CN112574222A - Process for extracting high-purity heme iron from pig blood to prepare blood-benefiting crystal granule intermediate - Google Patents

Process for extracting high-purity heme iron from pig blood to prepare blood-benefiting crystal granule intermediate Download PDF

Info

Publication number
CN112574222A
CN112574222A CN202011449969.9A CN202011449969A CN112574222A CN 112574222 A CN112574222 A CN 112574222A CN 202011449969 A CN202011449969 A CN 202011449969A CN 112574222 A CN112574222 A CN 112574222A
Authority
CN
China
Prior art keywords
pig blood
heme iron
acetic acid
blood
centrifugation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202011449969.9A
Other languages
Chinese (zh)
Inventor
许云
肖雄
刘瑾
胡锐敏
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangxi Jinshuibao Pharmaceutical Co ltd
Jiangxi Jimin Kexin Pharmaceutical Co Ltd
Original Assignee
Jiangxi Jinshuibao Pharmaceutical Co ltd
Jiangxi Jimin Kexin Pharmaceutical Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jiangxi Jinshuibao Pharmaceutical Co ltd, Jiangxi Jimin Kexin Pharmaceutical Co Ltd filed Critical Jiangxi Jinshuibao Pharmaceutical Co ltd
Priority to CN202011449969.9A priority Critical patent/CN112574222A/en
Publication of CN112574222A publication Critical patent/CN112574222A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D487/00Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00
    • C07D487/22Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00 in which the condensed system contains four or more hetero rings

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Medicines Containing Material From Animals Or Micro-Organisms (AREA)
  • Peptides Or Proteins (AREA)

Abstract

The invention relates to a method for extracting high-purity heme iron from pig blood, which comprises the following steps: 1) naturally coagulating fresh pig blood; 2) crushing and homogenizing by a multifunctional colloid mill; 3) centrifuging by a centrifuge; 4) preparing by an acetic acid method; 5) and (4) obtaining the high-purity heme iron after high-speed tubular centrifugation and continuous automatic spraying, washing and purifying.

