CN105524128B - A kind of continuous chromatography separating technology of Gentamicin C1a - Google Patents
A kind of continuous chromatography separating technology of Gentamicin C1a Download PDFInfo
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Abstract
The present invention relates to a kind of continuous separation purifying technique of Gentamicin C1a recovered liquid, the present invention realizes efficiently separating for Gentamicin C1a recovered liquid using continuous chromatography chromatography technique.By the Gentamicin C1a of recycling gained, into continuous chromatography system through adsorbing, washing miscellaneous, elution, collect eluent and chromatography column regeneration, the eluent of collection concentrates, Gentamicin C1a is obtained again, Gentamicin C1a yield using this law separation is high, and purity is high, at low cost, environmental protection is suitble to industrialized production.
Description
Technical field
The invention belongs to semi-synthetic chemical pharmacy fields, are related to the Gentamicin C1a recovered liquid side of isolating and purifying of high-purity
Method.
Background technology
Etimicin Sulfate (Etimicin sulfate) is that China scientific research personnel voluntarily develops, and possesses independent intellectual production
Efficient, less toxic, antimicrobial agent the semi-synthetic aminoglycoside antibiotics of a new generation of power is that unique first class national new drug that obtains is demonstrate,proved
The anti-infectives of book.This product is suitable for its sensitive Escherichia coli, Klebsiella pneumoniae, Serratia
Category, Citrobacter Freundii, Enterobacter, acinetobacter, Proteus, haemophilus influenzae, pseudomonas aeruginosa and grape
Various infection caused by coccus etc..Clinical studies show this product has a better effect following infection:Respiratory tract infection:It is such as acute
Bronchitis, acute exacerbation of chronic bronchitis, community's pulmonary infection etc..Kidney and urogenital infections:Such as acute kidney
Meng's ephritis, cystitis, chronic pyelonephritis or chronic cystitis acute attack etc..Skin soft tissue and other infection:Such as skin
And soft tissue infection, wound, wound and the infection in postpartum of performing the operation and other sensitive bacterias infect.There is lower ear, kidney poison simultaneously
Property adverse reaction rate, it was demonstrated that Etimicin Sulfate be in clinical application efficiently, the semi-synthetic amino sugar of a new generation of safety
Tobramycin antibiotic.
Currently, the technique that production Etimicin Sulfate uses is the technique (application number of patent report：
93112412.3).It is mainly comprised the following steps：Zinc acetate, acetic anhydride is added in Gentamicin C1a alkali in a solvent, generates 3,2 ", 6 " ,-
Three-N- acetyl group Gentamicin C1as (P1) are concentrated by extraction, and concentrate is passed through hydrogen sulfide gas and removes zinc ion, through preliminary
The P1 that isolated purity is 90%, is then added acetaldehyde, is hydrogenated with reducing agent in 0~5 DEG C of ice-water bath, obtain 3,2 ",
6 ",-three-N- acetyl group -1-N-EthagentamycinC1a (Etimicin) obtains purity after the separation of absorbent-type macroreticular resin
The sodium hydroxide solution of 1N, hydrolysis reflux 48 hours, hydrolyzate warp is added in higher Etimicin, the higher Etimicin of purity
1-N-EthagentamycinC1a (Etimicin) solution that the isolated purity of absorbent-type macroreticular resin is 90% or more, acid adding
At salt, activated carbon decolorizing is freeze-dried to get Etimicin salt.
There is a large amount of Gentamicin C1a to remain in Etimicin eluent, by recycling Gentamicin C1a, can save
Cost.But having substantial portion of impurity in Gentamicin C1a recovered liquid, such as 1-N- ethyls garamine, 6, " celebrating of-N- ethyls is big
Mycin C1a, 1-N- ethyl gentamicinC2 b etc., these impurity structures are similar to Gentamicin C1a, more difficult with traditional fixed bed
It removes, it is therefore desirable to develop efficient process for separating and purifying, to improve product quality, advocate Green Chemistry.
Invention content
The method of recommendation is
The purpose of the present invention is to provide a kind of methods for the Gentamicin C1a obtaining high-purity-using continuous chromatography point
Gentamicin recovered liquid is set more effectively to be isolated and purified from system.
