CN102198152B - Injection containing astragalus polysaccharide-iron complex for swine, and preparation method thereof - Google Patents
Injection containing astragalus polysaccharide-iron complex for swine, and preparation method thereof Download PDFInfo
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- CN102198152B CN102198152B CN 201110128690 CN201110128690A CN102198152B CN 102198152 B CN102198152 B CN 102198152B CN 201110128690 CN201110128690 CN 201110128690 CN 201110128690 A CN201110128690 A CN 201110128690A CN 102198152 B CN102198152 B CN 102198152B
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- 241001061264 Astragalus Species 0.000 title claims abstract description 88
- 235000006533 astragalus Nutrition 0.000 title claims abstract description 88
- 210000004233 talus Anatomy 0.000 title claims abstract description 88
- 238000002347 injection Methods 0.000 title claims abstract description 62
- 239000007924 injection Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 229940078042 polysaccharide iron complex Drugs 0.000 title abstract 5
- 241000282898 Sus scrofa Species 0.000 title abstract 4
- 150000004676 glycans Chemical class 0.000 claims abstract description 83
- 229920001282 polysaccharide Polymers 0.000 claims abstract description 82
- 239000005017 polysaccharide Substances 0.000 claims abstract description 82
- 150000002505 iron Chemical class 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000000605 extraction Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 91
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 84
- 239000007788 liquid Substances 0.000 claims description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000012153 distilled water Substances 0.000 claims description 23
- 238000001914 filtration Methods 0.000 claims description 23
- 238000002604 ultrasonography Methods 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000000706 filtrate Substances 0.000 claims description 22
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 22
- 239000002244 precipitate Substances 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 230000001476 alcoholic effect Effects 0.000 claims description 18
- 239000003480 eluent Substances 0.000 claims description 18
- 239000000284 extract Substances 0.000 claims description 18
- 239000003513 alkali Substances 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 239000009636 Huang Qi Substances 0.000 claims description 13
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 12
- 239000011347 resin Substances 0.000 claims description 12
- 229920005989 resin Polymers 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 11
- 229960002413 ferric citrate Drugs 0.000 claims description 11
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical group Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 11
- NPFOYSMITVOQOS-UHFFFAOYSA-K iron(III) citrate Chemical compound [Fe+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NPFOYSMITVOQOS-UHFFFAOYSA-K 0.000 claims description 11
- 238000001291 vacuum drying Methods 0.000 claims description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- 239000008187 granular material Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 239000012266 salt solution Substances 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 9
- DHCLVCXQIBBOPH-UHFFFAOYSA-N Glycerol 2-phosphate Chemical compound OCC(CO)OP(O)(O)=O DHCLVCXQIBBOPH-UHFFFAOYSA-N 0.000 claims description 9
- FRHBOQMZUOWXQL-UHFFFAOYSA-L ammonium ferric citrate Chemical compound [NH4+].[Fe+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O FRHBOQMZUOWXQL-UHFFFAOYSA-L 0.000 claims description 9
- 229960004642 ferric ammonium citrate Drugs 0.000 claims description 9
- 229940046257 glyceryl phosphate Drugs 0.000 claims description 9
- 239000004313 iron ammonium citrate Substances 0.000 claims description 9
- 235000000011 iron ammonium citrate Nutrition 0.000 claims description 9
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 9
- LHOWRPZTCLUDOI-UHFFFAOYSA-K iron(3+);triperchlorate Chemical compound [Fe+3].[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O LHOWRPZTCLUDOI-UHFFFAOYSA-K 0.000 claims description 9
- 230000000274 adsorptive effect Effects 0.000 claims description 6
- 239000012141 concentrate Substances 0.000 claims description 6
- 239000002609 medium Substances 0.000 claims description 6
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 238000012869 ethanol precipitation Methods 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 239000001509 sodium citrate Substances 0.000 claims description 5
- 241000894007 species Species 0.000 claims description 5
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 5
- 229940038773 trisodium citrate Drugs 0.000 claims description 5
- 239000008215 water for injection Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 230000004083 survival effect Effects 0.000 abstract description 7
- 230000036039 immunity Effects 0.000 abstract description 3
- 235000016709 nutrition Nutrition 0.000 abstract description 3
- 241000282887 Suidae Species 0.000 abstract 2
- 239000004615 ingredient Substances 0.000 abstract 1
- 229910052742 iron Inorganic materials 0.000 description 11
- MVZXTUSAYBWAAM-UHFFFAOYSA-N iron;sulfuric acid Chemical compound [Fe].OS(O)(=O)=O MVZXTUSAYBWAAM-UHFFFAOYSA-N 0.000 description 11
- 102000001554 Hemoglobins Human genes 0.000 description 6
- 108010054147 Hemoglobins Proteins 0.000 description 6
- 239000013589 supplement Substances 0.000 description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 5
- 241001071864 Lethrinus laticaudis Species 0.000 description 4
- 239000008280 blood Substances 0.000 description 4
- 210000004369 blood Anatomy 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 229920002307 Dextran Polymers 0.000 description 3
- 201000010099 disease Diseases 0.000 description 3
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005227 gel permeation chromatography Methods 0.000 description 3
- -1 hydroxy ferrum Chemical compound 0.000 description 3
- 206010025482 malaise Diseases 0.000 description 3
- 208000015710 Iron-Deficiency Anemia Diseases 0.000 description 2
- 231100000111 LD50 Toxicity 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 239000011790 ferrous sulphate Substances 0.000 description 2
- 235000003891 ferrous sulphate Nutrition 0.000 description 2
- 238000010255 intramuscular injection Methods 0.000 description 2
- 239000007927 intramuscular injection Substances 0.000 description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 2