Description

Process for extracting high-purity heme iron from pig blood to prepare blood-benefiting crystal granule intermediate
Technical Field
The invention relates to a medicine extraction technology, in particular to a method for extracting high-purity heme iron from pig blood, and belongs to the technical field of medicines.
Background
The heme iron, namely the porphyrin iron, is a porphyrin compound consisting of a porphyrin ring and a bivalent ferric ion, is separated and extracted from pig blood, is easy to be absorbed by a human body, and is a main intermediate for preparing blood benefiting crystal particles. The blood benefiting crystal particle is an innovative Chinese medicinal compound preparation prepared from a pig blood extract, astragalus and Chinese date, and is suitable for enriching blood and tonifying qi. Can be used for treating sallow complexion or pale complexion, dizziness, listlessness, and hypodynamia.
The existing extraction method of heme iron comprises the following steps:
filtering fresh pig blood according to the coagulation condition to remove residual blood, grinding by a colloid mill for 30 seconds, wherein the grinding particle size is 0.3cm, the material feeding temperature is 5 ℃, and the feeding speed is 1.5 t/h. Then 5 times of anhydrous acetic acid is added, 0.25 percent of sodium citrate and sodium chloride are added according to the proportion of 1:1, the mixture is refluxed and extracted for 30 minutes, the raw material feeding time is 15 minutes, the reaction temperature is 95 ℃, and the stirring speed is 30 r/min. Cooling at 20 deg.C for 24 hr, filtering with 100 mesh filter, refining with 15 times of 50% ethanol by tubular centrifugation for 20 times, vacuum drying under reduced pressure until the water content is not higher than 2.0% at 70 deg.C, and pulverizing with 120 mesh filter to obtain sanguis Sus Domestica extract.
The existing extraction method has the following defects:
the crude pig blood extract needs to be refined 20 times by tube-type centrifugal refining, 15 times of 50% ethanol is consumed each time, the production operation is very complicated, the automatic continuous level is low, the time and the labor are consumed, the ethanol consumption is huge, the production cost is high, and the pollution to the environment is large.
The invention optimizes the existing pig blood extraction process through technical innovation to prepare the high-purity heme iron and meets the industrialization requirement of high-quality blood-benefiting crystal particles.
Disclosure of Invention
The invention aims to provide a preparation method for extracting high-purity heme iron from pig blood, and the prepared heme iron has high purity and less impurities through a high-speed tubular centrifugation and continuous automatic spraying combined process technology, is beneficial to improving the quality of blood benefiting crystal particles, can save the using amount of ethanol during production, and reduces environmental pollution and production cost.
The method comprises the following steps:
1) naturally coagulating fresh pig blood;
2) crushing and homogenizing by a multifunctional colloid mill;
3) centrifuging by a centrifuge;
4) preparing by an acetic acid method;
5) and (4) obtaining the high-purity heme iron after high-speed tubular centrifugation and continuous automatic spraying, washing and purifying.
Wherein, in the step 1), fresh pig blood is naturally coagulated, and supernatant is removed to obtain hemoglobin;
in the step 2), homogenizing and crushing by using a multifunctional colloid mill to obtain homogenate, wherein the conditions for crushing and homogenizing are as follows: the time is 10-65 s;
wherein, in the step 3), a centrifuge is used for centrifuging the homogenate in the previous step, the upper layer of pig plasma is removed, and the lower layer of pig blood cells are collected, wherein the centrifugation time is 5-25 min;
wherein, in the step 4), the preparation is carried out by an acetic acid method, glacial acetic acid and sodium chloride are added into a reaction kettle, the reaction kettle is heated to 75-115 ℃ to dissolve the sodium chloride, the porcine blood cells in the previous step are slowly added, the temperature is kept at 75-115 ℃ for 10-60min, and then the mixture is cooled to room temperature, wherein the adding amount of the glacial acetic acid is 2-6 times of the weight of the porcine blood cells, and the adding amount of the sodium chloride is 0.1-0.8% of the weight of the porcine blood cells;
and in the step 5), the reaction liquid prepared by the acetic acid method flows into a high-speed tubular centrifuge through a pipeline, 10-25 times of water is added, the centrifugation is carried out, the normal operation of the high-speed tubular centrifuge is kept, the spraying is carried out through a continuous automatic spraying device, wherein the automatic washing solvent is 20-80% (v/v) ethanol water solution, the using amount of the ethanol water solution is 1-3 times of the volume of fresh pig blood, the temperature is 20-60 ℃, the centrifugation is carried out for 1-4 hours after 20-100min of the heme iron obtained by the primary centrifugal separation is sprayed, and the obtained solid heme iron is dried for 2-12 hours in a vacuum drying oven at the temperature of 40-80 ℃ to obtain the solid heme iron.
The method and technical parameters of the invention are obtained by screening, and the screening process is as follows:
in order to improve the purification effect of the pig blood extract by high-speed tubular centrifugation and continuous automatic spraying washing, the purity of heme iron is taken as an investigation index, process research is carried out aiming at a solvent, the dosage, the temperature and the centrifugation time, and process screening is carried out according to the parameters to determine the optimal pretreatment process.
TABLE 1 4-factor 3 horizontal table affecting purification effect of pig blood extract
Figure BDA0002831717770000021
Figure BDA0002831717770000031
TABLE 2 orthogonal Experimental tables for the screening of purification Effect factors
Figure BDA0002831717770000032
Analysis of variance of factors affecting purification effectiveness
Figure BDA0002831717770000033
(significant if the critical value of F is greater than 19.000.)
In summary, the following steps: the optimal purification process parameters are as follows: the refined solvent is 50% ethanol, the dosage of the refined solvent is 3 times of the volume of the fresh pig blood, the temperature of the refined solvent is 60 ℃, and the refined solvent is purified by high-speed tubular centrifugation and continuous automatic spraying.
The advantageous effects of the present invention (calculated as 200 parts by weight per batch) are further illustrated by comparative experiments as follows.
Item Purity of pig blood extract The amount of ethanol Production time per batch Amount of waste liquid
Inventive example 1 93% 600Vol. 70h 1600Vol.
Inventive example 2 95% 600Vol. 72h 1600Vol.
Prior art 1 89% 3000Vol. 140h 4000Vol.
Prior art 2 87% 3000Vol. 120h 4000Vol.
