CN106279320A - A kind of extracting method of erythromycin lactate - Google Patents
A kind of extracting method of erythromycin lactate Download PDFInfo
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- CN106279320A CN106279320A CN201610700756.6A CN201610700756A CN106279320A CN 106279320 A CN106279320 A CN 106279320A CN 201610700756 A CN201610700756 A CN 201610700756A CN 106279320 A CN106279320 A CN 106279320A
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- erythromycin
- lactate
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- extraction
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/08—Hetero rings containing eight or more ring members, e.g. erythromycins
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
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- Saccharide Compounds (AREA)
Abstract
The present invention relates to the extracting method of a kind of erythromycin lactate, its processing step is: first adds erythromycin extraction solvent in erythromycin filtrate and extracts, gained erythromycin extract is after saturated nacl aqueous solution is dehydrated, add butyl lactate solution to crystallize, after having crystallized, separate through sucking filtration, be dried, obtain erythromycin lactate dry product.The present invention as extractant with erythromycin extraction solvent, completes erythromycin extraction and erythromycin lactate crystallizes.This erythromycin extraction solvent boiling range is high, and water solublity is little, volatilizees low with dissolving loss.
Description
Technical field
The present invention relates to biology and new medical technology, particularly relate to the extracting method of a kind of erythromycin lactate.
Background technology
In prior art, the extraction of erythromycin lactate is to extract erythromycin using butyl acetate as extractant, the most past
In extract, stream adds lactic acid solution, and reactive crystallization obtains erythromycin lactate.This technique is big due to butyl acetate water solublity, causes molten
Agent loss height, and butyl acetate boiling point is low, potential safety hazard is big, it is impossible to be applied to industrialized production.
Summary of the invention
It is an object of the invention to overcome the defect of above-mentioned prior art, it is provided that a kind of erythromycin extraction solvent replaces former
Some butyl acetates are as extractant, in the case of not reducing erythromycin lactate yield and product quality, reduce solvent loss
Extracting method with the erythromycin lactate of potential safety hazard.
The technical scheme the most just gone is:
The extracting method of a kind of erythromycin lactate, it is characterised in that its processing step is: first add in erythromycin filtrate
Entering erythromycin extraction solvent to extract, gained erythromycin extract saturated nacl aqueous solution is dehydrated, and then stream adds lactic acid fourth
Ester solution crystallizes, and after having crystallized, separates through sucking filtration, is dried, obtains erythromycin lactate dry product；
Described extraction pH is 9.5-11.0, extraction temperature 30～40 DEG C, extraction time 3-5min.
Described erythromycin extraction solvent extraction erythromycin concentration controls as 15000-35000 μ g/ml.
Consumption is erythromycin filtrate volume 0.1～0.3 times of described erythromycin extraction solvent.
Described erythromycin extract through saturated nacl aqueous solution dehydration is: under stirring, adds erythromycin extraction
Take liquid and amass the saturated nacl aqueous solution dehydration 30～60min of 2～10%, stratification, divide bottom solution with separatory funnel
Aqueous phase, erythromycin extract is continued to employ.
Described lactic acid butyl ester solution is the lactic acid solution with butyl acetate preparation, and dose volume ratio is for lactic acid: butyl acetate
=10～50:90～50 (V/V).
The consumption of described lactic acid butyl ester solution be dehydration after erythromycin extract volume 10%～50%.
Described temperature is 5～45 DEG C, crystallization time 60～180min, and crystallization terminal pH controls to be 4.0～6.5.
Described butyl lactate solution stream adds the time and controls at 60-180min.
The present invention solves in existing erythromycin lactate production technology, n-butyl acetate extraction technique and erythromycin lactate crystallization
During solvent loss and yield problem, owing to butyl acetate dissolubility in water is big, boiling point is low, extracts at erythromycin
Cheng Zhong, the dissolving of solvent and volatilizing loss are high.In the present invention, with commercially available erythromycin extraction solvent as extractant, complete red
Mycin extraction and erythromycin lactate crystallize.This erythromycin extraction solvent boiling range is high, and in water, dissolubility is low, so being lost low, as
Butyl acetate extracts in erythromycin lactate technique, butyl acetate loss in weight 1.35ml/g, and in the present invention, erythromycin extraction is molten
Matchmaker's loss in weight is 0.32ml/g, and erythromycin extraction solvent loss is less than 1.03 points of butyl acetate；Meanwhile, extract with erythromycin
Solvent replaces butyl acetate, the crystallization yield of erythromycin lactate and quality zero difference.Therefore, second is replaced with erythromycin extraction solvent
Acid butyl ester, makes erythromycin lactate extraction process become a kind of applicable process for stabilizing producing popularization.
