CN108129485A - Make ferroheme and preparation method, converted starch solubilising ferroheme and preparation method by oneself - Google Patents
Make ferroheme and preparation method, converted starch solubilising ferroheme and preparation method by oneself Download PDFInfo
- Publication number
- CN108129485A CN108129485A CN201810034502.4A CN201810034502A CN108129485A CN 108129485 A CN108129485 A CN 108129485A CN 201810034502 A CN201810034502 A CN 201810034502A CN 108129485 A CN108129485 A CN 108129485A
- Authority
- CN
- China
- Prior art keywords
- ferroheme
- preparation
- control
- self
- 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
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 229920002472 Starch Polymers 0.000 title claims abstract description 19
- 235000019698 starch Nutrition 0.000 title claims abstract description 19
- 239000008107 starch Substances 0.000 title claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 32
- 238000005119 centrifugation Methods 0.000 claims abstract description 31
- 210000004369 blood Anatomy 0.000 claims abstract description 22
- 239000008280 blood Substances 0.000 claims abstract description 22
- 230000003381 solubilizing effect Effects 0.000 claims abstract description 20
- 241000282994 Cervidae Species 0.000 claims abstract description 17
- 108090000790 Enzymes Proteins 0.000 claims abstract description 17
- 102000004190 Enzymes Human genes 0.000 claims abstract description 17
- 230000009849 deactivation Effects 0.000 claims abstract description 12
- 235000013826 starch sodium octenyl succinate Nutrition 0.000 claims abstract description 11
- 239000001334 starch sodium octenyl succinate Substances 0.000 claims abstract description 11
- 238000002525 ultrasonication Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 9
- 235000013365 dairy product Nutrition 0.000 claims abstract description 9
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 9
- 239000004365 Protease Substances 0.000 claims abstract description 7
- 150000001413 amino acids Chemical class 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000007710 freezing Methods 0.000 claims abstract description 7
- 238000001694 spray drying Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 150000003278 haem Chemical class 0.000 claims abstract description 4
- 108091005804 Peptidases Proteins 0.000 claims abstract description 3
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 239000002504 physiological saline solution Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 238000001556 precipitation Methods 0.000 claims description 20
- 238000002604 ultrasonography Methods 0.000 claims description 11
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000011017 operating method Methods 0.000 abstract description 7
- 238000011084 recovery Methods 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000000284 extract Substances 0.000 abstract description 3
- 238000004321 preservation Methods 0.000 abstract description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 13
- 229940088598 enzyme Drugs 0.000 description 13
- 238000000605 extraction Methods 0.000 description 9
- 239000011780 sodium chloride Substances 0.000 description 8
- 238000003760 magnetic stirring Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 235000015165 citric acid Nutrition 0.000 description 5
- 239000003814 drug Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 4
- 108090000526 Papain Proteins 0.000 description 4
- 238000013019 agitation Methods 0.000 description 4
- 210000003743 erythrocyte Anatomy 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 125000005909 ethyl alcohol group Chemical group 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 229940055729 papain Drugs 0.000 description 4
- 235000019834 papain Nutrition 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000013049 sediment Substances 0.000 description 4
- 235000010469 Glycine max Nutrition 0.000 description 3
- 244000068988 Glycine max Species 0.000 description 3
- 241001465754 Metazoa Species 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 235000013336 milk Nutrition 0.000 description 3
- 239000008267 milk Substances 0.000 description 3
- 210000004080 milk Anatomy 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- -1 Iron ion Chemical class 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 208000007502 anemia Diseases 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000000050 nutritive effect Effects 0.000 description 2
- 150000004032 porphyrins Chemical class 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 241000282985 Cervus Species 0.000 description 1
- 241000283007 Cervus nippon Species 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 102000001554 Hemoglobins Human genes 0.000 description 1
- 108010054147 Hemoglobins Proteins 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- AQLLBJAXUCIJSR-UHFFFAOYSA-N OC(=O)C[Na] Chemical compound OC(=O)C[Na] AQLLBJAXUCIJSR-UHFFFAOYSA-N 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000002929 anti-fatigue Effects 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 239000003918 blood extract Substances 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000000994 depressogenic effect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000004438 eyesight Effects 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000007661 gastrointestinal function Effects 0.000 description 1
- 102000018146 globin Human genes 0.000 description 1
- 108060003196 globin Proteins 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000011132 hemopoiesis Effects 0.000 description 1
- 230000001900 immune effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 238000011369 optimal treatment Methods 0.000 description 1
