CN102167752B - Preparation method of water-soluble soybean polysaccharide ferrous coordination compound - Google Patents
Preparation method of water-soluble soybean polysaccharide ferrous coordination compound Download PDFInfo
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- CN102167752B CN102167752B CN2011101325045A CN201110132504A CN102167752B CN 102167752 B CN102167752 B CN 102167752B CN 2011101325045 A CN2011101325045 A CN 2011101325045A CN 201110132504 A CN201110132504 A CN 201110132504A CN 102167752 B CN102167752 B CN 102167752B
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- iron
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Abstract
The invention discloses a preparation method of a water-soluble soybean polysaccharide ferrous coordination compound, belonging to the technical field of a polysaccharide coordination compound. The preparation method comprises the steps of dissolving water-soluble soybean polysaccharide and a catalytic agent; putting the water-soluble soybean polysaccharide and the catalytic agent into water bath under 40-90DEG C; dropwise adding ferrous sulfate solution during stirring; simultaneously dropwise adding hydrochloric acid solution or sodium acetate solution; keeping the PH value of reaction solution at 2-5; continuously reaction for 0.5-3h during stirring after dropwise adding the ferrous sulfate; performing the alcohol deposition to the reaction solution after cooling; centrifugally separating; and washing and drying obtained precipitate to obtain the water-soluble soybean polysaccharide ferrous coordination compound. The water-soluble soybean polysaccharide ferrous coordination compound is flaxen powder, the iron content is 10-30%, ferrous iron is hard to oxidize, the bioavailability is high, the source of raw materials is easy to obtain, and the price is low, so that the compound can be developed into an iron-strengthened food additive and a nutritional type oral iron supplement agent.
Description
Technical field
The invention belongs to the polysaccharide complex technical field, the preparation method of the ferrous title complex of particularly a kind of water soluble soybean polysaccharide.
Background technology
Soybean polysaccharide is from the resulting water-soluble polysaccharides material of pulse family soybean cotyledon part.Because it is cheap and easy to get, and has many superior physiological functions and food function characteristic, has been widely used in each field of food.
Iron is one of trace element essential in the human body, is the core of oxyphorase and myohaemoglobin, and many in the cell have the enzyme of critical function also all to contain iron, is indispensable material in the many normal physiological processes of human body.Sideropenia can cause multiple disease, and iron-deficiency anaemia has become one of modal disease in the world, and human beings'health in serious threat, how to prevent and treat iron-deficiency anaemia more and more to receive people's attention.The research of existing many Polyferose title complexs both at home and abroad is like the benefit chalybeate niferex that has gone on the market, Iron-Dextrin Complex, Lalgine iron, angelica polysaccharide iron, Dihuang polysaccharide iron, GPS's iron etc.; Research shows that Polyferose class title complex not only can be avoided GI irritation, and it is little also to have a spinoff; Solubleness is good, the iron-holder advantages of higher, and the part polysaccharide of vegetable polysaccharides iron complex has other multiple efficacies concurrently; After the vegetable polysaccharides iron complex discharges in vivo, not only can mend iron, can also bring into play the effect of part; Body is played double protection, is a kind of up-and-coming benefit chalybeate.
After polysaccharide and ferric iron form title complex; The iron of this form must separate with organic moiety; And just can be absorbed after being reduced into ferrous iron, thereby, research water soluble soybean polysaccharide and ferrous title complex; Be expected to be developed to the foodstuff additive and the oral benefit chalybeate of nutritional type of reinforced iron, improve its bioavailability.
Summary of the invention
The object of the invention is to overcome the shortcoming of prior art; The preparation method of the ferrous title complex of a kind of water soluble soybean polysaccharide is provided, and its iron-holder is high, ferrously is difficult for oxidation; Bioavailability is high; Raw material sources are easy to get, and are cheap, are expected to be developed to the foodstuff additive and the oral benefit chalybeate of nutritional type of reinforced iron.
