CN105861611A - Preparation method of tetracycline based on fermentation effect improvement - Google Patents
Preparation method of tetracycline based on fermentation effect improvement Download PDFInfo
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- CN105861611A CN105861611A CN201610413732.2A CN201610413732A CN105861611A CN 105861611 A CN105861611 A CN 105861611A CN 201610413732 A CN201610413732 A CN 201610413732A CN 105861611 A CN105861611 A CN 105861611A
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P29/00—Preparation of compounds containing a naphthacene ring system, e.g. tetracycline
Abstract
The invention discloses a preparation method of tetracycline based on fermentation effect improvement. The preparation method includes the following steps that 1, fermentation liquor is prepared: golden streptomyces aureus spores are inoculated to a spore culture medium for culture for 5 days, then the prepared spores are transferred to a seeding tank for culture, and the prepared spores undergo fermentation culture after seed culture is completed; 2, the fermentation liquor is acidified; 3, the separation and purification of the fermentation liquor is are performed: filtration treatment is conducted on the acidified filtrate by using a plate frame, the filtrate obtained after filtration is decolored by using 122 ion exchange resin till the light transmittance of the filtrate is up to 90% or above, the filtrate is fed into a crystallizing tank for crystallization, then centrifugal separation is performed till the water content of wet crystals obtained after separation is up to 20% by mass percentage concentration, the wet crystals obtained through centrifugation are dried, and finally dried powder with the water content of 10% or below by mass percentage concentration is obtained. The preparation method includes few steps, reaction conditions are mild, industrialized production of tetracycline hydrochloride is easy to achieved, and a new thought is provided for production of the tetracycline hydrochloride.
Description
Technical field
The present invention relates to technical field of medicine synthesis, be specifically related to preparation method based on the tetracycline improving ferment effect.
Background technology
Quadracycline molecular formula is: C22H24N2O8HCl, molecular weight is 480.91.Yellow crystal, odorlessness.Bitter.Easily moisture absorption.Meet photochromic gradual change deep.Soluble in water, in methyl alcohol.Ethanol, insoluble in ether, hydroxyl class.It is the antibacterial material separated out from the nutrient solution of actinomyces gold chain clump bacterium (Streptomycesaureofaciens), gram-positive bacteria, negative bacterium, Richettsia, filtration row virus, Spirochaeta or even protozoon class there are is good inhibiting effect, the most invalid to tulase, mycetozoan etc..
Quadracycline is first generation TCs, and it has broad-spectrum antiseptic feature, can resist such as multiple-microorganisms such as Gram-negative and gram-positive bacteria, Chlamydia, mycoplasma and primary species parasites.The additionally crowd to a lot of penicillin-susceptible, can treat some disease with TCs product as an alternative.Owing to its cost is the highest, it is widely used in the treatment that human and animal is infected.
The synthesis process of existing quadracycline is complicated, is unfavorable for large-scale industrial production.
Summary of the invention
The present invention purpose be to provide the preparation method of tetracycline based on improving ferment effect, solve the problem that the synthesis process of existing quadracycline is complicated.
The present invention is achieved through the following technical solutions:
Preparation method based on the tetracycline improving ferment effect, comprises the following steps:
1), the preparation of zymotic fluid: will cultivate 5 days on streptomyces aureus spore inoculating to Spore cultivation base, until spore is ripe, then the spore of preparation is gone to seed tank culture, fermented and cultured is transferred to after seed tank culture, described seeding tank includes tank body, tank body be internally provided with agitating device, the outer wall of tank body is provided with sandwich, the lower end of described sandwich is provided with water inlet, the upper end of sandwich is provided with delivery port, described agitating device includes rotating shaft, helical blade it is provided with in rotating shaft, it is provided above cross bar at helical blade in rotating shaft, projection it is provided with on cross bar, projection is tapered protrusion；The bottom of described sandwich is set to arc structure, and the bottom of sandwich is provided with blow-off pipe, and blow-off pipe is provided with valve, and the sidewall of sandwich is provided with shower nozzle, and the water jet of described shower nozzle matches with the bottom of sandwich；
2), the acidifying of zymotic fluid: add oxalic acid and carry out acidification, be then filtrated to get acidified filtrate；
3), zymotic fluid isolated and purified: use sheet frame that acidified filtrate is carried out filtration treatment, filtrate after filtration is decoloured with 122 ion exchange resin, until entering crystallizing tank crystallization after filtrate light transmittance >=90%, at in crystallizing tank, temperature is 8 DEG C-10 DEG C, with ammoniacal liquor, the filtrate pH value after decolouring is adjusted to 4.4-4.8, then 50min-60min it is incubated, it is centrifuged again separating, until wet crystal water content reaches 20% based on mass percentage concentration after Fen Liing, pneumatic conveying drying mode is used to be dried in the centrifugal wet crystal obtained, keeping EAT is 100 DEG C-160 DEG C, finally obtain water content based on mass percentage concentration≤dry powder of 10%, gained dry powder is tetracycline powder.