Wherein, in the prior art 1, the fresh pig blood is filtered to remove the residual blood according to the coagulation condition, and is ground by a colloid mill for 30 seconds, the grinding particle size is 0.3cm, the material feeding temperature is 5 ℃, and the feeding speed is 1.5 t/h. Then 5 times of anhydrous acetic acid is added, 0.25 percent of sodium citrate and sodium chloride are added according to the proportion of 1:1, the mixture is refluxed and extracted for 30 minutes, the raw material feeding time is 15 minutes, the reaction temperature is 95 ℃, and the stirring speed is 30 r/min. Cooling at 20 deg.C for 24 hr, filtering with 100 mesh filter, refining with 15 times of 50% ethanol by tubular centrifugation for 20 times, vacuum drying under reduced pressure until the water content is not higher than 2.0% at 70 deg.C, and pulverizing with 120 mesh filter to obtain sanguis Sus Domestica extract.
In the prior art 2, the fresh pig blood is filtered to remove residual blood according to the coagulation condition, and is ground by a colloid mill for 30 seconds, the grinding particle size is 0.3cm, the material feeding temperature is 5 ℃, and the feeding speed is 1.5 t/h. Then 5 times of anhydrous acetic acid is added, 0.25 percent of sodium citrate and sodium chloride are added according to the proportion of 1:1, the mixture is refluxed and extracted for 30 minutes, the raw material feeding time is 15 minutes, the reaction temperature is 95 ℃, and the stirring speed is 30 r/min. Cooling at 20 deg.C for 24 hr, filtering with 100 mesh filter, refining with 20 times of 50% ethanol by tubular centrifugation for 15 times, vacuum drying under reduced pressure until the water content is not higher than 2.0% at 70 deg.C, and pulverizing with 120 mesh filter to obtain sanguis Sus Domestica extract.
The experimental data show that the technical scheme of the invention is superior to the prior art in technical effect.
The invention provides a process for preparing a blood-benefiting crystal particle intermediate by extracting high-purity heme iron from pig blood. The inventor prepares the hemoglobin iron with high purity and few impurities by a high-speed tubular centrifugation and continuous automatic spraying combined process technology, is beneficial to improving the quality of the blood benefiting crystal particles, and provides a technical basis for the quality improvement and the efficiency increase of subsequent blood benefiting crystal particle products.
Detailed Description
The present invention will be described in further detail with reference to the following examples. This should not be understood as limiting the scope of the above-described subject matter of the present invention to the following examples. All the technologies realized based on the above contents of the present invention belong to the scope of the present invention.
The raw materials and equipment used in the embodiment of the invention are all known products.
Example 1, a process for preparing a blood-benefiting crystal granule intermediate from pig blood by extracting high-purity heme iron from pig blood comprises the steps of naturally coagulating 50kg of fresh pig blood, removing supernatant to obtain hemoglobin, grinding the hemoglobin by using a multifunctional colloid mill for 30 seconds to break and homogenize, adding a certain amount of glacial acetic acid and sodium chloride (the weight ratio of the glacial acetic acid to the pig blood cells is 3, and the sodium chloride is 0.5 percent of the weight of the pig blood cells) into a reaction kettle, heating the reaction kettle to 100 ℃, dissolving the sodium chloride, slowly adding the pig blood cells, preserving the temperature at 100 ℃ for 20min, and cooling the mixture to room temperature. Adding purified water to make the ratio of material to liquid (kg/L) 1:20, introducing into high-speed tubular centrifuge, centrifuging for 30min, starting continuous automatic spraying system (50% ethanol/water as automatic washing solvent, 50 deg.C, and spraying speed of 150L/h), keeping the high-speed tubular centrifuge running, spraying after 1h, and vacuum drying at 60 deg.C for 5 hr.
Example 2, a process for preparing a blood-benefiting crystal granule intermediate from pig blood by extracting high-purity heme iron from pig blood comprises the steps of naturally coagulating 50kg of fresh pig blood, removing supernatant to obtain hemoglobin, grinding the hemoglobin by using a multifunctional colloid mill for 30 seconds to break and homogenize, adding a certain amount of glacial acetic acid and sodium chloride (the weight ratio of the glacial acetic acid to the pig blood cells is 3, and the sodium chloride is 0.5 percent of the weight of the pig blood cells) into a reaction kettle, heating the reaction kettle to 100 ℃, dissolving the sodium chloride, slowly adding the pig blood cells, preserving the temperature at 100 ℃ for 20min, and cooling the mixture to room temperature. Adding purified water to make the ratio of material to liquid (kg/L) 1:20, introducing into high-speed tubular centrifuge, centrifuging for 30min, starting continuous automatic spraying system (50% ethanol/water as automatic washing solvent, 50 deg.C, and spraying speed of 75L/h), keeping high-speed tubular centrifuge running, spraying after 2h, and vacuum drying at 60 deg.C for 5 hr.
Example 3, a process for preparing an intermediate of Yixuejing granule from pig blood by extracting high purity heme iron from pig blood comprises the steps of naturally coagulating 50kg of fresh pig blood, removing supernatant to obtain hemoglobin, grinding with a multifunctional colloid mill for 30s to break and homogenize, adding a certain amount of glacial acetic acid and sodium chloride (the weight ratio of glacial acetic acid to pig blood cell is 3, and the sodium chloride is 0.5% of the weight of pig blood cell) into a reaction kettle, heating to 100 ℃, dissolving the sodium chloride, slowly adding the pig blood cell, keeping the temperature at 100 ℃ for 20min, and cooling to room temperature. Adding purified water to make the ratio of material to liquid (kg/L) 1:20, introducing into high-speed tubular centrifuge, centrifuging for 30min, starting continuous automatic spraying system (50% ethanol/water as automatic washing solvent, 50 deg.C, and 50L/h spraying speed), keeping the high-speed tubular centrifuge running, spraying for 3h, and vacuum drying at 60 deg.C for 5 hr.
Example 4, a process for preparing an intermediate of Yixuejing granule from pig blood by extracting high purity heme iron from pig blood comprises the steps of naturally coagulating 50kg of fresh pig blood, removing supernatant to obtain hemoglobin, grinding with a multifunctional colloid mill for 30s to break and homogenize, adding a certain amount of glacial acetic acid and sodium chloride (the weight ratio of glacial acetic acid to pig blood cell is 3, and the sodium chloride is 0.5% of the weight of pig blood cell) into a reaction kettle, heating to 100 ℃, dissolving the sodium chloride, slowly adding the pig blood cell, keeping the temperature at 100 ℃ for 20min, and cooling to room temperature. Adding purified water to make the ratio of material to liquid (kg/L) 1:20, introducing into high-speed tubular centrifuge, centrifuging for 30min, starting continuous automatic spraying system (50% ethanol/water as automatic washing solvent, 50 deg.C, and 38L/h spraying speed), keeping the high-speed tubular centrifuge running, spraying after 4h, and vacuum drying at 60 deg.C for 5 hr.
Obviously, many modifications, substitutions, and variations are possible in light of the above teachings of the invention, without departing from the basic technical spirit of the invention, as defined by the following claims.

