CN100378103C - Process for extracting protohemin by using surfactant - Google Patents
Process for extracting protohemin by using surfactant Download PDFInfo
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- CN100378103C CN100378103C CNB2006100800229A CN200610080022A CN100378103C CN 100378103 C CN100378103 C CN 100378103C CN B2006100800229 A CNB2006100800229 A CN B2006100800229A CN 200610080022 A CN200610080022 A CN 200610080022A CN 100378103 C CN100378103 C CN 100378103C
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Abstract
The present invention relates to an extraction method of chlorhematin by a surface active agent, which comprises: mixed liquor is prepared from haemoglobin of livestock and fowl blood, water, acid, and a nonionic surface active agent or a cationic surface active agent; the mixed liquor is gradually heated when the mixed liquor is stirred; the heating is stopped after crystals appear, and the mixed liquor is continually stirred; chlorhematin crystals are separated with centrifugation after the mixed liquor is stood and cooled; the crystals are baked after the crystals are washed with water so as to obtain the products of chlorhematin. The extraction method has the advantages of smooth reaction, simple operation, safe production and low production cost; meanwhile, a large quantity of experiment proves that the repetitiveness of the extraction method is good.
Description
Technical field
The present invention relates to a kind of method of from poultry, fowl blood, extracting protohemine with tensio-active agent.
Background technology
Traditional protoheme manufacture method is a lot, but not ideal enough always, and a lot of patent reports are arranged by literature search both at home and abroad, and wherein most of technology exist with deleterious or inflammable and explosive solvent.Content of hemachrome is very low in the technical products that has.The technology that has does not have treatment process to pollute to the blood ingredient that extracts behind the protoheme.
Produce protohemine with organic solvent ice acetic acid method, ethanol/methyl alcohol method, Ethanol Method, glycerol method, glycol method, dimethyl formamide method, methylethylketone method or acetone method etc., consumption is difficult to greatly reclaim, so the production cost height.In the described organic solvent, all be inflammable and explosive solvent except that glycerol, ethylene glycol, and methyl alcohol there is stronger toxicity, causes a hidden trouble, environment is polluted to production safety.
The extracting method of Chinese patent ZL021223211 chlorhematin as iron-replenishing agent is with the natural coagulation of livestock and poultry animal blood, divides serum deprivation, make pulpous state, make blood meal again, blood meal is added contain in the acetum of salt then, separation can obtain protohemine after being incubated, leaving standstill, lowering the temperature.
The separation and the purifying of Chinese patent ZL87101834 protohemine, be when pH0.5-2.5, by means of cationic, non-ionic or amphoteric tensio-active agent or these surfactant mixtures, with them as catalyzer, temperature be about 90 ℃ to boiling point, rapid heating, crystallization goes out protohemine from contain the muriatic aqueous solution or suspension.This method use temperature height, heating is fast, then must be cooled to reaction below 55 ℃ rapidly and finish, and therefore needs special equipment, and the operation utmost point is not easy, and when heating and cooling, careless slightlyly promptly produces the globin sex change, can't obtain product.
The present invention is directed to the separation of ZL87101834 protohemine and the deficiency of purifying, develop a kind of water-soluble nonionogenic tenside or cats product of using and be catalyzer, in acidic aqueous solution, stir and be heated to gradually less than 85 ℃, crystallization can be separated out, stop heating, continue to stir, slowly cooling naturally, reaction can be finished.
Summary of the invention
The object of the invention is, has developed a kind of method of extracting protohemine with tensio-active agent.This method is that the oxyphorase in poultry, the fowl blood is added water, add acid, form mixed solution with nonionogenic tenside or cats product, under agitation be heated to 70-85 ℃ gradually, stop heating when waiting crystal to occur, continue to stir, behind the non-shock chilling, centrifugation protohemine crystal is washed crystal the back oven dry again and is promptly got the product protohemine.This method is compared with ZL87101834, in the reaction process, stirs in acidic aqueous solution and is heated to gradually less than 85 ℃, and crystallization can be separated out, and stops heating, continues to stir, and slowly lowers the temperature naturally, and reaction can be finished.Present method reacting balance, simple to operate, production safety, production cost is low, through a large amount of evidences, good reproducibility.
