CN1537860A - Purification method of protoheme - Google Patents
Purification method of protoheme Download PDFInfo
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- CN1537860A CN1537860A CNA2003101008943A CN200310100894A CN1537860A CN 1537860 A CN1537860 A CN 1537860A CN A2003101008943 A CNA2003101008943 A CN A2003101008943A CN 200310100894 A CN200310100894 A CN 200310100894A CN 1537860 A CN1537860 A CN 1537860A
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Abstract
A process for purifying heme includes such steps as mixing raw heme with diluted alkali solution, stirring, centrifugal separation of deposit, adding diluted acid solution, educing heme, centrifugal separation of deposit, regulating pH value to make it neutral and drying. Its advantages are high purity (more than 96%), low cost and no pollution.
Description
Technical field
The present invention relates to a kind of purification technique of protoheme, particularly a kind of method of utilizing the protoheme character purifying haemachrome that solvability is different in different pH values solution.
Background technology
Protoheme (Heme, Hame, Protoheme) in animal body normally oxyphorase (Hemoglobins), erythrocruorine (Erythrocrorins), myohaemoglobin (Myoglobins), cytochrome b (Cytochrome b) and some have the prothetic group (Prosthetic group) of the enzyme of biocatalysis such as peroxidase (Peroxidase), catalase (Catalast), Terminal oxidase (Cytochrome COxidase) etc., be quality (Colorfurnishing) composition of oxyphorase.
It is present in the red blood corpuscle (Erythrocyte) and combines with the non covalent bond form with the component globin that wherein constitutes oxyphorase in blood, and the blood color also is by due to the color development of protoheme.
Protoheme is a kind of ferruginous compound, coughs up ring by the poly-heterocyclic compounds that four carbon atom constituted by four arsenic, is called porphines, and the derivative of porphines is called porphyrin again, so protoheme is called protoporphyrin iron (Ferric protoporphyrin) again.Chemical name: 1,3,5,8-tetramethyl--2,4-divinyl porphines-6,7-dipropionic acid iron(ic) chloride, molecular formula: C
34H
32FeCLN
4O
4, molecular weight: 651.96, structural formula is:
Water insoluble, the acetic acid of protoheme is dissolved in dilute alkaline soln, and printing opacity is a brown, and refracted light is the blue look of steel.
Protoheme also has following multiple use except treating hypoferric anemia and the lead poisoning as biological iron:
(1) protoheme is the precursor of multiple important synthetic drugs, and protoheme is modified its side chain and can be obtained a series of porphyrin class medicine-photofrins, protoporphyrin etc. after deironing is handled.Proved that now photofrin and derivative thereof have special avidity to malignant cell, behind the laser radiation tumor locus, cancer cells is coagulation necrosis, and harmless normal cell illustrates that laser-haematoporphyrin combination therapy has lethal effect to cancer cells.(2) the porphyrin disodium salt all has good curative effect for acute, chronic persistent, chronic active hepatitis.(3) protoheme can change into uteroverdine through biochemical reaction, then is reduced into bilirubin, and the bilirubin cost of producing with this method only is 25% of an extraction method.(4) protoheme is the choice drug of treatment porphyria, and porphyria is a kind of hemolytic anemia disease, comes relief of symptoms by gulping down a large amount of blood of drink in the past, now alleviates the state of an illness with the protoheme intravenous drip.(5) protoheme also has the plasmodial effect of dissolving.
Protoheme is of many uses, and its market outlook are good.Especially the precursor as medicine or synthetic drugs more needs highly purified protoheme.The protoheme extraction process mainly contains the sodium-acetate method, distillation method, the tannic acid method, the carboxymethyl cellulose method, ice acetic acid method, acid acetone method, also once adopted esterification process to carry out overtesting in the prior art, but most methods can only prepare protoheme crude product (content is below 80%), the protoheme of will further purifying, make content of hemachrome be higher than 96%, basic be unableing to do without with an organic solvent in these methods, thereby cause the production cost height, environmental pollution is serious, cause product price high, the protoheme existing market selling price of 98% content is ten thousand yuan/kg of 1.0-1.2.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method of easy, fast purifying protoheme, to adapt to needs with low cost and can industrialized mass.