- 230000001151 other effect Effects 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 235000019419 proteases Nutrition 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 239000001054 red pigment Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035807 sensation Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 230000029663 wound healing Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D487/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00
- C07D487/22—Heterocyclic 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F15/00—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic Table
- C07F15/02—Iron compounds
- C07F15/025—Iron compounds without a metal-carbon linkage
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Medicinal Preparation (AREA)
Abstract
The present invention provides it is a kind of make by oneself ferroheme preparation method, including：The deer blood after anti-freezing is taken, it is stored refrigerated after centrifugation, washing；After addition physiological saline centrifuges 12 times, 3 10min of absolute ethyl alcohol ultrasonication is added in；Protease is added, heating stirring digests enzyme deactivation after 3 4h, centrifuges heme, washs drying, you can.The preparation method of the ferroheme of converted starch solubilising, includes the following steps：Starch Sodium Octenyl Succinate HI CAP 100, dairy products proteinoid, amino acid, polyethylene glycol are mixed to form solubilizing solution；After the solubilizing solution is mixed with self-control ferroheme, spray drying, you can.The deer blood that the self-control ferroheme of the present invention uses medical value high extracts preparation for raw material, and entire preparation method operating procedure of extracting is simple, and recovery rate is high, and obtained ferroheme quality preservation is high, and this method can be docked directly with production.
Description
Technical field
The present invention relates to the processing preparation field of ferroheme, in particular to a kind of self-control ferroheme and preparation method,
Converted starch solubilising ferroheme and preparation method.
Background technology
Ferroheme is combined by the ferrous ion of porphyrin and a molecule, the ferriporphyrin class compound of composition, in its porphyrin ring
Side chain on carry out the variation in relation to ferroheme analog derivative (in green for a long time and Zhang Lina, 2005).It is myoglobins and blood red
The prothetic group (i.e. activated centre) of albumen, ferroheme are present in the muscle and blood tissues of various animals, have very important
Biochemical physiological function (week is light preferably etc., 2002).Iron ion about 70% in animal body is deposited in the form of in ferroheme structure
In the case where changing in conditions environmental, ferroheme and globin can detach, and ferroheme and pyridine are easy to combine, and form
Hemochromogen substance, in two kinds of protein of myoglobins and hemoglobin, the content of ferroheme accounts for about 3.8% or so (Li Renqiang
Deng 2004).
Iron ion in ferroheme is easy to by the body of people using absorbing, so heme iron has preferable promotion marrow
Hematopoiesis and the therapeutic effect of blood loss anemia are currently known optimal treatment anaemia drugs, thus ferroheme food,
The industries such as medicine, cosmetics, health products, chemical industry have a wide range of applications.
In recent years, the application of ferroheme is increasingly valued by people, by having researched and proposed a variety of extractions
Method, from the point of view of the situation of current various document reports, the method applied to ferroheme extraction is mainly ice acetic acid method, carboxymethyl
Sodium cellulosate (CMC-Na) method, acid acetone method, surfactant method, selection solvent method and enzyme hydrolysis method etc..In the prior art
Although these extracting method techniques it is relatively ripe, there is complex process, production cost is high, recovery rate is low,
The problems such as obtained ferroheme purity is not high limits the marketing dynamics of ferroheme in itself.
In view of this, it is special to propose the present invention.
Invention content
The first object of the present invention is to provide a kind of preparation method for making ferroheme by oneself, special high using medical value
Deer blood extracts preparation for raw material, and entire preparation method operating procedure of extracting is simple, and recovery rate is high, obtained ferroheme product
Matter is higher, and this method can be docked directly with production, suitable for industrialized production, is highly suitable for being widely popularized answering
With.
The second object of the present invention is to provide the self-control ferroheme obtained using above-mentioned preparation method, the self-control ferroheme
Purity itself is high, and of good quality, nutritive value is higher, can be widely used in the industries such as food, medicine.
The third object of the present invention is to provide a kind of preparation method for the ferroheme for being carried out solubilising using converted starch, be led to
After crossing solubilising, ferroheme can be made to form homogeneous phase solution in water, and do not precipitated for a long time, improve ferroheme steady in itself
It is qualitative.
The fourth object of the present invention is to provide the ferroheme of converted starch solubilising that above-mentioned preparation method obtains, dissolve
Degree significantly increases, and more feasible scheme is provided for the follow-up downstream product for preparing.
