CN105924452A - Preparation method of Hainanmycin sodium finished product - Google Patents
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- CN105924452A CN105924452A CN201610279991.0A CN201610279991A CN105924452A CN 105924452 A CN105924452 A CN 105924452A CN 201610279991 A CN201610279991 A CN 201610279991A CN 105924452 A CN105924452 A CN 105924452A
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- 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 title claims abstract description 78
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 78
- 239000011734 sodium Substances 0.000 title claims abstract description 78
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000047 product Substances 0.000 claims abstract description 37
- 239000007788 liquid Substances 0.000 claims abstract description 27
- 239000002904 solvent Substances 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 238000000926 separation method Methods 0.000 claims abstract description 15
- 238000000855 fermentation Methods 0.000 claims abstract description 14
- 230000004151 fermentation Effects 0.000 claims abstract description 14
- 239000012065 filter cake Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000000605 extraction Methods 0.000 claims abstract description 7
- 239000000284 extract Substances 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 5
- 230000001105 regulatory effect Effects 0.000 claims abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 36
- 239000000243 solution Substances 0.000 claims description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 238000001914 filtration Methods 0.000 claims description 19
- 239000007787 solid Substances 0.000 claims description 14
- 238000001953 recrystallisation Methods 0.000 claims description 7
- 239000006166 lysate Substances 0.000 claims description 6
- 230000001186 cumulative effect Effects 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000012141 concentrate Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 2
- 238000003828 vacuum filtration Methods 0.000 abstract 2
- 239000008186 active pharmaceutical agent Substances 0.000 abstract 1
- 239000013078 crystal Substances 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 description 9
- 239000003814 drug Substances 0.000 description 8
- 241000894006 Bacteria Species 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 7
- 238000013019 agitation Methods 0.000 description 6
- 238000010298 pulverizing process Methods 0.000 description 6
- 238000001291 vacuum drying Methods 0.000 description 6
- 241000287828 Gallus gallus Species 0.000 description 5
- 239000003513 alkali Substances 0.000 description 5
- 239000002893 slag Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 4
- 229940079593 drug Drugs 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000004060 metabolic process Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 241000283690 Bos taurus Species 0.000 description 2
- 241001494479 Pecora Species 0.000 description 2
- 239000003674 animal food additive Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 235000013372 meat Nutrition 0.000 description 2
- 230000007886 mutagenicity Effects 0.000 description 2
- 231100000299 mutagenicity Toxicity 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 208000031404 Chromosome Aberrations Diseases 0.000 description 1
- 208000003495 Coccidiosis Diseases 0.000 description 1
- 230000005778 DNA damage Effects 0.000 description 1
- 231100000277 DNA damage Toxicity 0.000 description 1
- 241000192125 Firmicutes Species 0.000 description 1
- 241000272496 Galliformes Species 0.000 description 1
- 206010023076 Isosporiasis Diseases 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- 241000282849 Ruminantia Species 0.000 description 1
- 241000607142 Salmonella Species 0.000 description 1
- 241001052560 Thallis Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000010564 aerobic fermentation Methods 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000037396 body weight Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 231100000005 chromosome aberration Toxicity 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 230000001079 digestive effect Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000003623 enhancer Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000006052 feed supplement Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000002054 inoculum Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 244000144977 poultry Species 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000017854 proteolysis Effects 0.000 description 1
- 238000012372 quality testing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 210000004767 rumen Anatomy 0.000 description 1
- 231100000188 sister chromatid exchange Toxicity 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 231100000820 toxicity test Toxicity 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/02—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains two hetero rings
- C07D493/10—Spiro-condensed systems
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to a preparation method of a Hainanmycin sodium finished product. The method comprises the following steps: by using Hainanmycin sodium fermentation liquid as a raw material, carrying out solid-liquid separation and drying to obtain dry mycelia, adding a solvent into the dry mycelia to perform extraction, regulating the pH value, carrying out solid-liquid separation, concentrating the obtained extract at 30-70 DEG C, recycling the organic solvent, putting the concentrated solution into a crystallizing tank, performing cooling under stirring to crystallize, carrying out vacuum filtration, adding a solvent to dissolve the filter cake, adding water which is 20-50 % of the total volume of the solution, performing cooling under stirring to recrystallize, carrying out vacuum filtration, adding the obtained crystals into a biconical dryer, and performing drying at 20-70 DEG C under the vacuum degree of (-0.09) MPa for 3-8 hours, thereby obtaining the Hainanmycin sodium finished product. The method has the advantages of simple production process, convenient operation, high production efficiency, high product purity, high economy, environment friendliness, recyclable solvents and the like. The extracted Hainanmycin sodium can be prepared into the Hainanmycin sodium active pharmaceutical ingredient or Hainanmycin sodium premixes with different specifications according to needs.