The step of synthesis technique of the present invention is few, and reaction condition is gentle, easily realizes the industrialized production of quadracycline, and the production for quadracycline provides a new thinking.
Further, Spore cultivation base consists of the following composition: wheat bran 3.0%-3.8%, magnesium sulfate 0.1%-0.3%, potassium dihydrogen phosphate 0.2%-0.4%, agar 2.4%-3.2%, and surplus is water.
Further, being provided with culture medium in seeding tank, culture medium consists of the following composition: cornstarch 3.0%-5.0%, groundnut meal 1%-3%, soybean cake powder 1%-3%, dusty yeast 1%-2%, calcium carbonate 0.2%-0.5%, ammonium sulfate 0.2%-0.6%, potassium dihydrogen phosphate 0.2%-0.4%, amylase 0.03%-0.05%, defoamer 0.2%-0.4%, surplus is water.
Further, the condition of fermented and cultured is: temperature is 25 DEG C-30 DEG C, pressure be 0.02Mpa-0.05Mpa, pH be 5.6-6.2, fermentation time be more than 72 hours.
Further, helical blade is provided with protruding I.
Further, sandwich be internally provided with temperature sensor, temperature sensor is connected with the display screen being arranged on sandwich outer wall.
Further, the upper end of tank body is provided with charge door, and the sidewall of tank body is provided with probe tube, air inlet pipe.
The present invention compared with prior art, has such advantages as and beneficial effect:
1, the step of synthesis technique of the present invention is few, and reaction condition is gentle, easily realizes the industrialized production of quadracycline, and the production for quadracycline provides a new thinking.
2, projection of the present invention can puncture the bubble of liquid surface, it is to avoid the accumulation of bubble, and then instant invention overcomes the problem affecting mixing effect that existing fermentation tank causes because of bubble formation；And stirring vane of the present invention is helical structure, helical structure can produce eddy current during stirring, and the formation of eddy current has certain centrifugal action, and centrifugal action is conducive to reducing the generation of bubble, further reduces the accumulation of bubble in fermentation tank.
Accompanying drawing explanation
Accompanying drawing described herein is used for providing being further appreciated by the embodiment of the present invention, constitutes the part of the application, is not intended that the restriction to the embodiment of the present invention.In the accompanying drawings:
Fig. 1 is the structural representation of seeding tank.
Mark and the parts title of correspondence in accompanying drawing:
1-tank body, 2-sandwich, 3-rotating shaft, 4-shower nozzle, 5-blow-off pipe, 6-display screen, 11-charge door, 12-probe tube, 13-air inlet pipe, 21-water inlet, 22-delivery port, 31-helical blade, 32-projection I, 33-cross bar, 34-is protruding, 51-valve.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, and the exemplary embodiment of the present invention and explanation thereof are only used for explaining the present invention, not as a limitation of the invention.