In order to realize the above-mentioned purpose of the present invention, spy uses following technical scheme：
The present invention provides a kind of preparation methods for making ferroheme by oneself, include the following steps：
(A) the deer blood after anti-freezing is taken, it is stored refrigerated after centrifugation, washing；
(B) after addition physiological saline centrifuges 1-2 times, absolute ethyl alcohol ultrasonication 3-10min is added in；
(C) protease is added, heating stirring digests enzyme deactivation after 3-4h, centrifuges heme, washs drying, you can.
In the prior art, the application of ferroheme is increasingly valued by people, by having researched and proposed a variety of extractions
Method, from the point of view of the situation of current various document reports, the method applied to ferroheme extraction is mainly ice acetic acid method, carboxylic first
Base sodium cellulosate (CMC-Na) method, acid acetone method, surfactant method, selection solvent method and enzyme hydrolysis method etc..The prior art
Although these extracting method techniques in are relatively ripe, and there is complex process, production cost height, recovery rates
Low, the problems such as obtained ferroheme purity is not high, also ferroheme itself not soluble in water are also to limit what it was further applied
Importance, and then limit the marketing dynamics of ferroheme in itself.
The present invention in order to solve the above technical problems, provide it is a kind of make by oneself ferroheme preparation method, carried from deer blood
Ferroheme is taken, blood of the deer blood for animal in deer family sika deer or red deer, is traditional rare Chinese medicine.A large amount of zoopery now
Clinical research show deer blood have it is antifatigue, help strong, immunological regulation, beauty, enrich blood, beneficial to wound healing, tonifying kidney and benefiting sperm,
Radioresistance, anti-aging, Central nervous depressant also have been reported that the oral deer blood of discovery has improvement to remember, improve gastrointestinal function
And improve sleep, improve eyesight, adjust blood pressure, elegant wet one's whistle and other effects.Therefore in view of the very high medical value of deer blood, by deer blood
There is the meaning of reality as raw material extraction ferroheme.
And by comparing the control of each operating parameter suitable within the scope of in the extraction preparation process of the present invention,
So that the ferroheme purity that is prepared is high, when extraction, also can significantly improve recovery rate, particularly with the addition of absolute ethyl alcohol ultrasound
PH value control of solution after broken operating parameter control and addition enzyme etc. is that entire extraction operation needs in the process
Want the condition of stringent control.
Preferably, in the step (B), the temperature of ultrasonication is controlled at 28 DEG C hereinafter, ultrasonic power is 400-
600Hz, broken 2-3s stops 1-2s during ultrasonication, so repeatedly 2-3 times.Ultrasonication the step is entirely to extract
The step of stringent control is needed in journey, operation temperature, operating time and ultrasonic power etc., is required to control in suitable range
Interior, the time of ultrasonication is unsuitable long, because if the broken time is too long, can release the height that a large amount of sound wave generates moment
Temperature so that the protein heat denatured in ferroheme forms rock-steady structure, and ferroheme can cause to be difficult to discharge, certain Ultrasonic Pulverization
If temperature Tai Gao be also unfavorable, therefore be preferably controlled in less than 28 DEG C.
In addition, preferably a certain amount of water is added to be mixed with absolute ethyl alcohol before ultrasonication, the volume ratio of water and absolute ethyl alcohol
Control is at (20-30)：Between 1.Because appropriate plus water can reduce Premeabilisation of cells pressure so that haemocyte is easier to absorb water broken
Split, so as to improve the percentage of damage of haemocyte, if but this dosage continue increase may can not further improve haemocyte
Breakage rate, it is therefore desirable to control in suitable ratio range.
Preferably, in the step (C) of the present invention, the temperature of enzymolysis is controlled between 55-60 DEG C, the temperature control of enzyme deactivation
Between 95-96 DEG C.
In enzymolysis process, hydrolysis temperature and pH value that each enzyme has comparison suitable, in conjunction with handled enzyme
Object is solved, needs to control the operating conditions such as suitable temperature and pH value.
Preferably, the time control of enzyme deactivation is between 12-16min；
Preferably, the centrifugation rate of centrifugation is controlled between 7000-9000rpm；
Preferably, the step of centrifugation includes：Supernatant is removed in centrifugation, precipitates and is dissolved with NaOH to detach ferroheme,
It centrifuges again and removes precipitation, adding citric acid precipitates to detach ferroheme.
Preferably, the control of finally dried temperature is between 40-60 DEG C, and the dry time is more than for 24 hours.
