CN102286044A - Preparation method of natamycin laminar crystal - Google Patents
Preparation method of natamycin laminar crystal Download PDFInfo
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- CN102286044A CN102286044A CN2011102424851A CN201110242485A CN102286044A CN 102286044 A CN102286044 A CN 102286044A CN 2011102424851 A CN2011102424851 A CN 2011102424851A CN 201110242485 A CN201110242485 A CN 201110242485A CN 102286044 A CN102286044 A CN 102286044A
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Abstract
The invention relates to a preparation method of a natamycin laminar crystal, and the preparation method comprises the following steps: (1) adding natamycin mycelium into a methanol and water mixed liquid, wherein the volume ratio of methanol to water is (60-90):(40-10); (2) adjusting the pH value to 10-12 with a basic substance; (3) carrying out liquid-solid separation and collecting filtrate to obtain a natamycin extract; (4) concentrating the extract until the content of natamycin is 18-26 mg/mL, and flocculating to remove insoluble substances to obtain a natamycin fine extract; (5) acidifying the natamycin fine extract by two stages: firstly dripping acid slowly until the pH value decreases to 8-9, then stirring for more than 1 hour, then slowly dripping the acid until the pH value decreases to 6-7, and then stirring for more than 3 hours to obtain a crystallization liquid of the laminar natamycin crystal; and (6) carrying out liquid-solid separation and drying in vacuum to obtain the laminar natamycin crystal. By adoption of the preparation method provided by the invention, the uniform natamycin laminar crystal can be prepared, the subsequent crystal washing and drying difficulties are reduced, and the crystal filtering and drying time is shortened.
Description
Technical field
The present invention relates to a kind of method that from mycelium, prepares the tennecetin tabular crystal.
Background technology
Tennecetin (Natamycin) claims that again pimaricin (Pimaricin) is a kind of polyene macrolide antibiotics, and it can suppress the growth of yeast and mould, and does not act on the normal microflora in the human intestinal.The follow-up study and the evaluation of application facet just tennecetin have been carried out from China foodstuff additive council in 1996, the national standard of formally putting into effect tennecetin in 2011 is used for the course of processing of food such as cheese, cake, meat intestines as antimildew agent for food.
The tennecetin molecular formula is C33H47NO13; Molecular weight is 665.75 dalton; Be amphoteric substance, iso-electric point is 6.5.
Tennecetin is produced by streptomycete fermentation, and fermented liquid is collected mycelium after liquid-solid separation, by the method for adding organic solvent and regulating pH, finally can obtain the crystal of tennecetin.The crystalline substance of tennecetin is practised two kinds of sheet and needle-likes, and they all belong to α-tennecetin crystallographic system.
In the separation and purification process of tennecetin, the not isomorphous of tennecetin is practised can influence tennecetin crystalline filtration velocity and time of drying.Needle-like is brilliant to be practised and is easy to coalescent agglomeratingly, is easy to again wrap up impurity when coalescent and influences purity, increases filtration, washing and drying difficulty simultaneously.The tennecetin crystal that the extracting method that employing Chinese patent CN101062934A announces makes is short acicular or unbodied, is unfavorable for that the tennecetin crystalline filters and drying, and filtration and time of drying are all longer.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of tennecetin tabular crystal, it can make the tennecetin tabular crystal of homogeneous, thereby reduces follow-up crystal washing and drying difficulty, shortens crystalline and filters and time of drying.