For reaching above-mentioned purpose, the present invention adopts following technical scheme:
(1) with after water soluble soybean polysaccharide and the catalyst dissolution, place 40 ~ 90 ℃ of water-baths, stir and drip copperas solution down, while dripping hydrochloric acid or sodium acetate soln, keeping the pH of reaction solution is 2 ~ 5, drips the continued stirring reaction 0.5 ~ 3 hour;
(2) reaction solution cooling back alcohol is analysed, spinning, and the gained deposition gets the ferrous title complex of water soluble soybean polysaccharide after washing, drying;
Said catalyzer is Citrate trianion or tartrate.
Said Citrate trianion is trisodium citrate or citric acid tri potassium, and said tartrate is sodium tartrate or soluble tartrate.
The mass ratio of said water soluble soybean polysaccharide and catalyzer is 0.25:1 ~ 5:1.
It is in reaction solution, to add absolute ethyl alcohol that said alcohol is analysed, and separates out deposition.
Said washing is alcohol to be analysed the gained deposition wash with 95 % ethanol, absolute ethyl alcohol and anhydrous propanone successively.
Said drying is warm air drying, vacuum-drying, lyophilize or spraying drying.
The rate of addition of adjustment hydrochloric acid or sodium acetate soln, keeping the pH of reaction solution is 2 ~ 5, and the present invention does not limit the dripping quantity of ferrous sulfate, and preferred ferrous ion and water soluble soybean polysaccharide mass ratio are 1:1.
The present invention is with respect to advantage and beneficial effect that prior art had.
(1) the present invention utilizes water soluble soybean polysaccharide and ferrous sulfate in the bean dregs to prepare the ferrous title complex of water soluble soybean polysaccharide first.
(2) the ferrous title complex of water soluble soybean polysaccharide utilizes the phenanthroline spectrophotometry to measure its iron-holder at 10 ~ 30 %, and iron-holder is high, and is safer and more effective as the foodstuff additive and the oral benefit chalybeate of nutritional type of reinforced iron.The solution of the ferrous title complex of water soluble soybean polysaccharide is placed one day ferrous iron and can be oxidized to ferric iron and be reddish-brown, and stability is high, and ferrous in the ferrous title complex need not restore, and can directly be absorbed by the body.
(3) the ferrous title complex of water soluble soybean polysaccharide is the vegetable polysaccharides iron complex; The part polysaccharide of the ferrous title complex of vegetable polysaccharides has other multiple efficacies concurrently; After water soluble soybean polysaccharide-iron complex discharges in vivo, not only can mend iron, can also bring into play the effect of part.
Embodiment
Embodiment 1
Accurately take by weighing the 0.100g water soluble soybean polysaccharide and the 0.020g trisodium citrate is dissolved in the 15.00mL water, place 60 ℃ of water-baths, slowly drip the copperas solution 2mL of iron content 0.89mmol/mL; The hydrochloric acid soln adjusting pH that drips 1wt% simultaneously is 4.6; Stop to drip continued stirring reaction 1h, 1h is analysed with absolute ethyl alcohol alcohol, 5000r/min spinning 5min in the cooling back; Deposition does not contain ferrous ion with 95% ethanol, absolute ethyl alcohol and anhydrous propanone washing until washing lotion.Get SSPS-Fe (II) title complex after the drying, its iron-holder is 8.5 %.
Embodiment 2
Accurately take by weighing 0.100g water soluble soybean polysaccharide and 0.400g trisodium citrate and be dissolved in the 15.00mL water, other are with embodiment 1, and gained title complex iron-holder is 6.3 %.
Embodiment 3
Accurately take by weighing the 0.100g water soluble soybean polysaccharide and the 0.100g trisodium citrate is dissolved in the 15.00mL water, place 40 ℃ of water-baths, other are with embodiment 1, and gained title complex iron-holder is 16.6 %.
Embodiment 4
Accurately take by weighing the 0.100g water soluble soybean polysaccharide and the 0.100g trisodium citrate is dissolved in the 15.00mL water, place 90 ℃ of water-baths, other are with embodiment 1, and gained title complex iron-holder is 17.9 %.