By the way that the solution of the present invention is constantly optimized, the step of follow-up enzyme deactivation and isolated ferroheme also most
Good above-mentioned preferred embodiment according to the invention is operated, and the quality that could cause final ferroheme obtained of the invention is more excellent
It is different.
The present invention additionally provides in addition to providing a kind of self-control ferroheme and prepares converted starch solubilising using above-mentioned ferroheme
Ferroheme method, include the following steps：
(A) starch Sodium Octenyl Succinate HI-CAP 100, dairy products proteinoid, amino acid, polyethylene glycol are mixed into shape
Into solubilizing solution；
(B) after the solubilizing solution and the self-control ferroheme being dissolved in NaOH being mixed, spray drying, i.e.,
It can.
The present invention is by will be after the solubilizing solution containing converted starch mixes with self-control ferroheme, the blood that is spray-dried
Red pigment dissolubility and stability are significantly improved, and expand the application range of ferroheme.Solubilizing solution and ferroheme it
Between be by the way that solubilized complex and ferroheme are coordinated after, so as to increase the solubility of ferroheme.
Preferably, in order to enable the solubilizing effect between each component after compatibility is more excellent, in solubilizing solution of the invention,
In terms of mass fraction, starch Sodium Octenyl Succinate HI-CAP 100 30-40 part, 1-3 parts of dairy products proteinoid, amino acid 6-8
Part, 70-80 parts of polyethylene glycol.
More preferably, in the step (B), the inlet temperature of spray drying is controlled between 120-150 DEG C, outlet temperature control
System is between 70-90 DEG C.
Preferably, in the step (B), the flow control of spray drying is between 4-6ml/min, preferably 5ml/min.
There is good solubilizing effect using the ferroheme of converted starch solubilising that above-mentioned preparation method is prepared, can make
Ferroheme forms homogeneous phase solution in water, and does not precipitate for a long time.
Compared with prior art, beneficial effects of the present invention are：
(1) the deer blood for using medical value high using the self-control ferroheme spy of the present invention extracts preparation as raw material,
Entire extraction preparation method operating procedure is simple, and recovery rate is high, and obtained ferroheme quality preservation is high, this method can directly with
Production is docked, suitable for industrialized production, highly suitable for wide popularization and application；
(2) self-control ferroheme itself purity height of the invention, of good quality, nutritive value is higher, can be widely used in
The industries such as food, medicine；
(3) the present invention also provides a kind of ferroheme of converted starch solubilising, solubility significantly increases, and is prepared to be follow-up
Downstream product provides more feasible scheme.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person, the condition suggested according to normal condition or manufacturer carry out.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
Embodiment 1
The ferroheme preparation method of converted starch solubilising is as follows：
1) the deer blood after anti-freezing is taken, 3000rpm centrifugations, precipitation haemocyte is washed with 0.9wt%NaCl, 3000rpm centrifugations
It is 2 times, stored refrigerated.
2) red blood cell 250ml is taken, adds 10ml 1mol NaCl, 10-15ml absolute ethyl alcohols, the broken born of the same parents 10min of ultrasound in ice bath,
Power 400Hz, ultrasound open 2s, close 1s, and at 28 DEG C hereinafter, adding in papain 3.0g, magnetic stirring apparatus dissolves control temperature,
55 DEG C of enzymolysis 3h, 95 DEG C of enzyme deactivation 12min；
3) 7000rpm centrifuges 5min, takes precipitation plus 0.1mol NaOH dissolving ferrohemes, and 9000rpm centrifugation 5min take
Clear liquid, precipitation plus 0.1mol NaOH washing 8000rpm centrifugation 5min, take supernatant, each supernatant are merged, sink
It forms sediment plus 0.1mol citric acids precipitates ferroheme to pH=3.8,8000rpm centrifugation 15min take precipitation, 40 DEG C of dryings obtain for 24 hours
Make ferroheme by oneself；
4) solubilizing solution is prepared：100 30g of starch Sodium Octenyl Succinate HI-CAP, dairy products proteinoid 3g, amino acid
8g, polyethylene glycol 70g；
By above-mentioned ferroheme 0.35g, 0.1mol NaOH 5mL dissolvings are added in, adds in above-mentioned solubilizing solution, is placed in magnetic force
Blender gradually instills the solution of ferroheme, until being completely dispersed under agitation；
5) it is spray-dried：120 DEG C of inlet temperature, 70 DEG C of outlet temperature, flow velocity 4ml/min.Powder is sprayed, can quickly be divided
It dissipates in water, forms homogeneous phase solution, at room temperature, do not precipitated in 12h.