- 238000002372 labelling Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 241001533384 Circovirus Species 0.000 description 1
- 102000018832 Cytochromes Human genes 0.000 description 1
- 108010052832 Cytochromes Proteins 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 241000606807 Glaesserella parasuis Species 0.000 description 1
- 206010053759 Growth retardation Diseases 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 241000699670 Mus sp. Species 0.000 description 1
- 102000036675 Myoglobin Human genes 0.000 description 1
- 108010062374 Myoglobin Proteins 0.000 description 1
- 206010030113 Oedema Diseases 0.000 description 1
- 206010033546 Pallor Diseases 0.000 description 1
- 206010034107 Pasteurella infections Diseases 0.000 description 1
- 102000003992 Peroxidases Human genes 0.000 description 1
- 241000505673 Scintilla Species 0.000 description 1
- 241000191940 Staphylococcus Species 0.000 description 1
- QRSFFHRCBYCWBS-UHFFFAOYSA-N [O].[O] Chemical compound [O].[O] QRSFFHRCBYCWBS-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000007059 acute toxicity Effects 0.000 description 1
- 231100000403 acute toxicity Toxicity 0.000 description 1
- 208000007502 anemia Diseases 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000010241 blood sampling Methods 0.000 description 1
- 230000037396 body weight Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 206010061428 decreased appetite Diseases 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 208000001848 dysentery Diseases 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 229960004887 ferric hydroxide Drugs 0.000 description 1
- 239000007952 growth promoter Substances 0.000 description 1
- 231100000001 growth retardation Toxicity 0.000 description 1
- 208000033065 inborn errors of immunity Diseases 0.000 description 1
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
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- 231100000252 nontoxic Toxicity 0.000 description 1
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- 150000004804 polysaccharides Polymers 0.000 description 1
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- 230000000630 rising effect Effects 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
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Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to an injection containing an astragalus polysaccharide-iron complex for swine, comprising the following active components in parts by weight: 15-50 parts of astragalus polysaccharide and 10-45 parts of iron salt. The invention also relates to a preparation method of the injection containing the astragalus polysaccharide-iron complex for swine, comprising the steps of: extraction of the astragalus polysaccharide, preparation of the astragalus polysaccharide-iron complex and preparation of the finished products of the injection. The injection containing the astragalus polysaccharide-iron complex for swine has stable quality, lower production cost and a simple manufacture process, can effectively enhance the body immunity, improve the survival rate of baby pigs and enable the baby pigs to have more balanced and thorough nutritional ingredients, and is safe and reliable.
Description
Technical field
The invention belongs to pig and use iron supplement agent field, especially a kind of pig injection and preparation method thereof that contains astragalus polysaccharides ferrum.
Background technology
Iron deficiency anemia is a kind of common disease of newborn 2-4 piglet in age in week.The reserves of ferrum namely have been consumed as far back as the 3-4 age in days in the newborn piglet body, usually need artificial iron supplement, this is because the newborn piglet growth promoter is rapid, requirement to ferrum sharply increases, and in initial several weeks, the ferrum storage capacity in the newborn piglet body is few, only be 54mg, and iron-holder is about 1.3mg/L in the sow milk, and only can for every piglet provides about 1mg ferrum, therefore not satisfy piglet far away to the 15mg day requirement of ferrum every day.And piglet growth is faster, and it is faster that the ferrum reserves consume, and the sickness rate of anemia is also just higher.If untimely iron supplement can bring many harm to piglet: 1. can not form hemoglobin, Myoglobin, cytochrome enzyme and multiple peroxidase, thereby affect the conveying of endotrophic material; 2. content of hemoglobin is low, and blood is thin, and it is low to take the oxygen oxygen delivery capacity, causes biological organs depleted; 3. growth retardation, the sickness rate such as dysentery, edema, white muscle disease raise, and are disorderly thick by hair, skin and mucosal pallor, inappetence; 4 physiology defence function descends, hypoimmunity, the viral diseases such as reproductive and respiratory syndrome, circovirus disease, pseudorabies easily occur, also so that the sickness rate of the conditionality pathogenic bacterium such as escherichia coli, haemophilus parasuis, pasteurellosis bacillus, staphylococcus rising, cause huge economic loss, seriously restricted the development of China's pig industry.Be applied at present clinical piglet iron supplement product and be mainly ferrous sulfate and iron dextran etc.The absorbance of ferrous sulfate is lower, and the iron supplement effect is relatively poor; Iron dextran is relatively better to the therapeutic effect of piglet iron deficiency anemia, play very important effect for improving the pig level of production, but the synthetic of iron dextran is a very complicated process, the ferric hydroxide of nascent state and the complex reaction of scintilla dextran molecule, this complex reaction is very unstable, is subjected to pH value and the FeCl of reaction system
3The impact of solution concentration is larger, and product yield and quality are all not ideal enough, in addition, the dextran price is expensive, cause production cost higher, and iron dextran often needs deep intramuscular injection, cause serious stress, affected to a certain extent its clinical practice.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of pig injection that contains astragalus polysaccharides ferrum is provided, and this injection steady quality, production cost are lower, effectively enhancing human body immunity power, improve the piglet survival rate, make its nutritional labeling more balanced comprehensively, processing technology is simple.