Description
Technical field
The present invention relates to the preparation method of a kind of Hainanmycin sodium finished product, belong to chemical pharmacy field.
Background technology
Hainanmycin sodium is a kind of novel digestive enhancers or metabolism regulators, mainly to gram positive bacteria
There is inhibitory action, poor to gram negative bacteria effect.He is mainly used to prevent and treat coccidiosis of domestic fowls
With the feed additive as poultry such as cattle and sheep, promote growth of animal, improve the quality of meat.Hainanmycin
Sodium belongs to environment-friendly feed additive.
Nineteen sixty, Chinese find a strain class mycete of isolated in the soil in Fujian provincial stone horse area
Belong to a kind of yellow crystalline compound that C-1329 produces.Obtain when the continuation to this bacterium in 1977 is studied
A kind of white crystalline compound, through physical constant, chemical property, structural property, structure determination, medicine
Reason and toxicity test are studied.Proof is the natural active matter that a class is new, named Hainanmycin
(Hainanmeisu)。
Hu Hongbo (1994) uses chromosomal aberration test and sister chromatid exchange two kinds of tests of test
Method, has carried out the mutagenicity research of Hainanmycin sodium, and hereditism's terminal that it is detected includes dyeing
Body distortion and primitiveness DNA damage, done Salmonella reversion test in addition, in testing at two kinds, and Hainanmycin
Sodium does not shows mutagenicity.
2004, Zhang Tingrong toxic reaction and weightening finish effect to adding Hainanmycin sodium in broiler chicken feedstuff
Studied.Result shows to add 5-20mg/kg Hainanmycin sodium in broiler chicken feedstuff, does not appoint
What untoward reaction, can promote growth of meat chicken, and the toxic action young to broiler is little, at broiler chicken complete feed
Middle 5mg/kg, 10mg/kg of adding has the effect promoting weightening finish, is respectively increased 10.17% than matched group weightening finish
With 7.05%.
1998, the mechanism of action of Hainanmycin was studied by Ren Mingqiang, it was demonstrated that Hainanmycin sodium is theoretical
On can promote the growth of cattle and sheep body weight.
2004, the systematic study such as the Chen Jie situation of Hainanmycin regulation and control ruminant digestion metabolism, knot
Fruit shows, Hainanmycin can regulate function of rumen, improves propionate level, suppresses protein degradation, hence it is evident that
Improve absorption and the metabolism of nutrient substance, promote growth.
Summary of the invention
The technical problem to be solved is to provide the preparation method of a kind of Hainanmycin sodium finished product, this
Invention has that production technology is simple and convenient to operate, production efficiency is high, product purity high, cost-effective and environmentally friendly
Etc. advantage, it is also possible to as required the Hainanmycin sodium of extraction to be prepared as Hainanmycin sodium raw materials medicine or not
The Hainanmycin sodium pre-mixing agent of same specification.
