CN1064371C - Seaweed polysaccharide trace-element complex and its preparation method and usage - Google Patents
Seaweed polysaccharide trace-element complex and its preparation method and usage Download PDFInfo
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- CN1064371C CN1064371C CN96102440A CN96102440A CN1064371C CN 1064371 C CN1064371 C CN 1064371C CN 96102440 A CN96102440 A CN 96102440A CN 96102440 A CN96102440 A CN 96102440A CN 1064371 C CN1064371 C CN 1064371C
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Abstract
The present invention belongs to the technical field of the preparation of biomacromolecule metal complexes, particularly to a polysaccharide trace element complex prepared by the complex reactions of algae and trace elements. In order to fully use cheap algae as raw materials and save energy, the present invention provides a seaweed polysaccharide metal complex generated by that dry algae are soaked in alkali water to extract seaweed polysaccharide under the conditions of normal temperature and normal pressure and the seaweed polysaccharide takes part in the complex reactions with the ions of trace elements. The polysaccharide trace element complex can be used for animal feed additives, and the growth rate is increased by 10% after the polysaccharide trace element complex is eaten by animals.
Description
The invention belongs to the preparing technical field of biomacromolecule metal complex, particularly relate to the technical field that algae and micro-metals complex reaction prepare polysaccharide trace elements complex.
The biomacromolecule metal complex that biomacromolecule and micro-metal ion react formation under certain condition demonstrates special biological activity, as amino acid, nucleic acid metal complex.The amino acids metal complex compound is made the existing patent of fodder additives.As Methionin and copper complex people such as () the Polish Gdansk Kaczmarek of university, the complex compound that glycine and ferric ion form people such as () the Devore EC of department of chemistry of U.S. Univ Wyoming.Germany's publication number be the complex compound that forms of 2,209,616 medicinal halfcystine and zinc as the zinc supplementation agent, this method is that solder(ing)acid is joined in the halfcystine solution, with NaoH solution adjusting PH and form complex compound.
And for example U.S. Patent number is 3,821, disclose in 192 the specification sheets and a kind ofly formed sugar-iron complex with glucose, maltose, low molecular dextran and ferric chloride reaction, its preparation method mixes with dextran solution with the aqueous solution of ferric ion, and add alkaline solution and precipitate fully up to iron trichloride, this moment, PH was lower than 7, added till alkali makes PH rise to 11 above solution to be the homogeneous state through stirring, temperature remains on 80 ℃ in the reaction process, not above 95 ℃.For fully being precipitated out also, sugared iron-complex compound to add alcohol solution, through centrifugation, drying, be ground into required particle.The product of describing from above-mentioned patent documentation is with amino acid, glucose, maltose warp and metal ion reacting by heating, whole process all need keep higher temperature of reaction, and the complex compound effect of preparing is single, as prepares sugar-iron complex, only is used for the treatment of the piglet hypoferric anemia.
The objective of the invention is to overcome the shortcoming and defect of prior art, in order to make full use of cheap algae resource, and without under the heating condition, have additive, the foodstuff additive of the seaweed polysaccharide trace-element complex of difference in functionality with multiple metallic element complex reaction generation as animal-feed, make raw material with algae at normal temperatures and pressures and in alkali lye, soak (alkalization) and extract polysaccharides thereby provide a kind of, generate seaweed polysaccharide trace-element complex with micro-ion complexation reaction again.With ethanol sedimentation, the dry method of preparing as the seaweed polysaccharide trace-element complex of feed and foodstuff additive of separation.