Claims (1)

1. A method for extracting high-purity heme iron from pig blood comprises the following steps:
5) naturally coagulating fresh pig blood;
6) crushing and homogenizing by a multifunctional colloid mill;
7) centrifuging by a centrifuge;
8) preparing by an acetic acid method;
5) and (4) obtaining the high-purity heme iron after high-speed tubular centrifugation and continuous automatic spraying, washing and purifying.
Wherein, in the step 1), fresh pig blood is naturally coagulated, and supernatant is removed to obtain hemoglobin;
in the step 2), homogenizing and crushing by using a multifunctional colloid mill to obtain homogenate, wherein the conditions for crushing and homogenizing are as follows: the time is 10-65 s;
wherein, in the step 3), a centrifuge is used for centrifuging the homogenate in the previous step, the upper layer of pig plasma is removed, and the lower layer of pig blood cells are collected, wherein the centrifugation time is 5-25 min;
wherein, in the step 4), the preparation is carried out by an acetic acid method, glacial acetic acid and sodium chloride are added into a reaction kettle, the reaction kettle is heated to 75-115 ℃ to dissolve the sodium chloride, the porcine blood cells in the previous step are slowly added, the temperature is kept at 75-115 ℃ for 10-60min, and then the mixture is cooled to room temperature, wherein the adding amount of the glacial acetic acid is 2-6 times of the weight of the porcine blood cells, and the adding amount of the sodium chloride is 0.1-0.8% of the weight of the porcine blood cells;
and in the step 5), the reaction liquid prepared by the acetic acid method flows into a high-speed tubular centrifuge through a pipeline, 10-25 times of water is added, the centrifugation is carried out, the normal operation of the high-speed tubular centrifuge is kept, the spraying is carried out through a continuous automatic spraying device, wherein the automatic washing solvent is 20-80% (v/v) ethanol water solution, the using amount of the ethanol water solution is 1-3 times of the volume of fresh pig blood, the temperature is 20-60 ℃, the centrifugation is carried out for 1-4 hours after 20-100min of the heme iron obtained by the primary centrifugal separation is sprayed, and the obtained solid heme iron is dried for 2-12 hours in a vacuum drying oven at the temperature of 40-80 ℃ to obtain the solid heme iron.
CN202011449969.9A 2020-12-12 2020-12-12 Process for extracting high-purity heme iron from pig blood to prepare blood-benefiting crystal granule intermediate Pending CN112574222A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011449969.9A CN112574222A (en) 2020-12-12 2020-12-12 Process for extracting high-purity heme iron from pig blood to prepare blood-benefiting crystal granule intermediate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011449969.9A CN112574222A (en) 2020-12-12 2020-12-12 Process for extracting high-purity heme iron from pig blood to prepare blood-benefiting crystal granule intermediate