The technical scheme is that the preparation of a kind of Hainanmycin sodium finished product
Method, comprises the steps:
1) with Hainanmycin sodium fermentation liquid as raw material, through solid-liquid separation and be dried to obtain dry mycelium, add
Entering extraction, temperature controls at 20-50 DEG C, at the uniform velocity stirs 2-4 with rotating speed 50-300 rev/min little
Time；
2) regulating step 1) pH to 8-9 of lixiviating solution that obtains, and separate solid dreg, lixiviating solution
Use enrichment facility to concentrate under conditions of 30-70 DEG C, obtain concentrated solution；
3) by step 2) in the concentrated solution that obtains press-in crystallizer, stir with rotating speed 100-400 rev/min
Mix 2-10 hour after being cooled to 20-40 DEG C, sucking filtration；
4) filter cake obtained after sucking filtration is placed in double-cone dryer, 20-70 DEG C of vacuum-0.09MPa
Under be dried 3-8 hour, obtain Hainanmycin sodium finished product.
On the basis of above-mentioned preparation method, the present invention can also have and embodies further below or optimize:
Concrete, step 1) in, the consumption of described solvent is 3-7 times of dry mycelium quality.
Preferably, step 2) in, the volume of described concentrated solution is 0.1-0.2 times of lixiviating solution volume.
Preferably, step 3) and 4) between also include a recrystallization process: to step 3) obtain
Filter cake adds solvent heating for dissolving, and lysate is pressed into recrystallization tank, adds and accounts for lysate cumulative volume
The water of 20-50%, after within 2-10 hour, being cooled to 25-45 DEG C with rotating speed 100-400 rev/min stirring, takes out
Filter.
Concrete, during recrystallization, the consumption of described solvent is 1-2 times of filter cake quality.
Preferably, step 2) in solid dreg can be according to step 1) condition add extraction also
Experience step 2), 3), 4) prepare Hainanmycin sodium finished product.
Concrete, after three times extract, the content < 0.2% of Hainanmycin sodium in the solid dreg being dried.
Concrete, described solvent is the volume of the aqueous solution of methanol or ethanol, wherein methanol or ethanol and water
Ratio is 5-9:1.
Preferably, in described solvent, the volume ratio of methanol or ethanol and water is 9:1.
Compared with prior art, the preparation method of the Hainanmycin sodium finished product that the present invention provides is with Hainanmycin
Sodium fermentation liquid is that dry mycelium prepared by raw material, with solvent by mould for the Hainan in dry for Hainanmycin sodium mycelium
Element sodium extracts, and is then removed by solvent, obtains Hainanmycin sodium finished product, have after processing further
Production technology is simple and convenient to operate, production efficiency is high, product purity is high, the advantage such as cost-effective and environmentally friendly,
And solvent can reuse.The Hainanmycin sodium finished product of extraction can be further purified as required,
It is prepared as the Hainanmycin sodium pre-mixing agent of Hainanmycin sodium raw materials medicine or different size.
Detailed description of the invention
Principle and feature to the present invention are described below, and example is served only for explaining the present invention, and
Non-for limiting the scope of the present invention.
In the present invention, Hainanmycin sodium fermentation liquid used produces from Shandong Shengli Bioengineering Co., Ltd.
Product.Its preparation method comprises the following steps: first Hainanmycin sodium producing strains is accessed seed tank,
Being then passed through step by step after amplification culture, the inoculum concentration by 15% accesses fermentation tank, then according to fermentation liquid with
The volume ratio 1:0.5-1:1.5 ventilation of air, the rotating speed of stirring is 150 revs/min, controls temperature and is
26-30 DEG C, carry out aerobic fermentation；Sweat controls pH=6.7-7.2, according to thalli morphology, sugar
The feed supplement such as content, fermentation period is 220-240 hour, obtains Hainanmycin sodium fermentation liquid.