Task of the present invention is achieved in that
Adopt cheap marine alga to make raw material, wherein marine alga comprises: sargassun, brown alga, red algae, blue algae, green alga, chrysophyceae, sea-tangle etc.With putting into concentration for the dry seaweed of 100g in proportion is that 0.5-5 wt% sodium carbonate solution 1000-10000 ml soaks, and soaks altogether 12-24 hour, filters and extracts polysaccharides liquid, filters residue, again micro-metal ion such as Cu
2+, Fe
3+, Zn
2+, Mn
2+Drip in Sargassum polysaccharides liquid Deng the metal ion solution that is made into 2 mol/L concentration, stir while dripping, add 80-150 ml altogether, to drip the sodium hydroxide solution of 2 mol/L simultaneously, in carrying out, the PH=9-11 basic solution closes reaction, up to can not dissolve add micro-solion till, and the sodium hydroxide solution that continue to drip 2 mol/L stops to add sodium hydroxide solution when making solution reach PH=9-11, in order to make complex reaction even, continue to stir 0.5-2 hour, generate seaweed polysaccharide trace-element complex solution, the ethanol or other alcohol that add 2 times of liquor capacities more inward, till its product precipitation, and adopt centrifugal or filter method leaches it come, the throw out drying can also adopt mechanical means to be ground into required particle and make seaweed polysaccharide trace-element complex.Used chemical feedstocks purity all adopts more than the technical purity.
The structure of Sargassum polysaccharides is as follows:
The structure of seaweed polysaccharide trace-element complex is as follows:
M=Fe wherein
3+, Cu
2+, Zn
2+, Mn
2+
Seaweed polysaccharide trace-element complex of the present invention is used as animal feedstuff additive, and it is to replenish animal growth, breeding trace elements necessary, and can improve the immunologic function of animal, gives anti-and treatment animal hypoferric anemia.
Preparation method of the present invention reacts fully at ambient temperature, does not need pressurized, heated, technology simple, is easy to suitability for industrialized production.Main is to have developed the coastal rich seaweed resources of China.
Below in conjunction with embodiment the present invention is described in detail.Embodiment 1: preparation Sargassum polysaccharides-ferrous metal complex compound
Get the Na that dry sargassun 100 g% totally are placed on 1% concentration
2Co
3Soaked 24 hours in the 5000 ml solution, become the heavy-gravity dark brown solution, filter residue after filtration, in solution, add the FeCl of 2 mol/L
3Solution 100 ml, the limit edged stirs, and adds the pH value of 2 mol/L NaOH regulator solutions simultaneously, makes its solution keep alkalescence, observes in the solution to add FeCl
3Solution has no longer added micro-metal ion solution till can not dissolving, continuing to stir adding 2 mol/L NaOH stops to add when the PH=9-11 scope, restir 0.5 hour, after little precipitation all dissolves like the snowflake, stop to stir the industrial alcohol that adds 2 times of total liquor capacities again, produce a large amount of flockss, at room temperature place filtration or centrifugal in 3 hours, gained rust product is Sargassum polysaccharides one ferrous metal complex compound.Embodiment 2: preparation Sargassum polysaccharides-copper metal complex
Step is with embodiment 1, and raw material adopts sargassun 100 g and Na
2CO
3Concentration is 5% 5000 ml that use, and soak time adopted 12 hours, and micro-metal ion solution is with the CuSO of 2 mol/L
4Solution regulates to generate sargassan-copper complex formazan blue green solution with NaOH solution, more after filtration, drying obtains final blue green complex compound product.Embodiment 3: preparation Sargassum polysaccharides-zinc complex
Press the preparation of embodiment 1 step, wherein raw material adopts sargassun 100 g, Na
2CO
3Concentration is 2.5% (weight percent), 5000 ml, soaks 18 hours, and adding concentration is the ZuSO of 2 mol/L
4Zinc solution, and to add NaOH concentration simultaneously be that 2 mol/L stirred 1 hour, placed 5 hours under the room temperature, all the other prepare canescence Sargassum polysaccharides-zinc network and thing with embodiment 1.Embodiment 4: preparation laminarin-iron complex
Press embodiment 1 step, condition preparation, just adopt sea-tangle to do raw material, get and clean dried sea-tangle 100g, be placed on the Na of 1% concentration
2CO
3Soaked 24 hours in the 5000 ml solution, filter residue after filtration, in solution, add the FeCl that 2 mol/ rise
3Solution 100 ml, the limit edged stirs, and adds the pH value of 2 mol/L NaOH regulator solutions simultaneously, makes its solution keep alkalescence, observes in the solution to add FeCl
3Till can not dissolving, solution no longer adds FeCl
3Solution, continuing to stir adding 2 mol/L NaOH stops to add when the PH=9-11 scope, restir 0.5 hour, after little precipitation all dissolves like the snowflake, stop to stir the industrial alcohol that adds 2 times of total liquor capacities again, produce a large amount of flockss, place filtration or centrifugal in 3 hours under the room temperature, gained rust product is laminarin-ferrous metal complex compound.Embodiment 5: preparation Sargassum polysaccharides-manganese complex
Step just adopts the MnCl of sargassun 100g and 2 mol/L with embodiment 1
2Solution is done raw material, Na
2Co
3Concentration is 5%, uses 5000 ml, and soak time adopted 12 hours, generates the solution of sargassan-manganese complex, more after filtration, drying obtains the manganese complex product.Embodiment 6:
Be used for fodder additives the rate of animals delivered to the slaughter-house of chicken is improved greatly, advanced 2856 of baby chicks (28 case) on December 3rd, 1994, chick is a U.S. AA chicken, and feed is the fast large-scale fryer material of " five is rich " board that the herding of academy of agricultural sciences, Guangdong Province is produced.From 28 casees chickens, arbitrarily extract 4 casees (102 in every case) out, weigh and make original records, with the insulation of 250W insulation lamp.All the other conditions are identical and weigh ages in one, three, six weeks.