Another object of the present invention is to provide a kind of pig that contains astragalus polysaccharides ferrum preparation method of injection.
The present invention is achieved by the following technical solutions:
A kind of pig injection that contains astragalus polysaccharides ferrum, the active component of its injection and ratio of weight and number thereof are: astragalus polysaccharides 15-50 part; Iron salt 10-45 part.
And described iron salt is ferric chloride, ferric nitrate, ferric citrate, iron acetate, ferric perchlorate, ferric ammonium citrate, ferric ammonium nitrate or ferric glycerylphosphate wherein a kind of.
A kind of pig that contains astragalus polysaccharides ferrum preparation method of injection, it is characterized in that: the step of this preparation method is:
(1) extraction of astragalus polysaccharides: get the Radix Astragali and with the distilled water of weight ratio 1: 1.5～3 Radix Astragali is carried out preimpregnation and spend the night and obtain presoak, the concentration that the weight such as adds in the presoak is 35%～70% alcoholic solution, then use microwave treatment 3 times, 20～60s/ time, obtain microwave-assisted and extract liquid; Extract to microwave-assisted that to add concentration by weight 1: 5～10 in the liquid be 35%～70% alcoholic solution, behind adjust pH to 3～5, extract twice, 15～40min/ time with Ultrasound Instrument again, temperature is controlled to be 20 ℃, obtains the Ultrasound Instrument extracting solution; Behind the Ultrasound Instrument extracting liquid filtering, filtrate for later use, to colourless, washing liquid and filtrate merge the residue of filtration with the distilled water cyclic washing, and the concentrated concentrated solution that obtains adopts macroporous adsorptive resins to separate after concentrated solution filters, and gets separating medium; And colourless to eluent with distilled water eluting resin column, collect eluent, merge separating medium and eluent and concentrate, then adding 3 times of amount concentration is that 75% alcoholic solution carries out precipitate with ethanol, and room temperature leaves standstill sucking filtration behind 8～15h, and vacuum drying gets astragalus polysaccharides;
(2) preparation of astragalus polysaccharides ferrum:
Take by weighing iron salt according to weight proportion, and iron salt is mixed with concentration is that the iron salt solutions of 0.05mol/L～8mol/L is for subsequent use;
Take by weighing by weight ratio the astragalus polysaccharides dissolved in distilled water, obtain solution A, the trisodium citrate that adds solution A weight 1/5, continue stirring and dissolving, obtain solution B, then the concentration that adds 1～3 times of solution B weight is 10%～25% alkali liquor, stir, obtain mixed liquor C after slowly dripping the iron salt solutions of 0.05mol/L～8mol/L, after the pH value of mixed liquor C transferred to 9～13, stir 1.5～3h in 70～80 ℃ of hot baths, carry out centrifugal treating 3～10min again under 40～60 ℃ of temperature, rotating speed is 4000r/min; Get the upper strata reddish brown liquid after centrifugal, add ethanol, complete to solution red-brown precipitation species precipitate, after the filtration, behind precipitate microwave treatment 2～5min, hold over night is carried out centrifugal 3～5min to the precipitate after the hold over night, rotating speed is 4000r/min, behind the vacuum drying, get the bronzing powder, the bronzing powder is water-soluble, be 75%～95% ethanol precipitation with concentration again, extremely without Fe
3+Detect, under 50～70 ℃ of conditions, dry, namely obtain astragalus polysaccharides ferrum;
(3) the injection finished product prepares: astragalus polysaccharides ferrum is joined be mixed with the solution that contains ferrum element 150-350mg/mL in the water for injection, the alkali liquor that adds 25-40% is transferred pH value to 11, solution after the alkalization is heated, heating and temperature control is at 50～80 ℃, then add 1-3 ‰ active carbon in the solution after the heating, the absorption insoluble granule, extremely without macroscopic insoluble granule, filter behind restir 20～60min, collect filtrate and filtrate is sterilized, obtain containing the pig injection finished product of astragalus polysaccharides ferrum.
And the parameter that described microwave treatment adopts is microwave power 340～510W, pressure 0.10MPa, constant voltage time 1～5min.
And the frequency of described Ultrasound Instrument is 20Hz～50Hz.
And described iron salt is ferric chloride, ferric nitrate, ferric citrate, iron acetate, ferric perchlorate, ferric ammonium citrate, ferric ammonium nitrate or ferric glycerylphosphate wherein a kind of.