Technical solution of the present invention is to constitute like this: a kind of preparation method of tennecetin tabular crystal is characterized in that: it may further comprise the steps:
A, get in the mixed solution that the tennecetin mycelium adds methyl alcohol and water; In the mixed solution of described methyl alcohol and water, the volume ratio of methyl alcohol and water is 60-90: 40-10; The mixed solution of every 1L methyl alcohol and water adds 90-110g tennecetin mycelium;
The pH value of b, the solution that obtains with the even stirring and adjusting step of alkaline matter a is dissolved in the mixing solutions tennecetin to 10-12;
C, the solution that step b is obtained carry out liquid-solid separation, collect the extracting solution that filtrate obtains tennecetin;
The extracting solution of the tennecetin that d, enrichment step c obtain to tennecetin content between 18～26mg/ml, and flocculation removes the insolubles of separating out in this process, obtain the smart extracting solution of tennecetin;
The smart extracting solution of the tennecetin of e, acidification step d acquisition in two stages:
Fs slowly drips acid while stirring the smart extracting solution of tennecetin, makes the pH value of the smart extracting solution of tennecetin progressively be reduced to 8-9, and under the situation that the pH value is no longer gone up, restir is more than 1 hour;
Subordinate phase continues slowly to drip acid while stirring the smart extracting solution of tennecetin, make the pH value of the smart extracting solution of tennecetin progressively be reduced to 6-7, under the situation that the pH value is no longer gone up, restir obtained flaky tennecetin crystalline crystal solution more than 3 hours;
F, the tennecetin crystalline crystal solution that step e is obtained are carried out liquid-solid separation, and vacuum-drying obtains sheet tennecetin crystal then.
Preparation principle of the present invention is described as follows: applicant of the present invention practises crystalline substance by the content of discovering methyl alcohol in the tennecetin extracting solution very big influence, and growing the grain technology can be improved the size distribution of tabular crystal in the crystallisation process of tennecetin, improves tennecetin crystalline purity.According to above 2 points, the present invention adopts the mixed solution of a certain proportion of methyl alcohol and water to extract from the tennecetin mycelium and the purifying tennecetin, then by crystallization and growing the grain technology, the smart extracting solution of acidifying tennecetin stage by stage, thus prepare the higher tennecetin crystal of flaky purity.The purpose of the smart extracting solution of acidifying tennecetin is stage by stage: in the fs, make the pH value of the smart extracting solution of tennecetin that the decline of control slowly be arranged by dripping acid, the solubleness that the reduction tennecetin of control is promptly slowly arranged prevents that the phenomenon of tennecetin outburst nucleation from occurring; Crystallization this moment and dissolving tend to be balanced, and be beneficial to crystalline and grow up, but solubleness was bigger this moment, and the words yield of direct filtration is low, so steadily pH is continued to regulate to subordinate phase in the back, reach the iso-electric point of tennecetin, solubleness minimum, yield height this moment.If directly be transferred to iso-electric point, tennecetin rapid crystallization then, the crystal size heterogeneity that obtains and parcel impurity.The purpose that subordinate phase continues slowly and controlledly to regulate pH value to 6～7 is to make the surface that mainly occurs in established nucleus of separating out of tennecetin, and the tennecetin tabular crystal particle that obtains thus greatly, size-grade distribution is more even, and purity is higher.
Compared to prior art, the invention has the advantages that: the present invention is an object with the mycelium of tennecetin culture, by methyl alcohol and the ratio of water and the crystallisation process of tennecetin in the control extracting solution, thereby can make the tennecetin tabular crystal of homogeneous, reducing follow-up crystal filters and drying difficulty, shorten crystalline and filter and time of drying, be convenient to industrialized production control.
Description of drawings
Fig. 1 is the photomicrography crystal morphology figure of embodiment 1 gained tabular crystal.
Fig. 2 is embodiment 4 gained crystalline photomicrography crystal morphology figure.
Fig. 3 is the group 9 gained crystalline photomicrography crystal morphology figure that the contrast experiment organizes.
Embodiment
Below in conjunction with embodiment, embodiment and Figure of description content of the present invention is elaborated:
One, embodiment:
The specific embodiment of the invention provides a kind of preparation method of tennecetin tabular crystal, it is characterized in that: it may further comprise the steps:
A, get in the mixed solution that the tennecetin mycelium adds methyl alcohol and water; In the mixed solution of described methyl alcohol and water, the volume ratio of methyl alcohol and water is 60-90: 40-10; The mixed solution of every 1L methyl alcohol and water adds 90-110g tennecetin mycelium;
Tennecetin mycelium described in this step is wet mycelium or the dry mycelium that natamycin fermentation liquor obtains by liquid-solid isolation technique, the dry mycelium of preferred moisture content≤5%.Certainly, also can adopt wet mycelium,, then preferably measure the moisture content of wet mycelium in advance, like this ratio that can suitable corresponding minimizing water when the mixed solution of preparation methyl alcohol and water if the water content of wet mycelium is higher.The volume ratio of described methyl alcohol and water is preferably 73: 27, and the mixed solution of every 1L methyl alcohol and water preferably adds 100g tennecetin mycelium.