The method of extracting protohemine with tensio-active agent of the present invention, this method is with poultry, oxyphorase in the fowl blood adds water, add acid, form mixed solution with nonionogenic tenside fatty alcohol-polyoxyethylene ether or cats product, wherein each proportion of raw materials is: dried oxyphorase: water: hydrochloric acid: tensio-active agent=1: 75-100: 20-65: 13-52, under agitation be heated to 70-85 ℃ gradually, stop heating when waiting crystal to occur, continue to stir 30 minutes, behind the non-shock chilling, centrifugation protohemine crystal is washed crystal the back oven dry again and is promptly got the product protohemine.
The method of extracting protohemine with tensio-active agent of the present invention, hydrochloric acid wherein: the product that is content 〉=35% produced by the GB1897-95 compulsory standard, by same regulation, the finished product protohemine is after repeatedly washing, do not contain hydrochloric acid in the finished product, meet the state food safety requirements.Water: get final product for meeting the softening water that boiler uses.Catalyzer: this method has been carried out a large amount of tests to positively charged ion, a plurality of kinds of nonionic surface active agent, can both obtain the protohemine product, and wherein fatty alcohol-polyoxyethylene ether is optimum, and it is nontoxic and be easy to natural degradation, and is cheap.
Embodiment
All embodiment all by (dried oxyphorase: water=1: the 75-100 volume/weight, hydrochloric acid: dried oxyphorase=20%-65%: 1 weight/volume, tensio-active agent: dried oxyphorase=13%-52%: 1 w/w) take by weighing:
Embodiment 1
Haemoglobin liquid 100ml (containing dried oxyphorase 15.2g) adds 840ml water, add nonionogenic tenside fatty alcohol-polyoxyethylene ether 8g 200ml water dissolution, add hydrochloric acid 10ml, under agitation be heated to 70 ℃ gradually, crystal to be occurred, the liquid look becomes livid purple look, and foam is snow-white, stops heating, continue to stir 30 minutes, behind the non-shock chilling, centrifugation protohemine crystal is washed crystal again, wash from triplicate, oven dry promptly gets product protohemine 0.5319g, and content 90%, yield are 86.34%.
Isolated liquid adds yellow soda ash and carries out neutralization reaction, produces cotton-shaped albumen, and with 400 order net elimination albumen, filtrate is discharged, and after the filter of albumen washing net, is drying to obtain protein powder.
Embodiment 2
Haemoglobin liquid 100ml (containing dried oxyphorase 15.2g) adds 1068ml water, add nonionogenic tenside fatty alcohol-polyoxyethylene ether 8g 200ml water dissolution, add hydrochloric acid 10ml, under agitation be heated to 80 ℃ gradually, crystal to be occurred, the liquid look becomes livid purple look, and foam is snow-white, stops heating, continue to stir 30 minutes, behind the non-shock chilling, centrifugation protohemine crystal is washed crystal again, wash from triplicate, oven dry promptly gets product protohemine 0.5173g, and content 94.57%, yield are 88.34%.
Isolated liquid adds yellow soda ash and carries out neutralization reaction, produces cotton-shaped albumen, and with 400 order net elimination albumen, filtrate is discharged, and after the filter of albumen washing net, is drying to obtain protein powder.
Embodiment 3
Haemoglobin liquid 100ml (containing dried oxyphorase 15.2g) adds 1064ml water, add nonionogenic tenside fatty alcohol-polyoxyethylene ether 8g 200ml water dissolution, add hydrochloric acid 14ml, under agitation be heated to 78 ℃ gradually, crystal to be occurred, the liquid look becomes livid purple look, and foam is snow-white, stops heating, continue to stir 30 minutes, behind the non-shock chilling, centrifugation protohemine crystal is washed crystal again, wash from triplicate, oven dry promptly gets product protohemine 0.5340g, and content 92.82%, yield are 88.34%.