And described alkali liquor is the wherein a kind of of sodium hydroxide solution, sodium carbonate liquor, potassium hydroxide solution, Ammonia or solution of potassium carbonate.
Advantage of the present invention and beneficial effect are:
1. the pig that originally contains astragalus polysaccharides ferrum is raw material with the very cheap astragalus polysaccharides of injection employing cost, stability is better in the production, and water solublity is higher, can absorb with molecular forms, toxic and side effects is the desirable iron supplement agent that meets international standard less than traditional iron dextran.
2. the pig that originally contains astragalus polysaccharides ferrum with injection take nanotechnology as guidance, take astragalus polysaccharides and trivalent iron salt as primary raw material, through synthesis of hydroxy ferrum oxide ferrum parent nucleus, and then obtain astragalus polysaccharides rail injection liquid with the astragalus polysaccharides part complexation of alkalization, refining, preparation and sterilization, this injection can Effective Raise piglet blood content of hemoglobin, increase fast the body weight of piglet, improve the survival rate of piglet.
2. the pig that originally contains astragalus polysaccharides ferrum can be improved the content of iron ion in the crude drug with the preparation method of injection, strengthens the stability of iron ion in crude drug, and course of reaction is easy to control, good product quality, yield are high, and production cost is lower.
3. injection steady quality of the present invention, production cost are lower, and effectively enhancing human body immunity power improves the piglet survival rate, makes its nutritional labeling more balanced comprehensively, and processing technology is simple, is a kind of safe and reliable pig injection that contains astragalus polysaccharides ferrum.
The specific embodiment
The present invention is described in further detail by following examples.Need to prove: following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
The Radix Astragali among the present invention and iron salt all can be bought in market and obtain.
Embodiment 1
A kind of pig injection that contains astragalus polysaccharides ferrum, active component and the weight thereof of its injection are respectively: astragalus polysaccharides 15Kg; Iron salt 10Kg, this iron salt are ferric chloride, ferric nitrate, ferric citrate, iron acetate, ferric perchlorate, ferric ammonium citrate, ferric ammonium nitrate or ferric glycerylphosphate wherein a kind of, and the present embodiment iron salt adopts ferric chloride.
A kind of pig that contains astragalus polysaccharides ferrum preparation method of injection, the step of its preparation method is:
(1) extraction of astragalus polysaccharides: get the Radix Astragali and with 1: 1.5 distilled water of weight ratio the Radix Astragali is carried out preimpregnation and spend the night and obtain presoak, the concentration that the weight such as adds in the presoak is 35% alcoholic solution, then use microwave treatment 3 times, 20s/ time, the parameter that microwave treatment adopts is microwave power 340W, pressure 0.10MPa, constant voltage time 1min obtains microwave-assisted and extracts liquid; Extract to microwave-assisted that to add concentration by weight 1: 5 in the liquid be 35% alcoholic solution, behind the adjust pH to 3, extract twice with Ultrasound Instrument again, 15min/ time, temperature is controlled to be 20 ℃, and the frequency of Ultrasound Instrument is 20Hz, obtains the Ultrasound Instrument extracting solution; Behind the Ultrasound Instrument extracting liquid filtering, filtrate for later use, to colourless, washing liquid and filtrate merge the residue of filtration with the distilled water cyclic washing, and the concentrated concentrated solution that obtains adopts macroporous adsorptive resins to separate after concentrated solution filters, and gets separating medium; And colourless to eluent with distilled water eluting resin column, collect eluent, merge separating medium and eluent and concentrate, then adding 3 times of amount concentration is that 75% alcoholic solution carries out precipitate with ethanol, and room temperature leaves standstill sucking filtration behind the 8h, and vacuum drying gets astragalus polysaccharides;
(2) preparation of astragalus polysaccharides ferrum:
Take by weighing iron salt according to weight proportion, and iron salt is mixed with concentration is that the iron salt solutions of 0.05mol/L is for subsequent use; This iron salt is ferric chloride, ferric nitrate, ferric citrate, iron acetate, ferric perchlorate, ferric ammonium citrate, ferric ammonium nitrate or ferric glycerylphosphate wherein a kind of, and present embodiment adopts ferric chloride;
Take by weighing by weight ratio the astragalus polysaccharides dissolved in distilled water, obtain solution A, the trisodium citrate that adds solution A weight 1/5, continue stirring and dissolving, obtain solution B, then the concentration that adds 1 times of solution B weight is 10% alkali liquor, this alkali liquor is sodium hydroxide solution, sodium carbonate liquor, potassium hydroxide solution, Ammonia or solution of potassium carbonate wherein a kind of, present embodiment adopts sodium hydroxide solution, stirs, and obtains mixed liquor C after slowly dripping the iron salt solutions of 0.05mol/L, after the pH value of mixed liquor C transferred to 9, stir 1.5h in 70 ℃ of hot baths, carry out centrifugal treating 3min again under 40 ℃ of temperature, rotating speed is 4000r/min; Get the upper strata reddish brown liquid after centrifugal, add ethanol, complete to solution red-brown precipitation species precipitate, after the filtration, behind precipitate microwave treatment 2min, hold over night, the parameter that microwave treatment adopts is microwave power 340W, pressure 0.10MPa, constant voltage time 1min, precipitate after the hold over night is carried out centrifugal 3min, and rotating speed is 4000r/min, behind the vacuum drying, get the bronzing powder, the bronzing powder is water-soluble, be 75% ethanol precipitation with concentration again, extremely without Fe
3+Detect, under 50 ℃ of conditions, dry, namely obtain astragalus polysaccharides ferrum;
(3) the injection finished product prepares: astragalus polysaccharides ferrum is joined be mixed with the solution that contains ferrum element 150mg/mL in the water for injection, the alkali liquor of adding 25% is transferred pH value to 11, solution after the alkalization is heated, heating and temperature control is at 50 ℃, then adds 1 ‰ active carbons, the absorption insoluble granule in the solution after the heating, extremely without macroscopic insoluble granule, filter behind the restir 20min, collect filtrate and filtrate is sterilized, obtain containing the pig injection finished product of astragalus polysaccharides ferrum.
