of amounts (volume) in the supernatant liquor, leave standstill in the refrigerator, filter, with 95% ethanol, dehydrated alcohol, acetone, anhydrous diethyl ether washing, it is Chinese yam polysaccharide-ferric iron mixture that vacuum-drying gets the red-brown powder to filter residue successively.Wherein the Chinese yam polysaccharide mass content 48.3%, and ferric iron mass content 21.8%, the solubleness under 25 ℃ of temperature of mixture in 100 ml waters are 10.8 grams.
In embodiment 2, the present embodiment, the Chinese yam polysaccharide aqueous solution (1.9586g/250ml) consumption 20ml, trisodium citrate substitute the sodium tartrate aqueous solution (0.1392mol/l) consumption 5ml, FeCl with sodium tartrate 3The aqueous solution (0.5477mol/l) consumption 4ml, other are with embodiment 1.Chinese yam polysaccharide mass content 46.2% in gained Chinese yam polysaccharide-ferric iron mixture, ferric iron mass content 32.1%, the solubleness under 25 ℃ of temperature of mixture in 100 ml waters are 11.2 grams.
In embodiment 3, the present embodiment, the Chinese yam polysaccharide aqueous solution (1.9586g/250ml) consumption 20ml, trisodium citrate substitute the sodium tartrate aqueous solution (0.1392mol/l) consumption 5ml, FeCl with sodium tartrate 3The aqueous solution (0.5477mol/l) consumption 4ml, solution PH is adjusted to 7-8 with aqueous sodium carbonate, 90 ℃ of temperature of reaction, 2 hours reaction times.Other are with embodiment 1.Chinese yam polysaccharide mass content 37.2% in gained Chinese yam polysaccharide-ferric iron mixture, ferric iron mass content 20.7%, the solubleness under 25 ℃ of temperature of mixture in 100 ml waters are 11.4 grams.
In embodiment 4, the present embodiment, the Chinese yam polysaccharide aqueous solution (1.9586g/250ml) consumption 20ml, trisodium citrate aqueous solution (0.1392mol/l) consumption 5ml, FeCl 3The aqueous solution (NH 4) 2Fe (SO 4) 2The aqueous solution substitutes, (NH 4) 2Fe (SO 4) 2The aqueous solution (0.5033mol/l) consumption 10ml, pH value of solution is adjusted to 7-8 with the NaOH aqueous solution, 80 ℃ of temperature of reaction, 2 hours reaction times.Other are with embodiment 1.Chinese yam polysaccharide mass content 18.6% in gained Chinese yam polysaccharide-ferrous iron mixture, ferrous iron mass content 23.6%, the solubleness under 25 ℃ of temperature of mixture in 100 ml waters are 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.
CNB031592910A 2003-06-06 2003-09-16 Chinese yam polysaccharide and ferrum compound and preparation process Expired - Fee Related CN100362021C (en)

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CN101328222B (en) * 2007-06-20 2011-05-18 赵玉英 Liquorice polyose metal complexes and preparation thereof
CN107417802B (en) * 2017-07-12 2019-06-28 河南大学 A kind of preparation method and applications of the Chinese yam polysaccharide Zn complex with hypoglycemic effect
CN107325198A (en) * 2017-07-27 2017-11-07 福建农林大学 A kind of preparation method and applications of Chinese yam polysaccharide chromic compound
CN110212192A (en) * 2019-06-25 2019-09-06 河南大学 A kind of adjustable nano ferriferrous oxide composite material and preparation method of cladding carbon layers having thicknesses and application
CN111567717A (en) * 2020-05-27 2020-08-25 河南大学 Chinese yam mucilage-nano zinc oxide solution and preparation method and application thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1308520A2 (en) * 2001-11-01 2003-05-07 MicroBioSystems Limited Partnership Taxonomic identification of pathogenic micro-organisms and their toxic proteins

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1308520A2 (en) * 2001-11-01 2003-05-07 MicroBioSystems Limited Partnership Taxonomic identification of pathogenic micro-organisms and their toxic proteins

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
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山药水溶性多糖的化学及体外抗氧化活性. 何书英,詹彤,王淑如.中国药科大学学报,第25卷第6期. 1994 *

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