Embodiment 1
Above-mentioned Hainanmycin sodium fermentation liquid solid-liquid separation is obtained dry mycelium with being dried, weighs dry mycelium
800g, adds 400mL water and 3600mL methanol, carries out even by the mechanical agitation that speed is 50 revs/min
Speed stirring 4 hours, the temperature of whole system controls at 20 DEG C；After system solid-liquid separation, solid dreg
Standby, add alkali and lixiviating solution is adjusted to pH=9, lixiviating solution is placed in Rotary Evaporators, in 65 DEG C of water-baths
Methanol is boiled off 3200mL, and organic solvent is reclaimed, obtain concentrated solution 450ml.Concentrated solution is added knot
In brilliant tank, insulated and stirred 2 hours, sucking filtration at 40 DEG C.After sucking filtration, filter cake is transferred in vacuum drying oven,
It is dried 1-2 hour under 60-70 DEG C of vacuum-0.09MPa, after pulverizing, obtains Hainanmycin sodium finished product
119.4g, wherein the content of Hainanmycin sodium is 90%.Hainanmycin sodium finished product prepared by the present invention can enter
One step is made the pre-mixing agent of all size or is further purified and makes the Hainanmycin sodium raw materials that content is higher
Medicine.
Embodiment 2
Above-mentioned Hainanmycin sodium fermentation liquid solid-liquid separation is obtained dry mycelium with being dried, weighs dry mycelium
800g, adds 500mL water and 4500mL methanol, carries out by the mechanical agitation that speed is 150 revs/min
At the uniform velocity stirring 3 hours, the temperature of whole system controls at 50 DEG C；After system solid-liquid separation, solid bacterium
Slag is standby, adds alkali and lixiviating solution is adjusted to pH=9, and lixiviating solution is placed in Rotary Evaporators, 50 DEG C of water-baths
Middle 4000mL that methanol is boiled off, and organic solvent is reclaimed, obtain concentrated solution 530mL.Concentrated solution is added
In crystallizer, insulated and stirred 6 hours, sucking filtration at 30 DEG C.After sucking filtration, filter cake is transferred to vacuum drying oven
In, it is dried 4-5 hour under 40-50 DEG C of vacuum-0.09MPa, after pulverizing, obtains Hainanmycin sodium finished product
119.9g, wherein the content of Hainanmycin sodium is 93%.Hainanmycin sodium finished product prepared by the present invention can enter
One step is processed into the pre-mixing agent of all size or is further purified and makes the Hainanmycin sodium that content is higher
Crude drug.
Embodiment 3
Above-mentioned Hainanmycin sodium fermentation liquid solid-liquid separation is obtained dry mycelium with being dried, weighs dry mycelium
800g, adds 500mL water and 4500mL ethanol, carries out by the mechanical agitation that speed is 300 revs/min
At the uniform velocity stirring 2 hours, the temperature of whole system controls at 35 DEG C；After system solid-liquid separation, solid bacterium
Slag is standby, adds alkali and lixiviating solution is adjusted to pH=8, and lixiviating solution is placed in Rotary Evaporators, 70 DEG C of water-baths
Middle 4000mL that ethanol is boiled off, and organic solvent is reclaimed, obtain concentrated solution 550mL.Concentrated solution is added
In crystallizer, insulated and stirred 10 hours, sucking filtration at 20 DEG C.After sucking filtration, filter cake is transferred to vacuum drying
In case, it is dried 7-8 hour under 25-35 DEG C of vacuum-0.09MPa, after pulverizing, obtains Hainanmycin sodium
Product 120.4g, wherein the content of Hainanmycin sodium is 91.5%.Hainanmycin sodium finished product prepared by the present invention
The pre-mixing agent of all size can be made further or be further purified and make the Hainanmycin sodium that content is higher
Crude drug.