Isolated liquid adds yellow soda ash and carries out neutralization reaction, produces cotton-shaped albumen, and with 400 order net elimination albumen, filtrate is discharged, and after the filter of albumen washing net, is drying to obtain protein powder.
Embodiment 4
Haemoglobin liquid 100ml (containing dried oxyphorase 15.2g) adds 1068ml water, add nonionogenic tenside fatty alcohol-polyoxyethylene ether 8g 200ml water dissolution, add hydrochloric acid 3ml, under agitation be heated to 76 ℃ gradually, crystal to be occurred, the liquid look becomes livid purple look, and foam is snow-white, stops heating, continue to stir 30 minutes, behind the non-shock chilling, centrifugation protohemine crystal is washed crystal again, wash from triplicate, oven dry promptly gets product protohemine 0.5086g, and content 94.57%, yield are 86.85%.
Isolated liquid adds yellow soda ash and carries out neutralization reaction, produces cotton-shaped albumen, and with 400 order net elimination albumen, filtrate is discharged, and after the filter of albumen washing net, is drying to obtain protein powder.
Embodiment 5
Haemoglobin liquid 100ml (containing dried oxyphorase 15.2g) adds 1068ml water, add nonionogenic tenside fatty alcohol-polyoxyethylene ether 2g 200ml water dissolution, add hydrochloric acid 10ml, under agitation be heated to 85 ℃ gradually, crystal to be occurred, the liquid look becomes livid purple look, and foam is snow-white, stops heating, continue to stir 30 minutes, behind the non-shock chilling, centrifugation protohemine crystal is washed crystal again, wash from triplicate, oven dry promptly gets product protohemine 0.5106g, and content 92.12%, yield are 84.94%.
Isolated liquid adds yellow soda ash and carries out neutralization reaction, produces cotton-shaped albumen, and with 400 order net elimination albumen, filtrate is discharged, and after the filter of albumen washing net, is drying to obtain protein powder.
Embodiment 6 (pilot scale)
Haemoglobin liquid 90.5kg (containing dried oxyphorase 11.9g) adds 800kg water, adds nonionogenic tenside fatty alcohol-polyoxyethylene ether 2.84kg 90kg water dissolution, adds 7.1 liters of hydrochloric acid, in acidproof still, stir, be heated to 81 ℃ gradually, crystal occurs, stop heating, continue to stir 30 minutes, behind the non-shock chilling, separate the protohemine crystal, again crystal is washed with tubular-bowl centrifuge, wash from triplicate, oven dry promptly gets product protohemine 352g.
Isolated liquid adds yellow soda ash and carries out neutralization reaction, produces cotton-shaped albumen, and with 400 order net elimination albumen, filtrate is discharged, and after the filter of albumen washing net, is drying to obtain protein powder.
Embodiment 7 (pilot scale)
Haemoglobin liquid 90.5kg (containing dried oxyphorase 11.9g) adds 800kg water, adds nonionogenic tenside fatty alcohol-polyoxyethylene ether 5.68kg 90kg water dissolution, adds 7.1 liters of hydrochloric acid, in acidproof still, stir, be heated to 71 ℃ gradually, crystal occurs, stop heating, continue to stir 30 minutes, behind the non-shock chilling, separate the protohemine crystal, again crystal is washed with tubular-bowl centrifuge, wash from triplicate, oven dry promptly gets product protohemine 365.3g.
Isolated liquid adds yellow soda ash and carries out neutralization reaction, produces cotton-shaped albumen, and with 400 order net elimination albumen, filtrate is discharged, and after the filter of albumen washing net, is drying to obtain protein powder.
