CN1233650C - Lincomycin extracting process with binary extractant including benzyl alcohol and n-octyl alcohol - Google Patents
Lincomycin extracting process with binary extractant including benzyl alcohol and n-octyl alcohol Download PDFInfo
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- CN1233650C CN1233650C CN 03144332 CN03144332A CN1233650C CN 1233650 C CN1233650 C CN 1233650C CN 03144332 CN03144332 CN 03144332 CN 03144332 A CN03144332 A CN 03144332A CN 1233650 C CN1233650 C CN 1233650C
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Abstract
The present invention relates to a lincomycin extracting method using binary extraction agents including benzyl alcohol and n-octyl alcohol. The method has the technology: the benzyl alcohol and the n-octyl alcohol are mixed in the volume proportion of 60: 40 to 90: 10 at room temperature, processed lincomycin fermenting filter liquor is extracted, hydrochloric acid or sulphuric acid water solutions whose concentration is 0.01 to 1 M are used for back extraction, and products of lincomycin hydrochloride can be obtained after back extraction liquor is further refined. The binary extraction agents of the present invention have low toxicity, small environmental pollution and low harm for personnel, and working environment can be better improved. Extraction is operated near normal temperature and is easily controlled, and operating environment is improved. First-stage extraction rate is high, and higher economic benefit can be obtained. The present invention can be widely used for the field of biologic pharmaceutical industry.
Description
Technical field
The invention belongs to the antibiotic method of solvent extraction of field of biological pharmacy, particularly a kind of phenylcarbinol of using---the method for n-Octanol binary extraction agent extraction lincomycin.
Background technology
At present, it mainly is the butanols extraction process that the lincomycin that each manufacturer of China is adopted refines production technique, and this technology reports in 1996 documents that at " microorganism medicine chemistry and analysis " it is to be proposed in 1963 years by American Mason.Although this method is still used till today, exist shortcomings such as extraction agent consumption is big, energy consumption is high, operating environment difference.At " Chinese microbiotic magazine " 2002,27 (6): (332-336) disclose a kind of " the alcohol mixture extraction is in order to reduce the technical study of B component concentration in the lincomycin product " in the document, report adopts a kind of novel extraction agent alcohol mixture (extraction lincomycin of C8～C10) in the document, this extraction agent has well solved the water-soluble height of propyl carbinol, big this shortcoming of loss, but be to use this extraction agent solvent evaporates degree height, the smell is awful, percentage extraction also obviously descends than propyl carbinol simultaneously, disclose a kind of " improvement of antibiotic solvent extraction " in CN 1031334A patent documentation, this patent adopts isobutyl acetate to make extraction agent; Disclose a kind of " method of solvent extraction of lincolnensin " in CN 1044819A patent documentation, this patent adopts octanol to make extraction agent; At chemical industry metallurgical, 1994,15 (4): 330) disclose a kind of " research of oximes extraction U-10149 " in the document, report adopts oximes extraction U-10149 in the document; Disclose a kind of " extracting antibiotic with neutral organophosphorus (phosphine) kind of extractants from fermented liquid " in the CN1037343A patent documentation, this patent adopts lincomycin in the neutral organic phosphine compounds extractive fermentation liquid; Disclose a kind of " method of purifying lincomycin " in CN 1053790A patent documentation, this patent adopts the technology of long-chain alcohol in conjunction with neutral phosphine two-section extraction lincomycin.But the effect of extracting that these extraction agents reached all can not satisfy processing requirement fully.For example: neutral phosphorus extractant price comparison height, and toxic, influence final product quality; And oximes extraction agent reextraction process is difficult to realize.
Summary of the invention
The objective of the invention is to solve the solvent evaporates degree height that exists in the existing technology, the problem that percentage extraction is low and service temperature is high, thus provide that a kind of solvent evaporates degree is low, toxicity is little, percentage extraction is high and service temperature near normal temperature or room temperature the phenylcarbinol of use---n-Octanol binary extraction agent extracts the method for lincomycin.
Technical solution of the present invention is as follows:
With the method for phenylcarbinol-n-Octanol binary extraction agent extraction lincomycin, the processing step of present method is:
(1) preparation of binary extraction agent: be 60: 40～90: 10 mixed with volume ratio at room temperature, just make phenylcarbinol-n-Octanol binary extraction agent with phenylcarbinol and n-Octanol;
(2) the pH value of adjustment fermented filtrate of lincomycin: add sodium hydroxide solution in fermented filtrate of lincomycin, making its pH is 9～12;
(3) extraction: above-mentioned phenylcarbinol-n-Octanol binary extraction agent is joined through extracting in the fermented filtrate of lincomycin of above-mentioned processing, the volume ratio of fermented filtrate of lincomycin and binary extraction agent is 1～5: 1, extraction temperature is 20～40 ℃, 20～40 minutes extraction time, just obtain the lincomycin extraction liquid;
(4) strip: the hydrochloric acid or the aqueous sulfuric acid that add concentration and be 0.01～1M in the lincomycin extraction liquid are stripped, lincomycin extraction liquid and hydrochloric acid or vitriolic aqueous solution volume ratio are 1～4: 1, the reextraction temperature is 20～40 ℃, back-extraction time is 20～40 minutes, just obtains the lincomycin anti-stripping agent.