Embodiment 5
Accurately taking by weighing 0.100g water soluble soybean polysaccharide and 0.100g trisodium citrate is dissolved in the 15.00mL water; Place 60 ℃ of water-baths; Slowly drip the copperas solution 2mL of iron content 0.89mmol/mL, the hydrochloric acid soln adjusting pH that drips 1wt% simultaneously is 4.6, stops to drip continued stirring reaction 0.5 h; Other are with embodiment 1, and gained title complex iron-holder is 13.9 %.
Embodiment 6
Accurately taking by weighing 0.100g water soluble soybean polysaccharide and 0.100g trisodium citrate is dissolved in the 15.00mL water; Place 60 ℃ of water-baths; Slowly drip the copperas solution 2mL of iron content 0.89mmol/mL, the hydrochloric acid soln adjusting pH that drips 1wt% simultaneously is 4.6, stops to drip continued stirring reaction 3.0 h; Other are with embodiment 1, and gained title complex iron-holder is 13.3 %.
Embodiment 7
Accurately taking by weighing 0.100g water soluble soybean polysaccharide and 0.100g trisodium citrate is dissolved in the 15.00mL water; Place 60 ℃ of water-baths; Slowly drip the copperas solution 2mL of iron content 0.89mmol/mL, dripping 1wt% hydrochloric acid adjusting pH simultaneously is 2, stops to drip continued stirring reaction 1.0 h; Other are with embodiment 1, and gained title complex iron-holder is 5.8 %.
Embodiment 8
Accurately taking by weighing 0.100g water soluble soybean polysaccharide and 0.100g trisodium citrate is dissolved in the 15.00mL water; Place 60 ℃ of water-baths; Slowly drip the copperas solution 2mL of iron content 0.89mmol/mL, dripping 10wt % sodium-acetate adjusting pH simultaneously is 5, stops to drip continued stirring reaction 1.0 h; Other are with embodiment 1, and gained title complex iron-holder is 15.8 %.
Claims (6)
1. the preparation method of the ferrous title complex of water soluble soybean polysaccharide is characterized in that, may further comprise the steps:
(1) with after water soluble soybean polysaccharide and the catalyst dissolution; Place 40 ~ 90 ℃ of water-baths, stir and drip copperas solution, dripping hydrochloric acid or sodium acetate soln simultaneously down; Keeping the pH of reaction solution is 2 ~ 5, and ferrous sulfate dripped the continued stirring reaction 0.5 ~ 3 hour;
(2) reaction solution cooling back alcohol is analysed, spinning, and the gained deposition gets the ferrous title complex of water soluble soybean polysaccharide after washing, drying;
Said catalyzer is Citrate trianion or tartrate.
2. method according to claim 1 is characterized in that, said Citrate trianion is trisodium citrate or citric acid tri potassium, and said tartrate is sodium tartrate or soluble tartrate.
3. method according to claim 1 is characterized in that, the mass ratio of said water soluble soybean polysaccharide and catalyzer is 0.25:1 ~ 5:1.
4. method according to claim 1 is characterized in that, it is in reaction solution, to add absolute ethyl alcohol that said alcohol is analysed, and separates out deposition.
5. method according to claim 1 is characterized in that, said washing is alcohol to be analysed the gained deposition wash with 95 % ethanol, absolute ethyl alcohol and anhydrous propanone successively.
6. method according to claim 1 is characterized in that, said drying is warm air drying, vacuum-drying, lyophilize or spraying drying.
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CN102511926B (en) * | 2011-12-23 | 2014-04-02 | 华南理工大学 | Method for extracting and separating laminarin with low molecular weight and application thereof in cigarette products |
CN109824792A (en) * | 2018-12-20 | 2019-05-31 | 中国农业科学院兰州畜牧与兽药研究所 | A kind of preparation method and applications of Radix Salviae Miltiorrhizae ferrous iron polysaccharide |
CN112094361A (en) * | 2020-11-02 | 2020-12-18 | 石家庄飞龙饲料有限公司 | Agaricus blazei murill polysaccharide iron complex, preparation method and application |
CN114288320A (en) * | 2021-12-29 | 2022-04-08 | 珠海天翼医药技术开发有限公司 | Oral iron supplement for pigs and preparation method thereof |
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