The structural formula of Gentamicin C1a is as follows：
Chemical name is as follows：
O-3-deoxy-4-C-methyl-3-(methylamino)-β-L-arabinopyranosyl-(1→6)-O-
[2,6-diamino-2,3,4,6-tetradeoxy-α-D-erythro-hexopyranosyl-(1→4)]-2-deo xy-D-
Streptamine
The purpose of the present invention can obtain by the following technical programs：
A. continuous chromatography column on recovered liquid divides the decorrelation impurity ("-N- ethyl gentamicins of 1-N- ethyls garamine, 6
C1a, 1-N- ethyl gentamicinC2 b etc.), obtain the Gentamicin C1a of high-purity；
B. it being concentrated under reduced pressure again with heating, operating condition is 0.02~0.15Mpa of vacuum degree, and operation temperature is 35~90 DEG C,
It is 15%~70% to be concentrated into Gentamicin C1a mass concentration；
C. concentrate ELSD measures Gentamicin C1a purity >=90%；
Described to utilize continuous chromatography isolation technics, it is big mould that the Gentamicin C1a recovered liquid of upper continuous chromatography column is diluted to celebrating
Plain C1a mass concentrations control is 1%~40%.
It is described to utilize continuous chromatography isolation technics, Gentamicin C1a is isolated and purified in Gentamicin C1a recovered liquid, is adopted
Chromatographic column quantity is 10~20, resin D103, HPD100, China shake chromatography No. 1, China shake chromatography No. 2, JK006,
DK110, D110, DK-1, D101, YPR- II etc., resin aperture are 30~100 mesh, the chromatographic column in each area be respectively adopted series connection or
Parallel way connects；The areas Xi Za purifying water washing；Desorption zone using ethanol solution elute, desorption solvent be 3wt%~
20wt% ethanol solutions；Regeneration activating area uses ethyl alcohol, water to replace activating and regenerating successively.
It is further recommended that
Continuous chromatography disk conveying type continuous chromatography piece-rate system or the separation of Simulation moving bed formula continuous chromatography
System can reach the desired effect of the present invention.
(1) technique of Simulation moving bed formula continuous chromatography piece-rate system separating-purifying Gentamicin C1a：
According to the characteristic of each ingredient in Gentamicin C1a recovered liquid, the selected resin of the present invention is macroporous absorbent resin,
Resin particle diameter is in 30~100 mesh, 95% or more the uniformity.
Simulation moving bed formula continuous chromatography piece-rate system is divided into adsorption zone, the areas Xi Za, desorption zone, four, regeneration washing area
Area.
1) adsorption zone：1 column；Coutroi velocity, Gentamicin C1a recovered liquid enter from 11 or No. 1 columns.
2) areas Xi Za：3~6 columns；After absorption, resin column goes to the areas Xi Za, coutroi velocity.
3) desorption zone：5~10 columns；It is connect for series and parallel between each pillar.Coutroi velocity, using the ethyl alcohol of various concentration
Desorption, and all using positive charging.
4) regeneration washing area：1~5 column；Coutroi velocity, it is forward and inverse to independent charging；Eluant, eluent recycles.
Simulation moving bed formula continuous chromatography piece-rate system described in step (1) generally comprises constant flow pump, jacketed ion is handed over
Change column, control valve, pH meter, thermometer.
Simulation moving bed formula continuous chromatography piece-rate system described in step (1), needs the inlet and outlet by each area along material
Liquid flow direction carries out periodical switching respectively, collects eluent.
The described periodical switching refers to, by adjusting feeding liquid, washing miscellaneous dose, the flow of eluant, eluent, regenerative agent so that each
After first pillar processing completely in area, while next area is switched into, becomes last root pillar in next area, execute next
Area's flow.
First, each area pillar refers to the pillar at each area's liquid-inlet.
First, each area pillar is handled all referring to first pillar adsorption saturation of adsorption zone, first, the areas Xi Za
Pillar impurity is washed off completely；The pillar Gentamicin C1a of desorption zone first is eluted completely；The pillar resin of renewing zone first is complete
It is reproduced entirely, next round absorption can be met.
(2) disk conveying type continuous chromatography piece-rate system separating-purifying Gentamicin C1a technique：
Disk conveying type continuous chromatography piece-rate system is divided into adsorption zone, the areas Xi Za, desorption zone, area of four, regeneration washing area.
1) adsorption zone：1~3 unit；Coutroi velocity, hydrolyzate enter from 11 or No. 5 units.
2) areas Xi Za：1~10 unit；After absorption, resin column goes to the areas Xi Za, coutroi velocity.
3) desorption zone：5~12 units；Each outlet solution is collected respectively with continuous, gradient desorption mode in the desorption zone
Imbibition.
4) regeneration washing area：1~5 unit；Individually charging, and be suitable, backward feed, eluant, eluent recycles.