Embodiment 1:
As it is shown in figure 1, preparation method based on the tetracycline improving ferment effect, comprise the following steps:
1), the preparation of zymotic fluid: will cultivate 5 days on streptomyces aureus spore inoculating to Spore cultivation base, until spore is ripe, then the spore of preparation is gone to seed tank culture, fermented and cultured is transferred to after seed tank culture, described seeding tank includes tank body 1, tank body 1 be internally provided with agitating device, the outer wall of tank body 1 is provided with sandwich 2, the lower end of described sandwich 2 is provided with water inlet 21, the upper end of sandwich 2 is provided with delivery port 22, described agitating device includes rotating shaft 3, helical blade 31 it is provided with in rotating shaft 3, it is provided above cross bar 33 at helical blade 31 in rotating shaft 3, protruding 34 it are provided with on cross bar 33, protruding 34 is tapered protrusion；The bottom of described sandwich 2 is set to arc structure, and the bottom of sandwich 2 is provided with blow-off pipe 5, and blow-off pipe 5 is provided with valve 51, and the sidewall of sandwich 2 is provided with shower nozzle 4, and the water jet of described shower nozzle 4 matches with the bottom of sandwich 2；
Described helical blade 31 is provided with protruding I 32；Described sandwich 2 be internally provided with temperature sensor, temperature sensor is connected with the display screen 6 being arranged on sandwich 2 outer wall；The upper end of described tank body 1 is provided with charge door 11, and the sidewall of tank body 1 is provided with probe tube 12, air inlet pipe 13；
Described Spore cultivation base consists of the following composition: wheat bran 3.0%, magnesium sulfate 0.1%, potassium dihydrogen phosphate 0.2%, agar 2.4%, and surplus is water；
Being provided with culture medium in described seeding tank, culture medium consists of the following composition: cornstarch 3.0%, groundnut meal 1%, soybean cake powder 1%, dusty yeast 1%, calcium carbonate 0.2%, ammonium sulfate 0.2%, potassium dihydrogen phosphate 0.2%, amylase 0.03%, defoamer 0.2%, and surplus is water；
The condition of described fermented and cultured is: temperature is 25 DEG C, pressure be 0.02Mpa, pH be 5.6, fermentation time is 80 hours；
2), the acidifying of zymotic fluid: add oxalic acid and carry out acidification, be then filtrated to get acidified filtrate；
3), zymotic fluid isolated and purified: use sheet frame that acidified filtrate is carried out filtration treatment, filtrate after filtration is decoloured with 122 ion exchange resin, until filtrate light transmittance is entrance crystallizing tank crystallization after 90%, at in crystallizing tank, temperature is 8 DEG C, with ammoniacal liquor, the filtrate pH value after decolouring is adjusted to 4.4, then 50min it is incubated, it is centrifuged again separating, until wet crystal water content reaches 20% based on mass percentage concentration after Fen Liing, pneumatic conveying drying mode is used to be dried in the centrifugal wet crystal obtained, keeping EAT is 100 DEG C, finally obtain water content and be calculated as the dry powder of 9% by mass percentage concentration, gained dry powder is tetracycline powder.
Embodiment 2:
As it is shown in figure 1, preparation method based on the tetracycline improving ferment effect, comprise the following steps:
1), the preparation of zymotic fluid: will cultivate 5 days on streptomyces aureus spore inoculating to Spore cultivation base, until spore is ripe, then the spore of preparation is gone to seed tank culture, fermented and cultured is transferred to after seed tank culture, described seeding tank includes tank body 1, tank body 1 be internally provided with agitating device, the outer wall of tank body 1 is provided with sandwich 2, the lower end of described sandwich 2 is provided with water inlet 21, the upper end of sandwich 2 is provided with delivery port 22, described agitating device includes rotating shaft 3, helical blade 31 it is provided with in rotating shaft 3, it is provided above cross bar 33 at helical blade 31 in rotating shaft 3, protruding 34 it are provided with on cross bar 33, protruding 34 is tapered protrusion；The bottom of described sandwich 2 is set to arc structure, and the bottom of sandwich 2 is provided with blow-off pipe 5, and blow-off pipe 5 is provided with valve 51, and the sidewall of sandwich 2 is provided with shower nozzle 4, and the water jet of described shower nozzle 4 matches with the bottom of sandwich 2；
Described helical blade 31 is provided with protruding I 32；Described sandwich 2 be internally provided with temperature sensor, temperature sensor is connected with the display screen 6 being arranged on sandwich 2 outer wall；The upper end of described tank body 1 is provided with charge door 11, and the sidewall of tank body 1 is provided with probe tube 12, air inlet pipe 13；
Described Spore cultivation base consists of the following composition: wheat bran 3.8%, magnesium sulfate 0.3%, potassium dihydrogen phosphate 0.4%, agar 3.2%, and surplus is water；
Being provided with culture medium in described seeding tank, culture medium consists of the following composition: cornstarch 5.0%, groundnut meal 3%, soybean cake powder 3%, dusty yeast 2%, calcium carbonate 0.5%, ammonium sulfate 0.6%, potassium dihydrogen phosphate 0.4%, amylase 0.05%, defoamer 0.4%, and surplus is water；
The condition of described fermented and cultured is: temperature is 30 DEG C, pressure be 0.05Mpa, pH be 6.2, fermentation time is 72 hours；
2), the acidifying of zymotic fluid: add oxalic acid and carry out acidification, be then filtrated to get acidified filtrate；
3), zymotic fluid isolated and purified: use sheet frame that acidified filtrate is carried out filtration treatment, filtrate after filtration is decoloured with 122 ion exchange resin, until filtrate light transmittance is entrance crystallizing tank crystallization after 92%, at in crystallizing tank, temperature is 10 DEG C, with ammoniacal liquor, the filtrate pH value after decolouring is adjusted to 4.8, then 50min-60min it is incubated, it is centrifuged again separating, until wet crystal water content reaches 20% based on mass percentage concentration after Fen Liing, pneumatic conveying drying mode is used to be dried in the centrifugal wet crystal obtained, keeping EAT is 160 DEG C, finally obtain water content and be calculated as the dry powder of 9% by mass percentage concentration, gained dry powder is tetracycline powder.