Detailed description of the invention
It is explained the present invention below, it should be understood that example is for illustrating rather than this with example
The restriction of invention.The scope of the present invention is determined according to claims with core content.
In following embodiment
Erythromycin filtrate is originated Qiyuan Pharmaceutical Co., Ltd., Ningxia's erythromycin fermentation liquid plate-and-frame filtration.
Described erythromycin extraction solvent is commercially available Xi'an Li Jun group or yueyang, hunan or the second kills what that was offered for sale
Erythromycin extraction solvent.
Described lactic acid butyl acetate solution is for do solute with lactic acid, and butyl acetate does the solution of solvent preparation, volumetric concentration
10%～50%, collocation method is: lactic acid: butyl acetate volume ratio=10～50:90～50 (V/V), stands after stirring
More than 60min, divides and removes back water bottom solution.
Embodiment 1
Take and divide bisection with batch erythromycin filtrate, be separately added into isopyknic butyl acetate and erythromycin extraction solvent, extraction
Take unit and control 25000u/ml.Under agitation, after 30% sodium hydrate aqueous solution regulation pH of mixed to 9.5-11, stop
Stirring, stratification, divides and removes raffinate bottom solvent.Stay extract, under agitation, add the saturated chlorination of liquor capacity 2%
Sodium solution dehydration 30min, stratification, divides and removes back water bottom solvent, be the organic membrane filtration of 0.65u with aperture.
Under stirring, what dropping in solvent solutions prepared etc. is extracted toward erythromycin butyl acetate solution and erythromycin respectively
Amount butyl lactate solution, controls crystallization time 180min, crystallization temperature 35 DEG C, crystallizes terminal pH4.0-6.5, and crystallization terminates, and takes out
Filter separates 60min, accurately measures mother solution volume with graduated cylinder, and send mother solution detection residual titer.Erythromycin lactate wet product is dried
Weigh, censorship moisture and component.
Experimental result see table:
Embodiment 2
Take and divide bisection with batch erythromycin filtrate, be separately added into isopyknic butyl acetate and erythromycin extraction solvent, extraction
Take unit and control 20000u/ml.Under agitation, after 30% sodium hydrate aqueous solution regulation pH of mixed to 9.5-11, stop
Stirring, forbids layering, divides and removes raffinate bottom solvent.Stay extract, under agitation, add the saturated chlorination of liquor capacity 2%
Sodium solution dehydration 30min, stratification, divides and removes back water bottom solvent, with the organic membrane filtration of 0.65u.
Under stirring, what dropping in solvent solutions prepared etc. is extracted toward erythromycin butyl acetate solution and erythromycin respectively
Amount butyl lactate solution, controls crystallization time 180min, crystallization temperature 35 DEG C, crystallizes terminal pH4.0-6.5, and crystallization terminates, and takes out
Filter separates 60min, accurately measures mother solution volume with graduated cylinder, and send mother solution detection residual titer.Erythromycin lactate wet product is dried
Weigh, censorship moisture and component.
Experimental result see table:
Embodiment 3
Take and divide bisection with batch erythromycin filtrate, be separately added into isopyknic butyl acetate and erythromycin extraction solvent, extraction
Take unit and control 25000u/ml.Under agitation, after 30% sodium hydrate aqueous solution regulation pH of mixed to 9.5-11, stop
Stirring, forbids layering, divides and removes raffinate bottom solvent.Stay extract, under agitation, add the saturated chlorination of liquor capacity 2%
Sodium solution dehydration 30min, static layering, divide and remove back water bottom solvent, with the organic membrane filtration of 0.65u.