Content of lincomycin is equal to or greater than 2000u/ml in the fermented filtrate of lincomycin.
In the reextraction operation, the aqueous sulfuric acid that can also add concentration and be 0.01～1M in the lincomycin extraction liquid is stripped.The volume ratio of lincomycin extraction liquid and aqueous sulfuric acid is 1～4: 1, and the reextraction temperature is 20～40 ℃, and back-extraction time is 20～40 minutes.
Can obtain the product U 10149a after anti-stripping agent after stripping is further refining.
The present invention adopts phenylcarbinol---n-Octanol binary extraction agent extraction lincomycin.Phenylcarbinol and n-Octanol are the solvents that lincomycin is all had better extraction ability, and wherein the performance of phenylcarbinol is higher, play main extraction agent effect.Phenylcarbinol mixes with n-Octanol and uses the various objectives can satisfy simultaneously in the extraction process.(1) reduces system viscosity.N-Octanol can play the effect of thinner in system, effectively reduce system viscosity.(2) guarantee percentage extraction.Because n-Octanol has extraction ability to lincomycin, therefore, phenylcarbinol can significantly not reduce because of adding n-Octanol the high extraction ability of lincomycin.
The present invention compared with prior art has following advantage:
1, the physico-chemical property of binary extraction agent own is better, and solubleness (＜3%) and vapour pressure (0.13MPa) all are lower than propyl carbinol in the water of binary extraction agent under operational condition, and this binary extraction agent is lower toxicity, and environmental pollution is little, personnel is injured low.Particularly main extraction agent phenylcarbinol is a kind ofly can once be used for the analgesic agent of penicillin injection liquid by the rapid metabolic material of human body.The experiment scene shows that this binary extraction agent smell is significantly less than other extraction agents, can be good at improving Working environment.
2, extracting operation is easy to realize.This binary extraction agent service temperature is being operated near under the normal temperature, significantly is lower than the propyl carbinol that adopted in the present industrial production and the service temperature of alcohol mixture system (55～60 ℃), and is easy to control, has improved operating environment.This binary extraction agent improves 10% and 30% respectively than the one-level percentage extraction of the propyl carbinol that uses in the present industrial production, alcohol mixture extraction agent, can obtain higher economic benefit.
3, this binary extraction agent is stripped and is easy to realize that strip with acidified water, the one-level stripping rate can reach more than 95%.
Embodiment
Embodiment 1
The concrete processing step that extracts the method for lincomycin with phenylcarbinol-n-Octanol binary extraction agent is:
(1) preparation of binary extraction agent: be 90: 10 mixed with volume ratio at room temperature, just make phenylcarbinol-n-Octanol binary extraction agent with phenylcarbinol and n-Octanol;
(2) adjust the pH value of fermented filtrate of lincomycin: add sodium hydroxide solution in content of lincomycin is the fermented filtrate of lincomycin of 3126.50u/ml, making its pH is 12;
(3) extraction: above-mentioned phenylcarbinol-n-Octanol binary extraction agent is joined through extracting in the fermented filtrate of lincomycin of above-mentioned processing, the volume ratio of fermented filtrate of lincomycin and binary extraction agent is 7: 3, extraction temperature is 20 ℃, 20 minutes extraction time, just obtain the lincomycin extraction liquid.
Get lincomycin raffinate sample and measure with polarimetry, the raffinate concentration of tiring is 198.03u/ml, and the one-level percentage extraction can reach 93.67%.
(4) strip: the aqueous hydrochloric acid that adds concentration and be 0.1M in the lincomycin extraction liquid is stripped, the volume ratio of lincomycin extraction liquid and aqueous hydrochloric acid is 4: 1, the reextraction temperature is 40 ℃, and back-extraction time is 20 minutes, just obtains the lincomycin anti-stripping agent.
Get lincomycin anti-stripping agent sample and measure with polarimetry, the anti-stripping agent concentration of tiring is 2.62 ten thousand u/ml, and the one-level stripping rate can reach 96.90%.
The lincomycin corresponding typical curve relational expression with specific rotation of concentration of tiring is in the solution: y=3.18141 * 10
-4X is in the formula: the x-lincomycin concentration (u/ml) of tiring, y-specific rotation.
Embodiment 2
(1) preparation of binary extraction agent: be 60: 40 mixed with volume ratio at room temperature, just make phenylcarbinol-n-Octanol binary extraction agent with phenylcarbinol and n-Octanol;
(2) adjust the pH value of fermented filtrate of lincomycin: add sodium hydroxide solution in content of lincomycin is the fermented filtrate of lincomycin of 3069.92u/ml, making its pH is 12;
(3) extraction: above-mentioned phenylcarbinol-n-Octanol binary extraction agent is joined through extracting in the fermented filtrate of lincomycin of above-mentioned processing, the volume ratio of fermented filtrate of lincomycin and binary extraction agent 5: 1, extraction temperature is 40 ℃, 40 minutes extraction time, just obtains the lincomycin extraction liquid.