Embodiment 4
Above-mentioned Hainanmycin sodium fermentation liquid solid-liquid separation is obtained dry mycelium with being dried, weighs dry mycelium
800g, adds 500mL water and 2500mL ethanol, carries out by the mechanical agitation that speed is 300 revs/min
At the uniform velocity stirring 2 hours, the temperature of whole system controls at 35 DEG C；After system solid-liquid separation, solid bacterium
Slag is standby, adds alkali and lixiviating solution is adjusted to PH=9, and lixiviating solution is placed in Rotary Evaporators, 45 DEG C of water-baths
Middle 2100mL that ethanol is boiled off, and organic solvent is reclaimed, obtain concentrated solution 425ml.Concentrated solution is added
In crystallizer, insulated and stirred 7 hours, sucking filtration at 30 DEG C.After sucking filtration, filter cake is transferred to vacuum drying oven
In, it is dried 7-8 hour under 20-30 DEG C of vacuum-0.09MPa, after pulverizing, obtains Hainanmycin sodium finished product
107.4g, wherein the content of Hainanmycin sodium is 95.2%.Hainanmycin sodium finished product prepared by the present invention can
Make the pre-mixing agent of all size further or to be further purified the Hainanmycin sodium making content higher former
Material medicine.
Embodiment 5
Above-mentioned Hainanmycin sodium fermentation liquid solid-liquid separation is obtained dry mycelium with being dried, weighs dry mycelium
800g, adds 500mL water and 2500mL ethanol, carries out by the mechanical agitation that speed is 300 revs/min
At the uniform velocity stirring 2 hours, the temperature of whole system controls at 35 DEG C；After system solid-liquid separation, solid bacterium
Slag is standby, adds alkali and lixiviating solution is adjusted to PH=9, and lixiviating solution is placed in Rotary Evaporators, 45 DEG C of water-baths
Middle 2100mL that ethanol is boiled off, and organic solvent is reclaimed, obtain concentrated solution 425ml.Concentrated solution is added
In crystallizer, insulated and stirred 7 hours, sucking filtration at 30 DEG C.Filter cake is added the solvent of its quality 1-2 times
And heating for dissolving, lysate is pressed into recrystallization tank, adds the water accounting for lysate cumulative volume 20-50%, with
After rotating speed 100-400 rev/min stirring is cooled to 25-45 DEG C in 2-10 hour, sucking filtration.After sucking filtration, filter
Cake is transferred in vacuum drying oven, is dried 5-6 hour, after pulverizing under 40-50 DEG C of vacuum-0.09MPa
Obtaining Hainanmycin sodium finished product 105.2g, wherein the content of Hainanmycin sodium is 97.2%.Prepared by the present invention
Hainanmycin sodium finished product also can be further purified and make the pre-mixing agent of all size or be further purified system
Become the Hainanmycin sodium raw materials medicine that content is higher.
Embodiment 6
In above-mentioned 5 embodiments, solid dreg still contains the Hainanmycin sodium of residual after quality testing,
Wherein, embodiment 1 is containing 1.6%, and embodiment 2 is containing 0.8%, and embodiment 3 is containing 0.8%, and embodiment 4 contains
0.9%, embodiment 5, containing 0.8%, takes 800g after collecting the solid dreg mixing of aforementioned four experiment, adds
400mL water and 3600mL methanol, at the uniform velocity stir by the mechanical agitation that speed is 100 revs/min,
Mixing time 3 hours, the temperature of whole system controls at 45 DEG C；After system solid-liquid separation, solid bacterium
Slag is standby, and (the Hainanmycin sodium content of dried detection residual is reduced to 0.3%, can again extract, then contain
Amount can decline further), lixiviating solution is placed in Rotary Evaporators, is boiled off by methanol in 60 DEG C of water-baths
3150mL, and organic solvent is reclaimed, obtain concentrated solution 460mL.Concentrated solution is added in crystallizer, 40 DEG C
Lower insulated and stirred 5 hours, sucking filtration.After sucking filtration, filter cake is transferred in vacuum drying oven, and 60-70 DEG C true
It is dried 1-2 hour under reciprocal of duty cycle-0.09MPa, after pulverizing, obtains Hainanmycin sodium finished product 7.2g, Qi Zhonghai
The content of south mycin sodium is 92.7%.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all in the present invention
Spirit and principle within, any modification, equivalent substitution and improvement etc. made, should be included in this
Within bright protection domain.