Embodiment 2
A kind of pig injection that contains astragalus polysaccharides ferrum, active component and the weight thereof of its injection are respectively: astragalus polysaccharides 50Kg; Iron salt 45Kg, this iron salt are ferric chloride, ferric nitrate, ferric citrate, iron acetate, ferric perchlorate, ferric ammonium citrate, ferric ammonium nitrate or ferric glycerylphosphate wherein a kind of, and the present embodiment iron salt adopts ferric nitrate.
A kind of pig that contains astragalus polysaccharides ferrum preparation method of injection, the step of its preparation method is:
(1) extraction of astragalus polysaccharides: get the Radix Astragali and with 1: 3 distilled water of weight ratio the Radix Astragali is carried out preimpregnation and spend the night and obtain presoak, the concentration that the weight such as adds in the presoak is 70% alcoholic solution, then use microwave treatment 3 times, 60s/ time, the parameter that microwave treatment adopts is microwave power 510W, pressure 0.10MPa, constant voltage time 5min obtains microwave-assisted and extracts liquid; Extract to microwave-assisted that to add concentration by weight 1: 5 in the liquid be 70% alcoholic solution, behind the adjust pH to 5, extract twice with Ultrasound Instrument again, 40min/ time, temperature is controlled to be 20 ℃, and the frequency of Ultrasound Instrument is 20Hz, obtains the Ultrasound Instrument extracting solution; Behind the Ultrasound Instrument extracting liquid filtering, filtrate for later use, to colourless, washing liquid and filtrate merge the residue of filtration with the distilled water cyclic washing, and the concentrated concentrated solution that obtains adopts macroporous adsorptive resins to separate after concentrated solution filters, and gets separating medium; And colourless to eluent with distilled water eluting resin column, collect eluent, merge separating medium and eluent and concentrate, then adding 3 times of amount concentration is that 75% alcoholic solution carries out precipitate with ethanol, and room temperature leaves standstill sucking filtration behind the 15h, and vacuum drying gets astragalus polysaccharides;
(2) preparation of astragalus polysaccharides ferrum:
Take by weighing iron salt according to weight proportion, and iron salt is mixed with concentration is that the iron salt solutions of 8mol/L is for subsequent use; This iron salt is ferric chloride, ferric nitrate, ferric citrate, iron acetate, ferric perchlorate, ferric ammonium citrate, ferric ammonium nitrate or ferric glycerylphosphate wherein a kind of, and present embodiment adopts ferric nitrate;
Take by weighing by weight ratio the astragalus polysaccharides dissolved in distilled water, obtain solution A, the trisodium citrate that adds solution A weight 1/5, continue stirring and dissolving, obtain solution B, then the concentration that adds 3 times of solution B weight is 25% alkali liquor, this alkali liquor is sodium hydroxide solution, sodium carbonate liquor, potassium hydroxide solution, Ammonia or solution of potassium carbonate wherein a kind of, present embodiment adopts sodium carbonate liquor, stirs, and obtains mixed liquor C after slowly dripping the iron salt solutions of 8mol/L, after the pH value of mixed liquor C transferred to 13, stir 3h in 80 ℃ of hot baths, carry out centrifugal treating 10min again under 60 ℃ of temperature, rotating speed is 4000r/min; Get the upper strata reddish brown liquid after centrifugal, add ethanol, complete to solution red-brown precipitation species precipitate, after the filtration, behind precipitate microwave treatment 5min, hold over night, the parameter that microwave treatment adopts is microwave power 510W, pressure 0.10MPa, constant voltage time 5min, precipitate after the hold over night is carried out centrifugal 5min, and rotating speed is 4000r/min, behind the vacuum drying, get the bronzing powder, the bronzing powder is water-soluble, be 95% ethanol precipitation with concentration again, extremely without Fe
3+Detect, under 70 ℃ of conditions, dry, namely obtain astragalus polysaccharides ferrum;
(3) the injection finished product prepares: astragalus polysaccharides ferrum is joined be mixed with the solution that contains ferrum element 350mg/mL in the water for injection, the alkali liquor of adding 40% is transferred pH value to 11, solution after the alkalization is heated, heating and temperature control is at 80 ℃, then adds 3 ‰ active carbons, the absorption insoluble granule in the solution after the heating, extremely without macroscopic insoluble granule, filter behind the restir 60min, collect filtrate and filtrate is sterilized, obtain containing the pig injection finished product of astragalus polysaccharides ferrum.