| Group | One group | Two groups | Three groups | Control group |
| One age in days | 44.1g | 43.6g | 47.1g | 44.7g |
| One age in week | 118.6g | 114.7g | 111.8g | 111.7g |
| Three ages in week | 602g | 601g | 623g | 625g |
| Six ages in week | 1910g | 1900g | 1875g | 1875g |
| The rate of animals delivered to the slaughter-house | 89.25％ | 86.27％ | 86.27％ | 81.37％ |
Annotate: the rate of animals delivered to the slaughter-house of jumpbogroup contrast is 79%.
The addition of sargassan iron complex is divided into as follows: add 1.5g first group of every day, second group is added 3.0g, and the 3rd group is 4.5g, and four groups and jumpbogroup are control group.When chick was marched into the arena, all chickens all carried out the conventional vaccine injection.The whole audience has carried out anti-pre-chicken septicemia body disease with the 0.05-0.1% chloramphenicol solution again when 12 ages in days.The experimental group chicken is not treated with other drug after removing and using this twice medicine again.Used paraxin before and after the chicken that control group and jumpbogroup are raised, doxycycline, the swollen toxicide of kidney, medicines such as poultry chick spirit.The drug cost of every chicken of experimental group is 0.06 yuan, and the average drug cost of every chicken that control group and jumpbogroup are raised is 0.20 yuan.Test first group of per 100 every day and only add 1.5g, but effect is best, the rate of animals delivered to the slaughter-house of raising than jumpbogroup exceeds 10%, and this can make the raiser obtain very considerable economic.
Experiment is taken turns in beginning on February 26 nineteen ninety-five second.The chicken kind is 3060 of age in days AA chickens, is divided into two groups with 3060, and one group is test group, and one group is control group, the raising condition, and two groups in feed is just the same, and per 100 chickens of test group are day to add 1.5g sargassan iron complex.Raised altogether 44 days.At finishing period, control group is successively used paraxin, powerful mould speed, and medicines such as poultry chick spirit, every chicken is used 0.20 yuan of expenses for medicine, and the not used any medicine of experimental group.The rate of animals delivered to the slaughter-house of experimental group is 81%, and the rate of animals delivered to the slaughter-house of control group is 76.3%.After experiment finishes, chicken is butchered, experimental group is taken out 84 internal organ at random, and control group takes out 50 chicken organs at random and delivers to animal medicine system of Agricultural University Of South China and carry out pathologic finding.Do the inspection of section Electronic Speculum with paraffin.Microscopy experimental group as a result has 10 of pathologies, accounts for 11.9% of experimental group sum, and control group has pathology is 7 and accounts for 14.00% of control group sum.Pathology is mainly Mareks pathology, hepatitis, visceral pericardium inflammation etc.