Claims (9)
1. the preparation method of a Hainanmycin sodium finished product, it is characterised in that including:
1) with Hainanmycin sodium fermentation liquid as raw material, through solid-liquid separation and be dried to obtain dry mycelium, add
Entering extraction, temperature controls at 20-50 DEG C, at the uniform velocity stirs 2-4 with rotating speed 50-300 rev/min little
Time；
2) regulating step 1) pH to 8-9 of lixiviating solution that obtains, and separate solid dreg, then at 30-70 DEG C
Under conditions of use enrichment facility concentrate, obtain concentrated solution；
3) by step 2) in the concentrated solution that obtains press-in crystallizer, stir with rotating speed 100-400 rev/min
Mix 2-10 hour after being cooled to 20-40 DEG C, sucking filtration；
4) filter cake obtained after sucking filtration is placed in double-cone dryer, at 20-70 DEG C of vacuum-0.09MPa
Under be dried 3-8 hour, obtain Hainanmycin sodium finished product.
The preparation method of Hainanmycin sodium finished product the most according to claim 1, it is characterised in that
Step 1) in, the consumption of described solvent is 3-7 times of dry mycelium quality.
The preparation method of Hainanmycin sodium finished product the most according to claim 1, it is characterised in that
Step 2) in, the volume of described concentrated solution is 0.1-0.2 times of lixiviating solution volume.
The preparation method of Hainanmycin sodium finished product the most according to claim 1, it is characterised in that
Step 3) and 4) between also include a recrystallization process: to step 3) filter cake that obtains after sucking filtration adds
Enter solvent heating for dissolving, lysate is pressed into recrystallization tank, add and account for lysate cumulative volume 20-50%
Water, after within 2-10 hour, being cooled to 25-45 DEG C with rotating speed 100-400 rev/min stirring, then sucking filtration.
The preparation method of Hainanmycin sodium finished product the most according to claim 4, it is characterised in that
During recrystallization, the consumption of described solvent is 1-2 times of filter cake quality.
6. according to the preparation method of the Hainanmycin sodium finished product described in any one of claim 1 to 5, its
Be characterised by, step 2) in solid dreg can be according to step 1) condition add extraction warp
Go through step 2), 3), 4) prepare Hainanmycin sodium finished product.
The preparation method of Hainanmycin sodium finished product the most according to claim 6, it is characterised in that
After three times extract, the content < 0.2% of Hainanmycin sodium in the solid dreg being dried.
8. according to the preparation method of the Hainanmycin sodium finished product described in any one of claim 1 to 5, its
Being characterised by, described solvent is the volume ratio of the aqueous solution of methanol or ethanol, wherein methanol or ethanol and water
For 5-9:1.
The preparation method of Hainanmycin sodium finished product the most according to claim 8, it is characterised in that
In described solvent, the volume ratio of methanol or ethanol and water is 9:1.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4038384A (en) * | 1974-06-10 | 1977-07-26 | Eli Lilly And Company | Antibiotic a-28086 and process for production thereof |
| CN102634553A (en) * | 2012-01-13 | 2012-08-15 | 山东胜利股份有限公司 | Hainanmycin fermentation method |
-
2016
- 2016-04-28 CN CN201610279991.0A patent/CN105924452A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4038384A (en) * | 1974-06-10 | 1977-07-26 | Eli Lilly And Company | Antibiotic a-28086 and process for production thereof |
| CN102634553A (en) * | 2012-01-13 | 2012-08-15 | 山东胜利股份有限公司 | Hainanmycin fermentation method |
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