Embodiment 3:
As it is shown in figure 1, preparation method based on the tetracycline improving ferment effect, comprise the following steps:
1), the preparation of zymotic fluid: will cultivate 5 days on streptomyces aureus spore inoculating to Spore cultivation base, until spore is ripe, then the spore of preparation is gone to seed tank culture, fermented and cultured is transferred to after seed tank culture, described seeding tank includes tank body 1, tank body 1 be internally provided with agitating device, the outer wall of tank body 1 is provided with sandwich 2, the lower end of described sandwich 2 is provided with water inlet 21, the upper end of sandwich 2 is provided with delivery port 22, described agitating device includes rotating shaft 3, helical blade 31 it is provided with in rotating shaft 3, it is provided above cross bar 33 at helical blade 31 in rotating shaft 3, protruding 34 it are provided with on cross bar 33, protruding 34 is tapered protrusion；The bottom of described sandwich 2 is set to arc structure, and the bottom of sandwich 2 is provided with blow-off pipe 5, and blow-off pipe 5 is provided with valve 51, and the sidewall of sandwich 2 is provided with shower nozzle 4, and the water jet of described shower nozzle 4 matches with the bottom of sandwich 2；
Described helical blade 31 is provided with protruding I 32；Described sandwich 2 be internally provided with temperature sensor, temperature sensor is connected with the display screen 6 being arranged on sandwich 2 outer wall；The upper end of described tank body 1 is provided with charge door 11, and the sidewall of tank body 1 is provided with probe tube 12, air inlet pipe 13；
Described Spore cultivation base consists of the following composition: wheat bran 3.3%, magnesium sulfate 0.2%, potassium dihydrogen phosphate 0.3%, agar 2.8%, and surplus is water；
Being provided with culture medium in described seeding tank, culture medium consists of the following composition: cornstarch 4.0%, groundnut meal 2%, soybean cake powder 2%, dusty yeast 1.5%, calcium carbonate 0.4%, ammonium sulfate 0.3%, potassium dihydrogen phosphate 0.3%, amylase 0.04%, defoamer 0.3%, surplus is water；
The condition of described fermented and cultured is: temperature is 28 DEG C, pressure be 0.03Mpa, pH be 5.8, fermentation time is 72 hours；
2), the acidifying of zymotic fluid: add oxalic acid and carry out acidification, be then filtrated to get acidified filtrate；
3), zymotic fluid isolated and purified: use sheet frame that acidified filtrate is carried out filtration treatment, filtrate after filtration is decoloured with 122 ion exchange resin, until filtrate light transmittance is entrance crystallizing tank crystallization after 90%, at in crystallizing tank, temperature is 9 DEG C, with ammoniacal liquor, the filtrate pH value after decolouring is adjusted to 4.6, then 550min it is incubated, it is centrifuged again separating, until wet crystal water content reaches 20% based on mass percentage concentration after Fen Liing, pneumatic conveying drying mode is used to be dried in the centrifugal wet crystal obtained, keeping EAT is 120 DEG C, finally obtain water content and be calculated as the dry powder of 9% by mass percentage concentration, gained dry powder is tetracycline powder.
Above-described detailed description of the invention; the purpose of the present invention, technical scheme and beneficial effect are further described; it is it should be understood that; the foregoing is only the detailed description of the invention of the present invention; the protection domain being not intended to limit the present invention; all within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. done, should be included within the scope of the present invention.