Embodiment 2
The ferroheme preparation method of converted starch solubilising is as follows：
1) the deer blood after anti-freezing is taken, 3000rpm centrifugations, precipitation haemocyte is washed with 0.9wt%NaCl, 3000rpm centrifugations
It is 2 times, stored refrigerated.
2) red blood cell 250ml is taken, adds 10ml 1mol NaCl, 10-15ml absolute ethyl alcohols, the broken born of the same parents 5min of ultrasound in ice bath,
Power 600Hz, ultrasound open 3s, close 2s, and at 28 DEG C hereinafter, adding in papain 3.0g, magnetic stirring apparatus dissolves control temperature,
60 DEG C of enzymolysis 4h, 96 DEG C of enzyme deactivation 16min；
3) 9000rpm centrifuges 5min, takes precipitation plus 0.1mol NaOH dissolving ferrohemes, and 7000rpm centrifugation 5min take
Clear liquid, precipitation plus 0.1mol NaOH washing 8000rpm centrifugation 5min, take supernatant, each supernatant are merged, sink
It forms sediment plus 0.1mol citric acids precipitates ferroheme to pH=3.8,8000rpm centrifugation 15min take precipitation, 60 DEG C of dryings obtain for 24 hours
Make ferroheme by oneself；
4) solubilizing solution is prepared：100 40g of starch Sodium Octenyl Succinate HI-CAP, dairy products proteinoid 1g, amino acid
6g, polyethylene glycol 80g；By above-mentioned ferroheme 0.35g, 0.1mol NaOH 5mL dissolvings are added in, are added in above-mentioned solubilizing solution,
Magnetic stirring apparatus is placed in, the solution of ferroheme is gradually instilled under agitation, until being completely dispersed；
5) it is spray-dried：150 DEG C of inlet temperature, 90 DEG C of outlet temperature, flow velocity 6ml/min.Powder is sprayed, can quickly be divided
It dissipates in water, forms homogeneous phase solution, at room temperature, do not precipitated in 12h.
Embodiment 3
The ferroheme preparation method of converted starch solubilising is as follows：
1) the deer blood after anti-freezing is taken, 3000rpm centrifugations, precipitation haemocyte is washed with 0.9wt%NaCl, 3000rpm centrifugations
It is 2 times, stored refrigerated.
2) take red blood cell 250ml, add 10ml 1mol NaCl, 10-15ml absolute ethyl alcohols, and add in deionized water, go from
The volume of sub- water is 20 times of absolute ethyl alcohol volume, and the broken born of the same parents 3min of ultrasound, power 500Hz, ultrasound open 3s in ice bath, closes 2s, control
Temperature processed is at 28 DEG C hereinafter, add in papain 3.0g, and magnetic stirring apparatus dissolving, 58 DEG C digest 4h, 96 DEG C of enzyme deactivation 14min；
3) 9000rpm centrifuges 5min, takes precipitation plus 0.1mol NaOH dissolving ferrohemes, and 7000rpm centrifugation 5min take
Clear liquid, precipitation plus 0.1mol NaOH washing 8000rpm centrifugation 5min, take supernatant, each supernatant are merged, sink
It forms sediment plus 0.1mol citric acids precipitates ferroheme to pH=3.8,8000rpm centrifugation 15min take precipitation, 60 DEG C of dryings obtain for 24 hours
Make ferroheme by oneself；
4) solubilizing solution is prepared：100 35g of starch Sodium Octenyl Succinate HI-CAP, dairy products proteinoid 2g, amino acid
7g, polyethylene glycol 75g；By above-mentioned ferroheme 0.35g, 0.1mol NaOH 5mL dissolvings are added in, are added in above-mentioned solubilizing solution,
Magnetic stirring apparatus is placed in, the solution of ferroheme is gradually instilled under agitation, until being completely dispersed；
5) it is spray-dried：140 DEG C of inlet temperature, 80 DEG C of outlet temperature, flow velocity 5ml/min.Powder is sprayed, can quickly be divided
It dissipates in water, forms homogeneous phase solution, at room temperature, do not precipitated in 12h.
Embodiment 4
The ferroheme preparation method of converted starch solubilising is as follows：
1) the deer blood after anti-freezing is taken, 4000rpm centrifugations, precipitation haemocyte is washed with 0.9wt%NaCl, 3000rpm centrifugations
It is 2 times, stored refrigerated.