Under stirring, what dropping in solvent solutions prepared etc. is extracted toward erythromycin butyl acetate solution and erythromycin respectively
Amount butyl lactate solution, controls crystallization time 180min, crystallization temperature 35 DEG C, crystallizes terminal pH4.0-6.5, and crystallization terminates, and takes out
Filter separates 60min, accurately measures mother solution volume with graduated cylinder, and send mother solution detection residual titer.Erythromycin lactate wet product is dried
Weigh, censorship moisture and component.
Experimental result see table:
Claims (9)
1. the extracting method of an erythromycin lactate, it is characterised in that its processing step is: first add in erythromycin filtrate
Erythromycin extraction solvent extracts, and gained erythromycin extract saturated nacl aqueous solution is dehydrated, and then stream adds butyl lactate
Solution crystallizes, and after having crystallized, separates through sucking filtration, is dried, obtains erythromycin lactate dry product.
2. according to the extracting method of the erythromycin lactate described in claim 1, it is characterised in that described extraction pH is 9.5-11.0,
Extraction temperature 30～40 DEG C, extraction time 3-5min.
3. according to the extracting method of the erythromycin lactate described in claim 1, it is characterised in that described erythromycin extraction solvent extraction
Take erythromycin concentration to control as 15000-35000 μ g/ml.
4. according to the extracting method of the erythromycin lactate described in claim 1 or 3, it is characterised in that described erythromycin extraction solvent
Consumption is erythromycin filtrate volume 0.1～0.3 times.
5. according to the extracting method of the erythromycin lactate described in claim 1, it is characterised in that described erythromycin extract is through full
With sodium chloride solution dehydration be: under stirring, add erythromycin extract volume 2～10% saturated sodium-chloride molten
Fluid dewatering 30～60 min, stratification, divides solution bottom aqueous phase, erythromycin extract to continue to employ with separatory funnel.
6. according to the extracting method of the erythromycin lactate described in claim 1, it is characterised in that described lactic acid butyl ester solution is for using
The lactic acid solution of butyl acetate preparation, dose volume ratio is for lactic acid: butyl acetate=10 ~ 50:90 ~ 50.
7. according to the extracting method of the erythromycin lactate described in claim 1 or 6, it is characterised in that described lactic acid butyl ester solution
Consumption be dehydration after erythromycin extract volume 10%～50%.
8. according to the extracting method of the erythromycin lactate described in claim 1, it is characterised in that described temperature is 5～45 DEG C, knot
The brilliant time 60～180min, crystallization terminal pH controls to be 4.0～6.5.
9. according to the extracting method of the erythromycin lactate described in claim 1, it is characterised in that described butyl lactate solution stream adds
Time controls at 60-180min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610700756.6A CN106279320A (en) | 2016-08-22 | 2016-08-22 | A kind of extracting method of erythromycin lactate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610700756.6A CN106279320A (en) | 2016-08-22 | 2016-08-22 | A kind of extracting method of erythromycin lactate |
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| CN106279320A true CN106279320A (en) | 2017-01-04 |
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| CN201610700756.6A Pending CN106279320A (en) | 2016-08-22 | 2016-08-22 | A kind of extracting method of erythromycin lactate |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1013837A (en) * | 1962-12-07 | 1965-12-22 | Pierrel Spa | Erythromycin salts and esters |
| CN103275151A (en) * | 2013-05-08 | 2013-09-04 | 宁夏启元药业有限公司 | Refining method of erythromycin thiocyanate |
-
2016
- 2016-08-22 CN CN201610700756.6A patent/CN106279320A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1013837A (en) * | 1962-12-07 | 1965-12-22 | Pierrel Spa | Erythromycin salts and esters |
| CN103275151A (en) * | 2013-05-08 | 2013-09-04 | 宁夏启元药业有限公司 | Refining method of erythromycin thiocyanate |
Non-Patent Citations (2)
| Title |
|---|
| 李武德 等: "红霉素协同萃取新工艺研究", 《河南化工》 * |
| 胡麦霞 等: "新型萃取剂在红霉素提炼中应用研究", 《医药工程设计杂志》 * |
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Application publication date: 20170104 |