Embodiment 3
A kind of pig injection that contains astragalus polysaccharides ferrum, active component and the weight thereof of its injection are respectively: astragalus polysaccharides 32Kg; Iron salt 22Kg, this iron salt are ferric chloride, ferric nitrate, ferric citrate, iron acetate, ferric perchlorate, ferric ammonium citrate, ferric ammonium nitrate or ferric glycerylphosphate wherein a kind of, and the present embodiment iron salt adopts ferric citrate.
A kind of pig that contains astragalus polysaccharides ferrum preparation method of injection, the step of its preparation method is:
(1) extraction of astragalus polysaccharides: get the Radix Astragali and with 1: 2 distilled water of weight ratio the Radix Astragali is carried out preimpregnation and spend the night and obtain presoak, the concentration that the weight such as adds in the presoak is 50% alcoholic solution, then use microwave treatment 3 times, 40s/ time, the parameter that microwave treatment adopts is microwave power 420W, pressure 0.10MPa, constant voltage time 3min obtains microwave-assisted and extracts liquid; Extract to microwave-assisted that to add concentration by weight 1: 5 in the liquid be 50% alcoholic solution, behind the adjust pH to 3, extract twice with Ultrasound Instrument again, 25min/ time, temperature is controlled to be 20 ℃, and the frequency of Ultrasound Instrument is 35Hz, obtains the Ultrasound Instrument extracting solution; Behind the Ultrasound Instrument extracting liquid filtering, filtrate for later use, to colourless, washing liquid and filtrate merge the residue of filtration with the distilled water cyclic washing, and the concentrated concentrated solution that obtains adopts macroporous adsorptive resins to separate after concentrated solution filters, and gets separating medium; And colourless to eluent with distilled water eluting resin column, collect eluent, merge separating medium and eluent and concentrate, then adding 3 times of amount concentration is that 75% alcoholic solution carries out precipitate with ethanol, and room temperature leaves standstill sucking filtration behind the 12h, and vacuum drying gets astragalus polysaccharides;
(2) preparation of astragalus polysaccharides ferrum:
Take by weighing iron salt according to weight proportion, and iron salt is mixed with concentration is that the iron salt solutions of 3mol/L is for subsequent use; This iron salt is ferric chloride, ferric nitrate, ferric citrate, iron acetate, ferric perchlorate, ferric ammonium citrate, ferric ammonium nitrate or ferric glycerylphosphate wherein a kind of, and present embodiment adopts ferric citrate;
Take by weighing by weight ratio the astragalus polysaccharides dissolved in distilled water, obtain solution A, the trisodium citrate that adds solution A weight 1/5, continue stirring and dissolving, obtain solution B, then the concentration that adds 2 times of solution B weight is 18% alkali liquor, this alkali liquor is sodium hydroxide solution, sodium carbonate liquor, potassium hydroxide solution, Ammonia or solution of potassium carbonate wherein a kind of, present embodiment adopts solution of potassium carbonate, stirs, and obtains mixed liquor C after slowly dripping the iron salt solutions of 3mol/L, after the pH value of mixed liquor C transferred to 11, stir 2h in 75 ℃ of hot baths, carry out centrifugal treating 7min again under 50 ℃ of temperature, rotating speed is 4000r/min; Get the upper strata reddish brown liquid after centrifugal, add ethanol, complete to solution red-brown precipitation species precipitate, after the filtration, behind precipitate microwave treatment 3min, hold over night, the parameter that microwave treatment adopts is microwave power 400W, pressure 0.10MPa, constant voltage time 3min, precipitate after the hold over night is carried out centrifugal 4min, and rotating speed is 4000r/min, behind the vacuum drying, get the bronzing powder, the bronzing powder is water-soluble, be 85% ethanol precipitation with concentration again, extremely without Fe
3+Detect, under 60 ℃ of conditions, dry, namely obtain astragalus polysaccharides ferrum;
(3) the injection finished product prepares: astragalus polysaccharides ferrum is joined be mixed with the solution that contains ferrum element 250mg/mL in the water for injection, the alkali liquor of adding 30% is transferred pH value to 11, solution after the alkalization is heated, heating and temperature control is at 65 ℃, then adds 2 ‰ active carbons, the absorption insoluble granule in the solution after the heating, extremely without macroscopic insoluble granule, filter behind the restir 40min, collect filtrate and filtrate is sterilized, obtain containing the pig injection finished product of astragalus polysaccharides ferrum.