2) take red blood cell 250ml, add 10ml 1mol NaCl, 10-15ml absolute ethyl alcohols, and add in deionized water, go from
The volume of sub- water is 30 times of absolute ethyl alcohol volume, and the broken born of the same parents 6min of ultrasound, power 550Hz, ultrasound open 3s in ice bath, closes 2s, control
Temperature processed adds in papain 3.0g, magnetic stirring apparatus dissolving, 58 DEG C of enzymolysis 4h, 96 DEG C of enzyme deactivation 15min at 25 DEG C；
3) 9000rpm centrifuges 5min, takes precipitation plus 0.1mol NaOH dissolving ferrohemes, and 7000rpm centrifugation 5min take
Clear liquid, precipitation plus 0.1mol NaOH washing 8000rpm centrifugation 5min, take supernatant, each supernatant are merged, sink
It forms sediment plus 0.1mol citric acids precipitates ferroheme and take precipitation to pH=3.8,8000rpm centrifugation 15min, 60 DEG C of dryings obtain certainly for 24 hours
Ferroheme processed；
4) solubilizing solution is prepared：100 36g of starch Sodium Octenyl Succinate HI-CAP, dairy products proteinoid 2.5g, amino
Sour 7g, polyethylene glycol 75g；By above-mentioned ferroheme 0.35g, 0.1mol NaOH 5mL dissolvings are added in, add above-mentioned solubilizing solution
In, magnetic stirring apparatus is placed in, the solution of ferroheme is gradually instilled under agitation, until being completely dispersed；
5) it is spray-dried：130 DEG C of inlet temperature, 85 DEG C of outlet temperature, flow velocity 5ml/min.Powder is sprayed, can quickly be divided
It dissipates in water, forms homogeneous phase solution, at room temperature, do not precipitated in 12h.
Comparative example 1
Remaining operating procedure is consistent with embodiment 4, and only the ultrasonication time in step 2) is 15min, is finally found
It is not precipitated in 12h.
Comparative example 2
Remaining operating procedure is consistent with embodiment 4, and only the ultrasonication time in step 2) is 1min, is finally found
It is not precipitated in 12h.
Comparative example 3
Remaining operating procedure is consistent with embodiment 4, only in solubilizing solution, only starch Sodium Octenyl Succinate HI-CAP
100, start to generate precipitation after finally finding 8h.
Comparative example 4
Remaining operating procedure is consistent with embodiment 4, only in solubilizing solution, does not add starch Sodium Octenyl Succinate HI-
CAP 100 starts to generate precipitation after finally finding 6h.
Experimental example 1
The extracted amount of self-control ferroheme that 1-4 of the embodiment of the present invention and comparative example 1-3 is prepared is compared, it is blood red
It is as shown in table 1 below specifically to extract obtained ferroheme quality by the quantification of 250ml of cell：
1 product quality test result of table
| Group | Extract obtained ferroheme purity (%) |
| Embodiment 1 | 31.5 |
| Embodiment 2 | 32.0 |
| Embodiment 3 | 35.4 |
| Embodiment 4 | 29.3 |
| Comparative example 1 | 20.3 |
| Comparative example 2 | 16.5 |
| Comparative example 3 | 18.1 |
As can be seen that if some operating parameters during preparing ferroheme are not controlled in this hair from upper table 1
In the range of bright embodiment requirement, then can have a certain impact to recovery rate.In addition, from upper table it can also be seen that
A certain amount of water is added in be advantageous for extracted amount.
Experimental example 2
Ferroheme after the last solubilisings of the embodiment of the present invention 1-4 and comparative example 1-5, which is added to be made in soya-bean milk, to be had
The soya-bean milk finished product of healthcare function, solubility property is compared, is specifically shown in the following table 2：
2 solubility property of table compares
| Group | Dissolution rate | State after dissolving |
| Embodiment 1 | 100% | Uniform solution is formed, without any particle |
| Embodiment 2 | 100% | Uniform solution is formed, without any particle |
| Embodiment 3 | 100% | Uniform solution is formed, without any particle |
| Embodiment 4 | 100% | Uniform solution is formed, without any particle |
| Comparative example 1 | 99% | Uniform solution is formed, without any particle |
| Comparative example 2 | 99% | Uniform solution is formed, without any particle |
| Comparative example 3 | 99% | Uniform solution is formed, without any particle |
| Comparative example 4 | 90% | There is granular sensation, do not form uniform solution |
The embodiment of the present invention, which is can be seen that, from the data in above-mentioned table eventually passes through solubilized ferroheme solubility higher,
Uniform solution can be formed by being added in soya-bean milk.