Publications (1)

Publication Number Publication Date
CN112574222A true CN112574222A (en) 2021-03-30

Family

ID=75131255

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011449969.9A Pending CN112574222A (en) 2020-12-12 2020-12-12 Process for extracting high-purity heme iron from pig blood to prepare blood-benefiting crystal granule intermediate

Country Status (1)

Country Link
CN (1) CN112574222A (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1998028302A1 (en) * 1996-12-20 1998-07-02 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Method of obtaining haemin from slaughter blood
CN102187937A (en) * 2011-03-22 2011-09-21 湖北宝迪农业科技有限公司 Method for producing globulin zymolytes of porcine blood
WO2012149689A1 (en) * 2011-05-05 2012-11-08 Chen Mutao New process for extracting chlorhematin from anymal blood
CN105566334A (en) * 2015-12-18 2016-05-11 湖南益阳益威生化试剂有限公司 Production method for preparing heme by using blood meal

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1998028302A1 (en) * 1996-12-20 1998-07-02 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Method of obtaining haemin from slaughter blood
CN102187937A (en) * 2011-03-22 2011-09-21 湖北宝迪农业科技有限公司 Method for producing globulin zymolytes of porcine blood
WO2012149689A1 (en) * 2011-05-05 2012-11-08 Chen Mutao New process for extracting chlorhematin from anymal blood
CN105566334A (en) * 2015-12-18 2016-05-11 湖南益阳益威生化试剂有限公司 Production method for preparing heme by using blood meal

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
袁曦、洪清: "氯化血红素提取工艺及质量标准研究", 《中国药学杂志》 *
钟耀广: "利用冰醋酸提取血红素的研究", 《食品科学》 *
马永征: "血红素提取和精制方法的研究进展", 《化工文摘》 *

Similar Documents

Publication Publication Date Title
CN110304994B (en) Method for extracting high-purity cannabidiol from industrial cannabis sativa
CN101831008B (en) New production process for refining crude heparin sodium
CN112174796B (en) Method for extracting coenzyme Q10 from coenzyme Q10 fermentation liquor
CN107337593B (en) Preparation method of coenzyme Q10 pure product
CN111875528A (en) Method for preparing astaxanthin oil from haematococcus pluvialis
CN107115367B (en) Fermentation production method for efficiently extracting flavone from ginkgo leaves
CN111893156A (en) Preparation method of refined yak bone collagen peptide
CN102311496B (en) Method for recovering albumin from deposited components I+II+III from cold ethanol method
CN107286270A (en) A kind of method that utilization enzymatic isolation method prepares liquaemin
CN112574222A (en) Process for extracting high-purity heme iron from pig blood to prepare blood-benefiting crystal granule intermediate
CN113980090B (en) Method for recycling biological source protein by using biological medicine fermentation fungus dreg
CN110615857A (en) Method for recycling waste in orange can processing production
CN113197935B (en) Extraction method of magnolia officinalis extract
CN105543185B (en) A kind of production method extracted from animal clot, purify SOD freeze-dried powder
CN107759467A (en) A kind of preparation method for improving carnosic acid content in rosemary fat-soluble antioxidant
CN111961111B (en) American cockroach polypeptide extraction method
KR101182008B1 (en) Method of extracting mandarin oil and pectin from sweet orange peels
CN110878014B (en) Method for rapidly extracting gingerol
CN111840323B (en) Preparation method of pig blood extract
CN106279345A (en) A kind of industrialized preparing process of thick glycyrrhizic acid
CN106883312A (en) A kind of extracting method of silkworm excrement pectin
US20220204522A1 (en) Process for separating and purifying artemisinin
CN110862429A (en) Preparation method of sodium aescinate
CN109734619A (en) A method of impurity A, C are isolated and purified from phenobarbital production waste residue
CN105153061B (en) A kind of method of solvent method treated rubber accelerator M

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20210330

RJ01 Rejection of invention patent application after publication