The pH value of b, the solution that obtains with the even stirring and adjusting step of alkaline matter a is dissolved in the mixing solutions tennecetin to 10-12;
The described alkaline matter of this step is preferably sodium hydroxide or ammoniacal liquor etc., is the industrial extremely alkaline material of regulator solution commonly used.
C, the solution that step b is obtained carry out liquid-solid separation, collect the extracting solution that filtrate obtains tennecetin;
The described solid separation method of this step can adopt in the microbiotic leaching process solid separation method commonly used,, suction filtration centrifugal, cross flow filter etc. as Plate Filtration, gravity, and its purpose is to remove the bacterium slag, collects filtrate to obtain the extracting solution of tennecetin.
The extracting solution of the tennecetin that d, enrichment step c obtain to tennecetin content between 18～26mg/ml, and flocculation removes the insolubles of separating out in this process, obtain the smart extracting solution of tennecetin;
The described concentration method of this step can adopt vacuum concentration method commonly used.
The smart extracting solution of the tennecetin of e, acidification step d acquisition in two stages:
Fs slowly drips acid while stirring the smart extracting solution of tennecetin, (optimum value is decided according to the concentration of tennecetin to make the pH value of the smart extracting solution of tennecetin progressively be reduced to 8-9, when being 22mg/ml as concentration when tennecetin, the pH value is 8.6), under the situation that the pH value is no longer gone up, restir is (preferred 1 hour) more than 1 hour, makes the nucleation of tennecetin and crystal growth reach balance;
Subordinate phase continues slowly to drip acid while stirring the smart extracting solution of tennecetin, make the pH value of the smart extracting solution of tennecetin progressively be reduced to 6-7, under the situation that the pH value is no longer gone up, restir is (preferred 3-5 hour) more than 3 hours, obtains flaky tennecetin crystalline crystal solution.
The acid that the acidifying regulate process of this step is used is industrial acid commonly used, example hydrochloric acid, sulfuric acid etc.Stir in this step and be conventional at the uniform velocity stirring means, as magnetic agitation, mechanical stirring etc., the purpose that stirs is crystal solution is mixed on the one hand, avoid the low excessively tennecetin outburst nucleation that causes of local pH, the crystal of tennecetin fully is suspended in the crystal solution, avoids crystal bonding parcel impurity.
F, the tennecetin crystalline crystal solution that step e is obtained are carried out liquid-solid separation, and vacuum-drying obtains sheet tennecetin crystal then.
The solid-liquid separating method that any conventional is selected in the liquid-solid separation of the crystal solution described in this step for use all can, as suction filtration, centrifuging etc.The tennecetin crystal that this step obtains through liquid-solid separation, available 50% alcohol-water (V: V) solution washing is 3 times, in 50 ℃ ,-the 0.09MPa condition under vacuum-drying to constant weight, can obtain white little yellowish sheet tennecetin crystal, purity about 90%.