The benefit of the present invention：
1) all steps of fixed-bed process are all integrated into a set of process system, simple system, and reduce technique
The arrangement of pipeline；Floor space saves 80%, and factory building height only needs the 1/3 of fixed bed height, the fixation of same production capacity
Assets investment saves 30% or more.
2) resin utilization rate is high, and product design, purity and yield optimize；Present invention process detaches work with fixed-bed resin
Skill compares, resin demand be only original 30%, and can be easily achieved forward and inverse stream inside resin and switch, with
Loose resin prevents from luming.
3) dosage for reducing chemical reagent and water, reduces the discharge of waste water；This technique realizes eluting solvent and returns set use,
Achieve the purpose that recycle.
4) system compact, and self-con-tained unit is used, reduce work load.
5) production efficiency is improved, production capacity is improved, when the production cycle reduces 1/3 relative to former fixed-bed resin separating technology
Between.
Description of the drawings
One continuous chromatography of figure isolates and purifies the flow chart of Gentamicin C1a
Specific implementation mode
Embodiment 1：
It is described in detail with reference to Fig. 1 and embodiment：
Resin selected by the present invention is that China's shake chromatographs No. 1 resin, and resin grain size is 100 95% or more mesh, and each resin column is filled out
Loading amount is 0.08m3, resin column capacity is 0.1m3, practical filling ratio is 80%.System overall size is 3m × 3m × 5m (long × wide
× high).
Disk conveying type continuous chromatography piece-rate system detaches the following region of Gentamicin C1a point:
1) adsorption zone：(No. 11 units)
The region shares 1 unit (No. 11 units), and by flow control, raw material initially enters No. 11 units, then passes through
Series connection into No. 12 units wash miscellaneous.
2) areas Xi Za：(10,12~No. 14 units)
After absorption, each resin needs to wash, and is located at before and after adsorption zone.After resin column rotates to absorption water wash zone, folder
Band is ejected in the feed liquid (mainly clarified solution) of interlaminar resin by water, and efflux mixes together with the efflux of No. 11 units of adsorption zone
Into No. 12 units.It washes away the feed liquid for being mixed in resin gap and takes away impurity as possible, prevent feed liquid entrainment from entering desorption zone,
The purity of stripping liquid is improved, and its water lotion is entered into adsorption zone, adsorbs the active principle in water lotion again.
3) desorption zone (3~No. 9 units)
It is collected elution Gentamicin C1a with continuous, gradient desorption mode in the desorption zone and exports stripping liquid, according to technique
Method design is divided into following several parts：
I 7~No. 9 are connected into 3wt% ethanol solutions, and stripping liquid enters No. 12 units；
II 4~No. 6 series connection, No. 4 units are adjusted to 5 wt% into purified water, by the ethanol solution concentration for entering the region, and 6
Number outlet stripping liquid collect be mainly Gentamicin C1a；
III No. 3 are connected into 10wt% ethanol solutions, and stripping liquid enters No. 4 units
4) regeneration washing area (1, No. 2 unit)；
Two, area unit is individually fed, and is reverse or forward feed.
Wherein No. 2 are 95% ethanol solution；No. 1 is purified water；
This example main design parameters are as follows：
Adsorption zone：Inlet amount 30L/hr；Resin total amount 0.08m3
60L/hr is washed after absorption；
Desorption zone：Purified water 1：120L/hr；Ethanol solution 1 (3wt% ethanol solutions)：120L/hr；Ethanol solution 2
(10wt% ethanol solutions)：270L/hr, purified water 2：270L/hr.
Renewing zone：Each unit regenerates：95% ethyl alcohol washes 120L/hr；Wash 120L/hr.
Embodiment 2：
It is described in detail with reference to Fig. 1 and embodiment：
Resin selected by the present invention is II resins of YPR-, and resin is 80 mesh, and each resin column amount of fill is 0.08m3, resin column
Capacity is 0.1m3, practical filling ratio is 80%.System overall size is about 3m × 3m × 5m (length × width × height).
Simulation moving bed formula continuous chromatography piece-rate system detaches the following region of Gentamicin C1a point:
1) adsorption zone：(No. 11 units)
The region shares 1 unit (No. 11 units), and by flow control, raw material initially enters No. 11 units, then passes through
Series connection into No. 12 units wash miscellaneous.