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that without departing substantially from the present invention's
Many other change and modification can be made in the case of spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.
Claims (10)
1. a kind of preparation method for making ferroheme by oneself, which is characterized in that include the following steps：
(A) the deer blood after anti-freezing is taken, it is stored refrigerated after centrifugation, washing；
(B) after addition physiological saline centrifuges 1-2 times, absolute ethyl alcohol ultrasonication 3-10min is added in；
(C) protease is added, heating stirring digests enzyme deactivation after 3-4h, centrifuges heme, washs drying, you can.
2. the preparation method of self-control ferroheme according to claim 1, which is characterized in that in the step (B), ultrasound is broken
Broken temperature is controlled at 28 DEG C hereinafter, ultrasonic power is 400-600Hz, and broken 2-3s stops 1-2s during ultrasonication, so
2-3 times repeatedly.
3. the preparation method of self-control ferroheme according to claim 1, which is characterized in that in the step (B), ultrasound is broken
Before broken plus water is mixed with absolute ethyl alcohol, and the volume ratio of water and absolute ethyl alcohol is controlled at (20-30)：Between 1.
4. the preparation method of self-control ferroheme according to claim 1, which is characterized in that in the step (C), enzymolysis
Temperature is controlled between 55-60 DEG C, and the temperature of enzyme deactivation is controlled between 95-96 DEG C；
Preferably, the time control of enzyme deactivation is between 12-16min；
Preferably, the centrifugation rate of centrifugation is controlled between 7000-9000rpm；
Preferably, the step of centrifugation includes：Supernatant is removed in centrifugation, precipitates and is dissolved to detach ferroheme with NaOH, then from
The heart removes precipitation, and adding citric acid precipitates to detach ferroheme；
Preferably, the control of finally dried temperature is between 40-60 DEG C, and the dry time is more than for 24 hours.
5. the self-control ferroheme that claim 1-4 any one of them preparation methods are prepared.
6. the method that the self-control ferroheme of claim 5 prepares the ferroheme of converted starch solubilising, which is characterized in that including as follows
Step：
(A) starch Sodium Octenyl Succinate HI-CAP 100, dairy products proteinoid, amino acid, polyethylene glycol are mixed to form increasing
Solution；
(B) after the solubilizing solution and the self-control ferroheme being dissolved in NaOH being mixed, spray drying, you can.
7. the method for the ferroheme according to claim 6 for preparing converted starch solubilising, which is characterized in that the step
(A) in, in terms of mass fraction, starch Sodium Octenyl Succinate HI-CAP 100 30-40 part, 1-3 parts of dairy products proteinoid, ammonia
6-8 parts of base acid, 70-80 parts of polyethylene glycol.
8. the method for the ferroheme according to claim 6 for preparing converted starch solubilising, which is characterized in that the step
(B) in, the inlet temperature of spray drying is controlled between 120-150 DEG C, and outlet temperature is controlled between 70-90 DEG C.
9. the method for the ferroheme according to claim 6 for preparing converted starch solubilising, which is characterized in that the step
(B) in, the flow control of spray drying is between 4-6ml/min, preferably 5ml/min.