The present invention addresses the above problem the technical scheme that is adopted: the crude product protoheme is mixed with dilute alkaline soln, the centrifugal precipitation of removing after fully stirring, by certain density dilute acid soln protoheme is separated out again again, and then centrifuging and taking throw out, and make throw out to neutral, last drying obtains pure product, and its purity can reach more than 96%.
Dilute alkaline soln of the present invention can be weak ammonia or dilute sodium hydroxide or rare potassium hydroxide, and its concentration is 0.5%-3%.
Abundant stirring of the present invention is meant that churning time is 5-15 minute.
Of the present inventionly protoheme is separated out again be meant that to add concentration again in dilute alkaline soln be the dilute acid soln of 5%-20% again by certain density dilute acid soln, and pH value is transferred to about 3.
Drying of the present invention obtains pure product and is meant that being dried to moisture content under 60 ℃-70 ℃ temperature condition obtains pure product less than 5%.
Dilute acid soln of the present invention can be dilute hydrochloric acid or rare nitric acid or dilute acetic acid.
Advantage of the present invention is: present method does not adopt organic solvent, with the crude product protoheme is raw material, pass through orthogonal test, with diluted alkaline, acid treatment method purifying haemachrome, purifying 1kg crude product protoheme (content is about 80%), its raw materials cost add artificial water power and are about about 300 yuan, its purified product purity is more than 96%, with low cost, pollution-free, for the purifying of protoheme provides a kind of simple and easy, convenient, good technology that cost is low, be convenient to suitability for industrialized production.
Embodiment
In 1kg crude product protoheme, add the 10-25L1.0-3.0% dilute ammonia solution, fully stir after 5-15 minute centrifugal, go precipitation, in dilute ammonia solution, add the 5-10% hydrochloric acid soln again, flocks appears, the centrifuging and taking throw out, and extremely neutral with this throw out of distillation washing, again under 60-70 ℃ temperature with this drying precipitate to moisture content less than 5%, promptly get content more than or equal to 96% pure product protoheme.
In 1kg crude product protoheme, add 100-500L 0.5-2.0% dilute ammonia solution, fully stir after 10-15 minute centrifugal, go precipitation, in dilute ammonia solution, add again 7 again under 60-70 ℃ degree with this drying precipitate to moisture content less than 5%, promptly get content more than or equal to 96% pure product protoheme.
In 1kg crude product protoheme, add 50-250L 1.0-2.5% dilute ammonia solution, fully stir after 5-10 minute centrifugal, go precipitation, in dilute ammonia solution, add the 10-20% hydrochloric acid soln again, flocks appears, the centrifuging and taking throw out, and extremely neutral with this throw out of distillation washing, again under 60-70 ℃ temperature with this drying precipitate to moisture content less than 5%, promptly get content more than or equal to 96% pure product protoheme.
The also available dilute sodium hydroxide of above-described weak ammonia or rare potassium hydroxide are replaced.Then available rare nitric acid of described hydrochloric acid or dilute acetic acid are replaced.
Embodiment 1:
Get the protoheme 1kg of 80% content, add 2.0% dilute ammonia solution 25L, stir after 15 minutes, the centrifugal precipitation of going adds in solution about 7.5% hydrochloric acid adjust pH to 3 again, flocks appears and after, the centrifuging and taking throw out, this throw out is washed with water repeatedly to neutrality, dry pure product, product purity is 98% by analysis.