2) areas Xi Za：(10,12~No. 14 units)
After absorption, each resin needs to wash, and is located at before and after adsorption zone.After resin column rotates to absorption water wash zone, folder
Band is ejected in the feed liquid (mainly clarified solution) of interlaminar resin by water, and efflux mixes together with the efflux of No. 11 units of adsorption zone
Into No. 12 units.It washes away the feed liquid for being mixed in resin gap and takes away impurity as possible, prevent feed liquid entrainment from entering desorption zone,
The purity of stripping liquid is improved, and its water lotion is entered into adsorption zone, adsorbs the active principle in water lotion again.
3) desorption zone (3~No. 9 units)
It is collected elution Gentamicin C1a with continuous, gradient desorption mode in the desorption zone and exports stripping liquid, according to technique
Method design is divided into following several parts：
I 7~No. 9 are connected into 5wt% ethanol solutions, and stripping liquid enters No. 12 units；
II 4~No. 6 series connection, No. 4 units are adjusted to 10wt% into purified water, by the ethanol solution concentration for entering the region,
It is mainly Gentamicin C1a that stripping liquid, which is collected,；
III No. 3 are connected into 15wt% ethanol solutions, and stripping liquid enters No. 4 units
4) regeneration washing area (1, No. 2 unit)；
Two, area unit is individually fed, and is reverse or forward feed.
Wherein No. 2 are 95% ethanol solution；No. 1 is purified water；
This example main design parameters are as follows：
Adsorption zone：Inlet amount 50L/hr；Resin total amount 0.08m3
50L/hr is washed after absorption；
Desorption zone：Purified water 1：120L/hr；Ethanol solution 1 (5wt% ethanol solutions)：120L/hr；Ethanol solution 2
(15wt% ethanol solutions)：270L/hr, purified water 2：270L/hr.
Renewing zone：Each unit regenerates：95% ethyl alcohol washes 100L/hr；Wash 100L/hr.
Separation purity：No. 6 are collected the requirement that part disclosure satisfy that downstream process；Gentamicin C1a is complete with other components
It separates.
In this continuous chromatography piece-rate system, accomplished batch in reuse, the water lotion after absorption comes back to adsorption zone, subtracts
Loss when absorption, and the active principle fully in exchange adsorption feed liquid are lacked；Water scouring water after regeneration be back to use wash it is miscellaneous
In desorption reagent, water and reagent have all been accomplished to recycle.
20 DEG C of simulated moving bed system operating temperature.Feeding liquid entrance, eluant, eluent entrance, eluent outlet and waste liquid are gone out
Opening's edge feed solution flow direction and carries out periodical switching respectively, collects eluent.Periodically switching refer to by adjust feeding liquid,
Wash miscellaneous dose, the flow of eluant, eluent, regenerative agent so that after first pillar processing completely in each area, switch into next area, become
Last root pillar in next area, executes next area's flow.
The pillar processing of first, the areas Shu Ge is all referring to first pillar adsorption saturation of adsorption zone, first, the areas Xi Za column
Sub- impurity is washed off completely；The pillar Gentamicin C1a of desorption zone first is eluted completely；The pillar resin of renewing zone first is complete
It is reproduced, next round absorption can be met.
Analysis of performance cost：
The operating cost of continuous chromatography piece-rate system is concentrated mainly on resin, ethanol solution, purified water this three parts, principal series
The electrisity consumption of system is few.In the case where feeding 700L/d, system resin demand is 1.2m3, the service life is as fixed bed；
Ethyl alcohol, water：95% ethyl alcohol 4500L/d (wherein 80% recovery)；Water consumption 15T/d.
Economic and Efficiency Analysis：
1. reducing resin demand, the consumption of regenerative agent and water is reduced；
Resin demand reduces 50%, and ethanol consumption reduces 50%, and water consumption reduces 50%.
2. purity improves；Purity originally can reach 95% or more now generally 90% or so.
3. continuous chromatography piece-rate system also brings the reduction of floor space, the simplicity of operation, production cycle shortening etc. many
Benefit.