Embodiment 8
Haemoglobin liquid 100ml (containing dried oxyphorase 15.2g) adds 1070ml water, add nonionogenic tenside fatty alcohol-polyoxyethylene ether 1g, OS154g and DC4g 300ml water dissolution, add hydrochloric acid 10ml, under agitation be heated to 84 ℃ gradually, crystal to be occurred, the liquid look becomes livid purple look, foam is snow-white, stop heating, continue to stir 30 minutes, behind the non-shock chilling, centrifugation protohemine crystal, crystal is washed again, washed from triplicate, oven dry promptly gets product protohemine 0.34g.
Isolated liquid adds yellow soda ash and carries out neutralization reaction, produces cotton-shaped albumen, and with 400 order net elimination albumen, filtrate is discharged, and after the filter of albumen washing net, is drying to obtain protein powder.
Embodiment 9
Haemoglobin liquid 100ml (containing dried oxyphorase 15.2g) adds 1070ml water, adds cats product cetyl trimethylammonium bromide 10g 200ml water dissolution, adds hydrochloric acid 10ml, under agitation be heated to 81 ℃ gradually, crystal to be occurred, the liquid look becomes livid purple look, foam is snow-white, stop heating, continue to stir 30 minutes, behind the non-shock chilling, centrifugation protohemine crystal, crystal is washed again, washed from triplicate, oven dry promptly gets product protohemine 0.41g.
Isolated liquid adds yellow soda ash and carries out neutralization reaction, produces cotton-shaped albumen, and with 400 order net elimination albumen, filtrate is discharged, and after the filter of albumen washing net, is drying to obtain protein powder.
Claims (1)
- One kind with tensio-active agent from the poultry, extract the method for protohemine in the fowl blood, it is characterized in that poultry, oxyphorase in the fowl blood adds water, add hydrochloric acid, form mixed solution with nonionogenic tenside fatty alcohol-polyoxyethylene ether or cats product, wherein each proportion of raw materials is: dried oxyphorase: water: hydrochloric acid: tensio-active agent=1: 75-100: 20-65: 13-52, under agitation be heated to 70-85 ℃ gradually, stop heating when waiting crystal to occur, continue to stir 30 minutes, behind the non-shock chilling, centrifugation protohemine crystal is washed crystal the back oven dry again and is promptly got the product protohemine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100800229A CN100378103C (en) | 2006-04-28 | 2006-04-28 | Process for extracting protohemin by using surfactant |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100800229A CN100378103C (en) | 2006-04-28 | 2006-04-28 | Process for extracting protohemin by using surfactant |
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| CN1844123A CN1844123A (en) | 2006-10-11 |
| CN100378103C true CN100378103C (en) | 2008-04-02 |
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| CNB2006100800229A Expired - Fee Related CN100378103C (en) | 2006-04-28 | 2006-04-28 | Process for extracting protohemin by using surfactant |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101353686B (en) * | 2008-09-09 | 2011-09-21 | 浙江大学 | Production method of haemachrome and decolorizing blood plasma albumen powder |
| WO2012149689A1 (en) * | 2011-05-05 | 2012-11-08 | Chen Mutao | New process for extracting chlorhematin from anymal blood |
| CN102617581B (en) * | 2012-03-15 | 2013-11-06 | 中国药科大学 | 58Fe hemin, preparation method and application of 58Fe hemin to study of pharmacokinetics |
| CN107098912A (en) * | 2017-05-24 | 2017-08-29 | 四川德博尔制药有限公司 | A kind of protoferriheme and preparation method thereof |
| CN110183497A (en) * | 2019-07-17 | 2019-08-30 | 甘肃养泰和生物科技有限公司 | A method of purifying hemin from animal blood cell |
| CN117886826B (en) * | 2023-12-13 | 2024-09-24 | 甘肃养泰和生物科技有限公司 | Method for extracting methemoglobin by heating and pressurizing |
-
2006
- 2006-04-28 CN CNB2006100800229A patent/CN100378103C/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| 氯化血红素的简便快速分离制备法. 范俊源等.化学通报，第9期. 1995 * |
| 血红素的制备与应用. 吴宝庆等.精细与专用化学品，第9期. 1999 * |
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| CN1844123A (en) | 2006-10-11 |
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