The relative molecular mass of product astragalus polysaccharides ferrum detects in the process of the present invention: utilize gel permeation chromatography (gel permeation chromatography, GPC) detect, make standard curve with 7 standard relative molecular mass dextrans, average weight-molecular mass is from 4,000～430,000, chromatography mobile phase is pure water, sample quality concentration 1g/L, flow velocity 0.16mL/min, 40 ℃ of detector temperatures, the gel chromatographic columns temperature 60 C.According to the American Pharmacopeia requirement, it is 34,000Da～60 that the apparent molecular weight of astragalus polysaccharides ferrum requires, 000Da, and the ratio of weight average molecular weight and number-average molecular weight is less than 1.7.
Iron content mensuration employing ICP method in the product astragalus polysaccharides ferrum in the process of the present invention: instrument is that U.S. Perkin～Elmer company produces Optima 3300DV, also can be according to the detection method of veterinary drug allusion quotation in 2005, adopt oxidation～reductometry by comparing, these two kinds of methods detect, and iron content is that the 5.0-6.0% iron content is basically identical.Equally, the chloride ion detection method also can by standards of pharmacopoeia, detect and all obtain standard-required.
Use advantage of the present invention below by concrete description of test:
1 clinical practice test
With the piglet of birth after 2～3 days, every nest piglet is divided into three groups at random.One group is test group of the present invention, two groups is the iron dextran experimental group, three groups is the blank group, wherein injects astragalus polysaccharides rail injection liquid 1ml for of the present invention group every, and iron dextran experimental group and matched group are injected respectively iron dextran inj and the normal saline of equivalent.Each group is all measured its blood content of hemoglobin (g/dl) in the rear two weeks blood sampling of test; It is all heavy the test same day and 21 ages in days wean time-division another name that each organizes piglet, and add up its weightening finish and survival condition.Its result is as shown in the table:
Blood content of hemoglobin table behind the table 1 piggy injection astragalus polysaccharides rail injection liquid:
As can be seen from the above table, astragalus polysaccharides rail injection liquid and iron dextran group, normal saline matched group that injection the present invention develops compare, and hemoglobin has increased respectively 80.9% and 60.8%.
Gain weight table behind the table 2 piggy injection astragalus polysaccharides rail injection liquid
As known from Table 2, the weight average that increases day by day behind the piggy injection astragalus polysaccharides rail injection liquid is higher than iron dextran combination matched group (normal saline group), has wherein significantly increased by 43.6% than normal saline group.
Survival condition table behind the table 3 piggy injection astragalus polysaccharides rail injection liquid
As known from Table 3, the piglet of injection astragalus polysaccharides rail injection liquid is than the piglet of injecting normal saline, and its survival rate has increased by 5.6%, has increased by 4.3% than iron dextran inj group piglet.
2 animal toxicity tests
Astragalus polysaccharides ferrum rail injection liquid of the present invention is transparent dark brown colloid solution, with white mice intramuscular injection astragalus polysaccharides rail injection liquid, adopt improvement Karber method to measure median lethal dose(LD 50) (LD50), the result is 800.58mg/kg, according to the acute toxicity classification, belong to actual nontoxic level.
Claims (5)
1. pig injection that contains astragalus polysaccharides ferrum, it is characterized in that: the active component of this injection and ratio of weight and number thereof are: astragalus polysaccharides 15-50 part; Iron salt 10-45 part.
(1) this pig that contains astragalus polysaccharides ferrum with the extracting method of one of component astragalus polysaccharides in the injection is: get the Radix Astragali and with the distilled water of weight ratio 1: 1.5～3 Radix Astragali is carried out preimpregnation and spend the night and obtain presoak, the concentration that the weight such as adds in the presoak is 35%～70% alcoholic solution, then use microwave treatment 3 times, 20～60s/ time, obtain microwave-assisted and extract liquid; Extract to microwave-assisted that to add concentration by weight 1: 5～10 in the liquid be 35%～70% alcoholic solution, behind adjust pH to 3～5, extract twice, 15～40min/ time with Ultrasound Instrument again, temperature is controlled to be 20 ℃, obtains the Ultrasound Instrument extracting solution; Behind the Ultrasound Instrument extracting liquid filtering, filtrate for later use, to colourless, washing liquid and filtrate merge the residue of filtration with the distilled water cyclic washing, and the concentrated concentrated solution that obtains adopts macroporous adsorptive resins to separate after concentrated solution filters, and gets separating medium; And colourless to eluent with distilled water eluting resin column, collect eluent, merge separating medium and eluent and concentrate, then adding 3 times of amount concentration is that 75% alcoholic solution carries out precipitate with ethanol, and room temperature leaves standstill sucking filtration behind 8～15h, and vacuum drying gets astragalus polysaccharides;
(2) this pig that contains astragalus polysaccharides ferrum is ferric chloride, ferric nitrate, ferric citrate, iron acetate, ferric perchlorate with the iron salt described in the injection, ferric ammonium citrate, ferric ammonium nitrate or ferric glycerylphosphate wherein a kind of.