The tigar prawn that is used for the fodder additives nursing, the amount by 1.5% add the sargassan iron complex in prawn feed raises tigar prawn.Tigar prawn grow a big body weight, the shrimp body is Bluish white, searches for food actively, original rubescent shrimp body also changes into bluish white transparent color through the raising of sargassan iron complex, in trial period none death of prawn, an average week increases by 1 centimeter.(annotate: healthy shrimp body is a Bluish white, and the shrimp body takes on a red color and then is on the verge of death.) embodiment 7:
The toxicology of seaweed polysaccharide trace-element complex of the present invention and biological activity test result are as follows: the toxicologic study of (1) sargassan trace-element complex
With water is solvent, and with sargassan iron, zinc, manganese, steel dissolving, concentration is 4.50 g100
-1Ml gives mouse stomach 15 days, none death of mouse, and the outward appearance behavior is normal, and it is all normal to be viewed as each organ of internal organ after the dissection, and sargassan trace-element complex no side effects is described.Calculating oral maximal dose is 9.9 gkg
-1LD
50＞9.99kg
-1Kg.(2) sargassan iron is to the influence of mouse oxyphorase
With 4.50 g kg
-1Ml dosage is given mouse stomach 15 days, and the oxyphorase of mouse is 11.8 ± 0.85g, and control group is 9.5 ± 0.5g.(3) to the effect of mouse immune organ
Respectively with high dosage (0.45gkg
-1), middle dosage (0.3gkg
-1), low dosage (0.15gkg
-1) gave mouse stomach 7 days, after the execution, claim its spleen, survey the index of cleaning up of serum, spleen index and to clean up index all good than control group is cleaned up index and is exceeded 2-3 doubly than control group as a result, and the effect of middle dosage group is best.
Claims (5)
1. seaweed polysaccharide trace-element complex is characterized in that: its structural formula:
Wherein M comprises Fe
3+, Cu
2+, Zn
2+, M
n 2+
2. method for preparing the described seaweed polysaccharide trace-element complex of claim 1, it is characterized in that: 1. being the sodium carbonate solution that 100 g dry seaweeds are soaked into 1000-10000 ml 0.5-5wt% in proportion, after-filtration extracted polysaccharides in 12-24 hour; 2. micro-metal cations Fe
3+, Cu
2+, Zn
2+, Mn
2+Be made into the metal ion solution of 2mol/L concentration respectively; 3. the metal ion solution that 80-150 ml has been prepared 2 mol/L concentration is added drop-wise in the polysaccharides that has extracted, the limit edged stirs and carries out complex reaction till solution is saturated, the sodium hydroxide solution that splashes into 2 mol/L simultaneously keeps the solution pH value to stop to add alkali in the 9-11 scope, continue to stir 0.5-2 hour, generate seaweed polysaccharide trace-element complex solution; 4. in the seaweed polysaccharide trace-element complex solution that 3. step generates, add alcohol, add alcohol amount be the amount of 2 times of seaweed polysaccharide trace-element complex liquor capacities, produce sedimentation and filtration or centrifugation, drying, make seaweed polysaccharide trace-element complex.
3. by the described method for preparing seaweed polysaccharide trace-element complex of claim 2, it is characterized in that: described marine alga comprises: sargassun, brown alga, red algae, blue algae, green alga, chrysophyceae.
4. press the method for the seaweed polysaccharide trace-element complex of the described preparation of claim 2, it is characterized in that: 4. described step makes dried seaweed polysaccharide trace-element complex again through being ground into required particle;
5. the purposes by the described seaweed polysaccharide trace-element complex of claim 1 is characterized in that: be used as foodstuff additive and animal feedstuff additive.
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|---|---|---|---|
| CN96102440A CN1064371C (en) | 1996-03-05 | 1996-03-05 | Seaweed polysaccharide trace-element complex and its preparation method and usage |
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| CN96102440A CN1064371C (en) | 1996-03-05 | 1996-03-05 | Seaweed polysaccharide trace-element complex and its preparation method and usage |
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|---|---|
| CN1148600A CN1148600A (en) | 1997-04-30 |
| CN1064371C true CN1064371C (en) | 2001-04-11 |
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| CN96102440A Expired - Fee Related CN1064371C (en) | 1996-03-05 | 1996-03-05 | Seaweed polysaccharide trace-element complex and its preparation method and usage |
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|---|---|---|---|---|
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