Claims (1)
1. a kind of continuous chromatography chromatography purification process of Gentamicin C1a recovered liquid, which is characterized in that steps are as follows：
Continuous chromatography column on Gentamicin C1a hydrolyzate, divides decorrelation impurity, obtains the Gentamicin C1a stripping liquid of high-purity,
Stripping liquid is further concentrated under reduced pressure with heating, and operating condition is 0.02 ~ 0.15MPa of vacuum degree, and operation temperature is 30 ~ 90 DEG C, dense
The mass concentration for being reduced to Gentamicin C1a is 15% ~ 70%,
The wherein described continuous chromatography column, the resin be China shake chromatograph No. 1 resin, resin grain size be 100 mesh, the uniformity 95% with
On, each resin column amount of fill is 0. 08m3, and resin column capacity is 0.1 m3, and practical filling ratio is 80%, and system overall size is long
× wide × a height of 3m × 3m × 5m,
Continuous chromatography column selects disk conveying type continuous chromatography piece-rate system, the following region of the system point:
1）Adsorption zone：No. 11 units
The region shares 1 unit, is No. 11 units, by flow control, raw material initially enters No. 11 units, then passes through series connection
Into No. 12 units wash it is miscellaneous,
2）The areas Xi Za：10,12 ~ No. 14 units
After absorption, each resin needs to wash, and is located at before and after adsorption zone, after resin column rotates to absorption water wash zone, is entrained in
The feed liquid of interlaminar resin is ejected by water, and the efflux of No. 11 units of efflux and adsorption zone mixes enters No. 12 units together, washes away
It is mixed in the feed liquid of resin gap and takes away impurity as possible, prevent feed liquid entrainment from entering desorption zone, improve the purity of stripping liquid,
And its water lotion is entered into adsorption zone, the active principle in water lotion is adsorbed again,
3）Desorption zone：3 ~ No. 9 units
In the desorption zone, with continuous, gradient desorption mode, collect elution Gentamicin C1a and export stripping liquid, desorption divide into as
Under several parts：
I 7 ~ No. 9 are connected into 3 wt% ethanol solutions, and stripping liquid enters No. 12 units；
II 4 ~ No. 6 series connection, No. 4 units are adjusted to 5 wt% into purified water, by the ethanol solution concentration for entering the region, and No. 6 go out
It is mainly Gentamicin C1a that mouth stripping liquid, which is collected,；
III No. 3 are connected into 10 wt% ethanol solutions, and stripping liquid enters No. 4 units,
4）Regeneration washing area：1, No. 2 units
Two, area unit is individually fed, and is reverse or forward feed, wherein No. 2 are 95% ethanol solution；No. 1 is purifying
Water,
Wherein：
Adsorption zone：Inlet amount 30L/hr；Resin total amount 0.08m3,
60L/hr is washed after absorption；
Desorption zone：Purified water 1：120L/hr；Ethanol solution 1：3 wt% ethanol solutions：120L/hr；Ethanol solution 2：10 wt% second
Alcoholic solution：270L/hr, purified water 2：270L/hr,
Renewing zone：Each unit regenerates：95% ethyl alcohol washes 120L/hr；Wash 120L/hr.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106498011A (en) * | 2016-11-28 | 2017-03-15 | 无锡福祈制药有限公司 | A kind of preparation method of Gentamicin C1a |
| CN107619421B (en) * | 2017-09-19 | 2018-10-12 | 江西国药有限责任公司 | The continuous chromatography isolation and purification method of lincomycin |
| CN110862427B (en) * | 2018-08-28 | 2024-04-23 | 河南仁华生物科技有限公司 | Purification method of gentamicin C1a |
| CN109438527A (en) * | 2018-09-20 | 2019-03-08 | 无锡济民可信山禾药业股份有限公司 | A method of recycling Gentamicin C1a from Etimicin sulfate intermediate synthesising by-product |
| CN109651087B (en) * | 2019-01-30 | 2020-12-04 | 南京工业大学 | Process for separating butanetriol fermentation liquor by using continuous chromatography technology |
| CN110054655B (en) * | 2019-05-23 | 2022-06-07 | 无锡济煜山禾药业股份有限公司 | Preparation method of high-purity gentamicin C1a sulfate |
| CN110563782B (en) * | 2019-09-29 | 2022-08-30 | 常州方圆制药有限公司 | Gentamicin C 1a Purification method of (2) |
| CN112730666A (en) * | 2020-12-23 | 2021-04-30 | 无锡济煜山禾药业股份有限公司 | Method for detecting content of gentamicin C1a alkali freeze-dried powder C1a |
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Address after: 214028 Changjiang South Road, new Wu District, Wuxi, Jiangsu Province, No. 12 Co-patentee after: Jiangxi Jinshuibao Pharmaceutical Co.,Ltd. Patentee after: Wuxi Jiyu Shanhe Pharmaceutical Co., Ltd Address before: 214028 No. 12 Changjiang South Road, New District, Jiangsu, Wuxi Co-patentee before: JIANGXI JIMINKEXIN JINSHUIBAO PHARMACEUTICAL Co.,Ltd. Patentee before: WUXI JIMIN KEXIN SHANHE PHARMACEUTICAL Co.,Ltd. |