2. a pig that contains astragalus polysaccharides ferrum as claimed in claim 1 is with the preparation method of injection, and it is characterized in that: the step of this preparation method is:
(1) extraction of astragalus polysaccharides: get the Radix Astragali and with the distilled water of weight ratio 1: 1.5～3 Radix Astragali is carried out preimpregnation and spend the night and obtain presoak, the concentration that the weight such as adds in the presoak is 35%～70% alcoholic solution, then use microwave treatment 3 times, 20～60s/ time, obtain microwave-assisted and extract liquid; Extract to microwave-assisted that to add concentration by weight 1: 5～10 in the liquid be 35%～70% alcoholic solution, behind adjust pH to 3～5, extract twice, 15～40min/ time with Ultrasound Instrument again, temperature is controlled to be 20 ℃, obtains the Ultrasound Instrument extracting solution; Behind the Ultrasound Instrument extracting liquid filtering, filtrate for later use, to colourless, washing liquid and filtrate merge the residue of filtration with the distilled water cyclic washing, and the concentrated concentrated solution that obtains adopts macroporous adsorptive resins to separate after concentrated solution filters, and gets separating medium; And colourless to eluent with distilled water eluting resin column, collect eluent, merge separating medium and eluent and concentrate, then adding 3 times of amount concentration is that 75% alcoholic solution carries out precipitate with ethanol, and room temperature leaves standstill sucking filtration behind 8～15h, and vacuum drying gets astragalus polysaccharides;
(2) preparation of astragalus polysaccharides ferrum:
Take by weighing iron salt according to weight proportion, and iron salt is mixed with concentration is that the iron salt solutions of 0.05mol/L～8mol/L is for subsequent use;
Take by weighing by weight ratio the astragalus polysaccharides dissolved in distilled water, obtain solution A, the trisodium citrate that adds solution A weight 1/5, continue stirring and dissolving, obtain solution B, then the concentration that adds 1～3 times of solution B weight is 10%～25% alkali liquor, stir, obtain mixed liquor C after slowly dripping the iron salt solutions of 0.05mol/L～8mol/L, after the pH value of mixed liquor C transferred to 9～13, stir 1.5～3h in 70～80 ℃ of hot baths, carry out centrifugal treating 3～10min again under 40～60 ℃ of temperature, rotating speed is 4000r/min; Get the upper strata reddish brown liquid after centrifugal, add ethanol, complete to solution red-brown precipitation species precipitate, after the filtration, behind precipitate microwave treatment 2～5min, hold over night is carried out centrifugal 3～5min to the precipitate after the hold over night, rotating speed is 4000r/min, behind the vacuum drying, get the bronzing powder, the bronzing powder is water-soluble, be 75%～95% ethanol precipitation with concentration again, extremely without Fe
3+Detect, under 50～70 ℃ of conditions, dry, namely obtain astragalus polysaccharides ferrum;
(3) the injection finished product prepares: astragalus polysaccharides ferrum is joined be mixed with the solution that contains ferrum element 150-350mg/mL in the water for injection, the alkali liquor that adds 25-40% is transferred pH value to 11, solution after the alkalization is heated, heating and temperature control is at 50～80 ℃, then add 1-3 ‰ active carbon in the solution after the heating, the absorption insoluble granule, extremely without macroscopic insoluble granule, filter behind restir 20～60min, collect filtrate and filtrate is sterilized, obtain containing the pig injection finished product of astragalus polysaccharides ferrum.
3. the pig that contains astragalus polysaccharides ferrum according to claim 2 is with the preparation method of injection, and it is characterized in that: the parameter that described microwave treatment adopts is microwave power 340～510W, pressure 0.10MPa, constant voltage time 1～5min.
4. the pig that contains astragalus polysaccharides ferrum according to claim 2 is with the preparation method of injection, and it is characterized in that: the frequency of described Ultrasound Instrument is 20Hz～50Hz.
5. the pig that contains astragalus polysaccharides ferrum according to claim 2 is with the preparation method of injection, and it is characterized in that: described alkali liquor is the wherein a kind of of sodium hydroxide solution, sodium carbonate liquor, potassium hydroxide solution, Ammonia or solution of potassium carbonate.
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| CN102552307B (en) * | 2012-03-13 | 2013-04-10 | 郑州百瑞动物药业有限公司 | Compound astragalus polysaccharide injection used for pigs and preparation method thereof |
| CN105456185A (en) * | 2015-12-16 | 2016-04-06 | 浙江大飞龙动物保健品有限公司 | Compound Astragalus polysaccharides injection and preparation method thereof |
| CN105924535B (en) * | 2016-04-27 | 2018-10-26 | 广西农业职业技术学院 | A kind of preparation method of astragalus polyose iron |
| CN106038591A (en) * | 2016-05-31 | 2016-10-26 | 田东县浙缘农业科技有限公司 | Pig injection liquid containing astragalus polysaccharide iron |
| CN107213115A (en) * | 2017-07-01 | 2017-09-29 | 山东中牧兽药有限公司 | A kind of compound Radix Astragali polysaccharide injection |
| CN107714720A (en) * | 2017-10-30 | 2018-02-23 | 兰州大学 | A kind of preparation method for the Radix Angelicae Sinensis astragalus polyose iron complexes for treating hypoferric anemia |
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