Claims (7)
1. preparation method based on the tetracycline improving ferment effect, it is characterised in that comprise the following steps:
1), the preparation of zymotic fluid: will cultivate 5 days on streptomyces aureus spore inoculating to Spore cultivation base, until spore is ripe, then the spore of preparation is gone to seed tank culture, fermented and cultured is transferred to after seed tank culture, described seeding tank includes tank body (1), tank body (1) be internally provided with agitating device, the outer wall of tank body (1) is provided with sandwich (2), the lower end of described sandwich (2) is provided with water inlet (21), the upper end of sandwich (2) is provided with delivery port (22), described agitating device includes rotating shaft (3), helical blade (31) it is provided with in rotating shaft (3), it is provided above cross bar (33) at helical blade (31) in rotating shaft (3), projection (34) it is provided with on cross bar (33), protruding (34) are tapered protrusion；The bottom of described sandwich (2) is set to arc structure, the bottom of sandwich (2) is provided with blow-off pipe (5), valve (51) it is provided with on blow-off pipe (5), being provided with shower nozzle (4) on the sidewall of sandwich (2), the water jet of described shower nozzle (4) matches with the bottom of sandwich (2)；
2), the acidifying of zymotic fluid: add oxalic acid and carry out acidification, be then filtrated to get acidified filtrate；
3), zymotic fluid isolated and purified: use sheet frame that acidified filtrate is carried out filtration treatment, filtrate after filtration is decoloured with 122 ion exchange resin, until entering crystallizing tank crystallization after filtrate light transmittance >=90%, at in crystallizing tank, temperature is 8 DEG C-10 DEG C, with ammoniacal liquor, the filtrate pH value after decolouring is adjusted to 4.4-4.8, then 50min-60min it is incubated, it is centrifuged again separating, until wet crystal water content reaches 20% based on mass percentage concentration after Fen Liing, pneumatic conveying drying mode is used to be dried in the centrifugal wet crystal obtained, keeping EAT is 100 DEG C-160 DEG C, finally obtain water content based on mass percentage concentration≤dry powder of 10%, gained dry powder is tetracycline powder.
Preparation method based on the tetracycline improving ferment effect the most according to claim 1, it is characterised in that described Spore cultivation base consists of the following composition: wheat bran 3.0%-3.8%, magnesium sulfate 0.1%-0.3%, potassium dihydrogen phosphate 0.2%-0.4%, agar 2.4%-3.2%, surplus is water.
Preparation method based on the tetracycline improving ferment effect the most according to claim 1, it is characterised in that be provided with culture medium in described seeding tank, culture medium consists of the following composition: cornstarch 3.0%-5.0%, groundnut meal 1%-3%, soybean cake powder 1%-3%, dusty yeast 1%-2%, calcium carbonate 0.2%-0.5%, ammonium sulfate 0.2%-0.6%, potassium dihydrogen phosphate 0.2%-0.4%, amylase 0.03%-0.05%, defoamer 0.2%-0.4%, surplus is water.
The most according to claim 1 based on the preparation method of tetracycline improving ferment effect, it is characterised in that the condition of described fermented and cultured is: temperature is 25 DEG C-30 DEG C, pressure be 0.02Mpa-0.05Mpa, pH be 5.6-6.2, fermentation time is more than 72 hours.
Preparation method based on the tetracycline improving ferment effect the most according to claim 1, it is characterised in that described helical blade (31) is provided with protruding I (32).
The most according to claim 1 based on the preparation method of tetracycline improving ferment effect, it is characterised in that described sandwich (2) be internally provided with temperature sensor, temperature sensor is connected with the display screen (6) being arranged on sandwich (2) outer wall.
Preparation method based on the tetracycline improving ferment effect the most according to claim 1, it is characterised in that the upper end of described tank body (1) is provided with charge door (11), and the sidewall of tank body (1) is provided with probe tube (12), air inlet pipe (13).
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| CN201610413732.2A CN105861611A (en) | 2016-06-14 | 2016-06-14 | Preparation method of tetracycline based on fermentation effect improvement |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106213122A (en) * | 2016-09-29 | 2016-12-14 | 芜湖市三山区绿色食品产业协会 | It is applicable to dehydrator and the operational approach thereof of nutritive powder |
| CN108191692A (en) * | 2017-12-25 | 2018-06-22 | 安徽永生堂药业有限责任公司 | A kind of process for separation and purification of tetracycline antibiotics |
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Application publication date: 20160817 |