Get lincomycin raffinate sample and measure with polarimetry, the raffinate concentration of tiring is 166.59u/ml, and the one-level percentage extraction can reach 94.57%,
(4) strip: the aqueous hydrochloric acid that adds concentration and be 1M in the lincomycin extraction liquid is stripped, the volume ratio of lincomycin extraction liquid and aqueous hydrochloric acid is 1: 1, the reextraction temperature is 35 ℃, and back-extraction time is 30 minutes, just obtains the lincomycin anti-stripping agent.
Get lincomycin anti-stripping agent sample and measure with polarimetry, the anti-stripping agent concentration of tiring is 1.38 ten thousand u/m, and the one-level stripping rate can reach 95.21%.Typical curve relational expression and embodiment 1 are same,
Embodiment 3
(1) preparation of binary extraction agent: be 75: 25 mixed with volume ratio at room temperature, just make phenylcarbinol-n-Octanol binary extraction agent with phenylcarbinol and n-Octanol;
(2) adjust the pH value of fermented filtrate of lincomycin: add sodium hydroxide solution in content of lincomycin is the fermented filtrate of lincomycin of 3130.69u/ml, making its pH is 9.5;
(3) extraction: above-mentioned phenylcarbinol-n-Octanol binary extraction agent is joined through extracting in the fermented filtrate of lincomycin of above-mentioned processing, the volume ratio of fermented filtrate of lincomycin and binary extraction agent is 1: 1, extraction temperature is 40 ℃, 30 minutes extraction time, just obtain the lincomycin extraction liquid.
Get lincomycin raffinate sample and measure with polarimetry, the raffinate concentration of tiring is 203.26u/ml, one-level percentage extraction 93.57%.
(4) strip: the aqueous sulfuric acid that adds concentration and be 0.01M in the lincomycin extraction liquid is stripped, the volume ratio of lincomycin extraction liquid and aqueous sulfuric acid is 2: 1, the reextraction temperature is 20 ℃, and back-extraction time is 40 minutes, just obtains the lincomycin anti-stripping agent.
Get lincomycin anti-stripping agent sample and measure with polarimetry, the anti-stripping agent concentration of tiring is 5700.04u/ml, and the one-level stripping rate can reach 97.39%.Typical curve relational expression and embodiment 1 are together.
Claims (2)
1, a kind of method with phenylcarbinol-n-Octanol binary extraction agent extraction lincomycin, it is characterized in that: the processing step of present method comprises:
(1) preparation of binary extraction agent: be 60: 40～90: 10 mixed with volume ratio at room temperature, just make phenylcarbinol-n-Octanol binary extraction agent with phenylcarbinol and n-Octanol;
(2) the pH value of adjustment fermented filtrate of lincomycin: add sodium hydroxide solution in fermented filtrate of lincomycin, making its pH is 9～12;
(3) extraction: above-mentioned phenylcarbinol-n-Octanol binary extraction agent is joined through extracting in the fermented filtrate of lincomycin of above-mentioned processing, the volume ratio of fermented filtrate of lincomycin and binary extraction agent is 1～5: 1, extraction temperature is 20～40 ℃, 20～40 minutes extraction time, just obtain the lincomycin extraction liquid;
(4) strip: the hydrochloric acid or the aqueous sulfuric acid that add concentration and be 0.01～1M in the lincomycin extraction liquid are stripped, the volume ratio of lincomycin extraction liquid and hydrochloric acid or aqueous sulfuric acid is 1～4: 1, the reextraction temperature is 20～40 ℃, back-extraction time is 20～40 minutes, just obtains the lincomycin anti-stripping agent.
2, according to the said method with phenylcarbinol-n-Octanol binary extraction agent extraction lincomycin of claim 1, it is characterized in that: content of lincomycin is equal to or greater than 2000u/ml in the said fermented filtrate of lincomycin.
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| CN 03144332 CN1233650C (en) | 2003-09-25 | 2003-09-25 | Lincomycin extracting process with binary extractant including benzyl alcohol and n-octyl alcohol |
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| CN106279309B (en) * | 2015-06-26 | 2019-10-18 | 广东东阳光药业有限公司 | A kind of purification process of lincomycin |
| CN106770234A (en) * | 2016-12-03 | 2017-05-31 | 无锡艾科瑞思产品设计与研究有限公司 | A kind of lincomycin detection method and detection card |
| CN108801725B (en) * | 2018-04-03 | 2020-09-08 | 新宇药业股份有限公司 | Preparation method of component B reference substance in lincomycin hydrochloride |
| CN112920021B (en) * | 2021-02-01 | 2022-04-29 | 大连理工大学 | Method for extracting 1, 3-propylene glycol from fermentation liquor by using alcohol mixed solvent |
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