10. the ferroheme of converted starch solubilising that claim 6-9 any one of them preparation methods are prepared.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810034502.4A CN108129485A (en) | 2018-01-15 | 2018-01-15 | Make ferroheme and preparation method, converted starch solubilising ferroheme and preparation method by oneself |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810034502.4A CN108129485A (en) | 2018-01-15 | 2018-01-15 | Make ferroheme and preparation method, converted starch solubilising ferroheme and preparation method by oneself |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108129485A true CN108129485A (en) | 2018-06-08 |
Family
ID=62400549
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810034502.4A Pending CN108129485A (en) | 2018-01-15 | 2018-01-15 | Make ferroheme and preparation method, converted starch solubilising ferroheme and preparation method by oneself |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108129485A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112094876A (en) * | 2020-09-25 | 2020-12-18 | 中国农业科学院特产研究所 | Preparation method of hemin and composition prepared by same |
| CN113332443A (en) * | 2021-05-09 | 2021-09-03 | 湖北美田农业生物技术有限公司 | Water-soluble rosemary antioxidant and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1252279A (en) * | 1999-08-30 | 2000-05-10 | 许德余 | Soluble heme and its preparation process and hematic composite with it |
| CN102887947A (en) * | 2012-09-24 | 2013-01-23 | 南昌大学 | Process for producing micromolecule hemepeptide, heme iron and plasma proteins by using duck blood as raw material |
| CN102994584A (en) * | 2012-09-24 | 2013-03-27 | 南昌大学 | Method for producing heme iron by using duck blood |
| CN104098579A (en) * | 2014-06-04 | 2014-10-15 | 黑龙江省野生动物研究所 | Method for preparation of deer blood heme by ultrasound and enzymolysis technologies |
-
2018
- 2018-01-15 CN CN201810034502.4A patent/CN108129485A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1252279A (en) * | 1999-08-30 | 2000-05-10 | 许德余 | Soluble heme and its preparation process and hematic composite with it |
| CN102887947A (en) * | 2012-09-24 | 2013-01-23 | 南昌大学 | Process for producing micromolecule hemepeptide, heme iron and plasma proteins by using duck blood as raw material |
| CN102994584A (en) * | 2012-09-24 | 2013-03-27 | 南昌大学 | Method for producing heme iron by using duck blood |
| CN104098579A (en) * | 2014-06-04 | 2014-10-15 | 黑龙江省野生动物研究所 | Method for preparation of deer blood heme by ultrasound and enzymolysis technologies |
Non-Patent Citations (1)
| Title |
|---|
| 秦凤贤等，: "梅花鹿血血红素的制备探究", 《食品安全导刊》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112094876A (en) * | 2020-09-25 | 2020-12-18 | 中国农业科学院特产研究所 | Preparation method of hemin and composition prepared by same |
| CN113332443A (en) * | 2021-05-09 | 2021-09-03 | 湖北美田农业生物技术有限公司 | Water-soluble rosemary antioxidant and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Yu et al. | Effects of high-pressure homogenization on functional properties and structure of mussel (Mytilus edulis) myofibrillar proteins | |
| Zhao et al. | Stability of lutein encapsulated whey protein nano-emulsion during storage | |
| CN108070629B (en) | Industrial production method of hemp protein oligopeptide | |
| Linares et al. | Ultrasound-assisted extraction of natural pigments from food processing by-products: A review | |
| WO2020248947A1 (en) | Walnut oligopeptide powder, manufacturing method therefor, and use thereof | |
| KR20120052991A (en) | Cosmetic composition for the treatment of acne comprising a peptide extract of schizandra | |
| WO2022242386A1 (en) | Bifunctional bean-derived polypeptide and preparation method therefor | |
| CN110037296A (en) | A kind of preparation method of lactalbumin base ginsenoside nanoemulsions | |
| CN108129485A (en) | Make ferroheme and preparation method, converted starch solubilising ferroheme and preparation method by oneself | |
| JP2019198260A (en) | Method for producing eggshell membrane protein soluble product, and composition containing eggshell membrane protein soluble product | |
| Murtaza et al. | Conventional and novel technologies in the production of dairy bioactive peptides | |
| CN108741100B (en) | Preparation method and application of chelated iron donkey-hide gelatin glycopeptide | |
| CN108743500A (en) | Not only oral administration but also can external application beautifying face and moistering lotion compound peptide functional food and preparation method thereof | |
| Li et al. | Effects of ultrasonic treatment on the structural and functional properties of cactus (Opuntia ficus-indica) seed protein | |
| JP4456585B2 (en) | Cell activator, collagen production promoter, whitening agent, antioxidant, anti-inflammatory agent, aromatase activity promoter, protease activity promoter, topical skin preparation and food | |
| RU2604137C2 (en) | Method of producing biologically active concentrate of raw antlers (options) | |
| JP5380649B2 (en) | Milk component hydrolyzate | |
| US6379719B1 (en) | Use of at least one protein fraction extracted from Hibiscus esculentus seeds and cosmetic composition containing such a fraction | |
| CN113057250B (en) | Preparation method of functional digestible micelle casein powder | |
| CN105779540A (en) | Blueberry small molecular peptide composition, as well as extracting method and application thereof | |
| KR100970371B1 (en) | Method of extracting porcine placenta, health food and cosmetic comprising the extract | |
| CN108685828A (en) | A kind of extracting method of placental hormone | |
| CN105943434B (en) | A kind of facial cleanser and preparation method thereof for treating acne | |
| CN107418992A (en) | A kind of bone peptide extracting method | |
| JP2002284632A (en) | Extinction substance for superoxide anion extracted from sake lees as effective component |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180608 |