Embodiment 2:
Get the protoheme 1kg of 80% content, add 1.0% diluted sodium hydroxide solution 50L, stir after 10 minutes, the centrifugal precipitation of going adds in solution about 5% hydrochloric acid adjust pH to 3 again, flocks appears and after, the centrifuging and taking throw out, this throw out is washed with water repeatedly to neutrality, dry pure product, product purity is 98% by analysis.
Embodiment 3:
Get the protoheme 1kg of 80% content, add 3.0% rare potassium hydroxide solution 10L, stir after 5 minutes, the centrifugal precipitation of going adds in solution about 10% hydrochloric acid adjust pH to 3 again, flocks appears and after, the centrifuging and taking throw out, throw out washes with water repeatedly to neutrality, dry pure product, and product purity is 98% by analysis.
Claims (6)
1, a kind of protoheme purification process, it is characterized in that: the crude product protoheme is mixed with dilute alkaline soln, the centrifugal precipitation of removing after fully stirring, by certain density dilute acid soln protoheme is separated out again again, and then centrifuging and taking throw out, and make this throw out to neutral, and last drying obtains pure product, and its purity can reach more than 96%.
2, protoheme purification process according to claim 1 is characterized in that: described dilute alkaline soln can be weak ammonia or dilute sodium hydroxide or rare potassium hydroxide, and its concentration is 0.5%-3%.
3, protoheme purification process according to claim 1 is characterized in that: described abundant stirring is meant that churning time is 5-15 minute.
4, protoheme purification process according to claim 1, it is characterized in that: describedly protoheme is separated out again be meant that to add concentration again in dilute alkaline soln be the dilute acid soln of 5%-20% again by certain density dilute acid soln, and pH value is transferred to about 3.
5, protoheme purification process according to claim 1 is characterized in that: described drying obtains pure product and is meant that being dried to moisture content under 60 ℃-70 ℃ temperature condition obtains pure product less than 5%.
6, according to claim 1 or 4 described protoheme purification process, it is characterized in that: described dilute acid soln can be dilute hydrochloric acid or rare nitric acid or dilute acetic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101008943A CN1280299C (en) | 2003-10-15 | 2003-10-15 | Purification method of protoheme |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101008943A CN1280299C (en) | 2003-10-15 | 2003-10-15 | Purification method of protoheme |
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| CN1537860A true CN1537860A (en) | 2004-10-20 |
| CN1280299C CN1280299C (en) | 2006-10-18 |
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| CNB2003101008943A Expired - Fee Related CN1280299C (en) | 2003-10-15 | 2003-10-15 | Purification method of protoheme |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008049335A1 (en) * | 2006-10-24 | 2008-05-02 | Nanjing Agricultural University | A plant growth regulator containing hemin |
| CN105669685A (en) * | 2016-03-22 | 2016-06-15 | 福建华灿制药有限公司 | Pig protoheme extraction method |
| CN107164340A (en) * | 2017-07-13 | 2017-09-15 | 成都宏安生物科技有限公司 | The extracting method of superoxide dismutase in a kind of fresh porcine blood |
| CN111084337A (en) * | 2019-12-18 | 2020-05-01 | 江苏省农业科学院 | Method for improving water-retaining property and quality of meat product |
-
2003
- 2003-10-15 CN CNB2003101008943A patent/CN1280299C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008049335A1 (en) * | 2006-10-24 | 2008-05-02 | Nanjing Agricultural University | A plant growth regulator containing hemin |
| CN105669685A (en) * | 2016-03-22 | 2016-06-15 | 福建华灿制药有限公司 | Pig protoheme extraction method |
| CN107164340A (en) * | 2017-07-13 | 2017-09-15 | 成都宏安生物科技有限公司 | The extracting method of superoxide dismutase in a kind of fresh porcine blood |
| CN111084337A (en) * | 2019-12-18 | 2020-05-01 | 江苏省农业科学院 | Method for improving water-retaining property and quality of meat product |
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| Publication number | Publication date |
|---|---|
| CN1280299C (en) | 2006-10-18 |
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