Two, specific embodiment
Embodiment 1
Get the dry mycelium 100g of tennecetin, wherein tennecetin content is 11.2% (w/w), adds the mixed solution (volume ratio of methyl alcohol and water is 75: 25) of 1L methyl alcohol and water, stirs mycelium is fully suspended.NaOH with 10mol/L regulates pH value to 11.35 back stirring 1 hour.Suction filtration isolate slag is collected filtrate, obtains the tennecetin extracting solution of yellowish brown.The extracting solution that concentrates tennecetin to the content of tennecetin is 22.6mg/ml, and flocculation removes the insolubles of separating out in this process, obtains the smart extracting solution of tennecetin.While stirring the HCl that slowly drips 10mol/L, make the pH value of the smart extracting solution of tennecetin progressively be reduced to 8.65 subsequently, under the situation that the pH value is no longer gone up, restir 1 hour.Then continue to make the pH value of the smart extracting solution of tennecetin progressively be reduced to 6.61 while stirring the slowly HCl of dropping 10mol/L, under the situation that the pH value is no longer gone up, restir 4 hours.Suction filtration crystal solution afterwards, obtain sheet tennecetin crystal, behind 50% ethanol-water solution washing crystal 3 times, in 50 ℃ ,-the 0.09MPa condition under vacuum-drying to constant weight, promptly obtain the little yellowish sheet tennecetin crystal 7.11g of white, purity 92.1%.Crystal is coated on the wave carrier piece, gets crystal morphology as shown in Figure 1 with Olympus VANOX-S type microscope 100 times of following photomicrographys, the brilliant habit is sheet, and thicker, big or small homogeneous does not wrap up impurity.
Embodiment 2
Get the dry mycelium 90g of tennecetin, wherein tennecetin content is
12.1%(w/w), add the mixed solution (volume ratio of methyl alcohol and water is 60: 40) of 1L methyl alcohol and water, stirring fully suspends mycelium.NaOH with 10mol/L regulates pH value to 10 back stirring 1.5 hours.Suction filtration isolate slag is collected filtrate, obtains the tennecetin extracting solution of yellowish brown.The extracting solution that concentrates tennecetin to the content of tennecetin is 18mg/ml, and flocculation removes the insolubles of separating out in this process, obtains the smart extracting solution of tennecetin.While stirring the HCl that slowly drips 10mol/L, make the pH value of the smart extracting solution of tennecetin progressively be reduced to 8 subsequently, under the situation that the pH value is no longer gone up, restir 1.5 hours.Then continue to make the pH value of the smart extracting solution of tennecetin progressively be reduced to 6 while stirring the slowly HCl of dropping 10mol/L, under the situation that the pH value is no longer gone up, restir 3 hours.The suction filtration crystal solution obtains sheet tennecetin crystal afterwards, behind 50% ethanol-water solution washing crystal 3 times, in 50 ℃ ,-the 0.09MPa condition under vacuum-drying to constant weight, promptly obtain white little yellowish sheet tennecetin crystal
6.96G, purity
91.5%.Tabular crystal shape under the microscopic examination is with embodiment 1.
Embodiment 3
Get the dry mycelium 110g of tennecetin, wherein tennecetin content is
10.3%(w/w), add the mixed solution (volume ratio of methyl alcohol and water is 90: 10) of 1L methyl alcohol and water, stirring fully suspends mycelium.NaOH with 10mol/L regulates pH value to 12 back stirring 1 hour.Suction filtration isolate slag is collected filtrate, obtains the tennecetin extracting solution of yellowish brown.The extracting solution that concentrates tennecetin to the content of tennecetin is 26mg/ml, and flocculation removes the insolubles of separating out in this process, obtains the smart extracting solution of tennecetin.While stirring the HCl that slowly drips 10mol/L, make the pH value of the smart extracting solution of tennecetin progressively be reduced to 9 subsequently, under the situation that the pH value is no longer gone up, restir 2 hours.Then continue to make the pH value of the smart extracting solution of tennecetin progressively be reduced to 7 while stirring the slowly HCl of dropping 10mol/L, under the situation that the pH value is no longer gone up, restir 5 hours.The suction filtration crystal solution obtains sheet tennecetin crystal afterwards, behind 50% ethanol-water solution washing crystal 3 times, in 50 ℃ ,-the 0.09MPa condition under vacuum-drying to constant weight, promptly obtain white little yellowish sheet tennecetin crystal
7.27G, purity
90.3%.Tabular crystal shape under the microscopic examination is with embodiment 1.
Embodiment 4 (control group)
As the method for embodiment 1, only the acidifying step changes into stage by stage: the HCl that directly drips 10mol/L in the smart extracting solution of tennecetin regulates pH value to 6.5.Suction filtration, washing crystal final vacuum are dried to constant weight afterwards, obtain coalescent and are surrounded by the tennecetin tabular crystal 7.51g of impurity, purity 85.5%.Method by microphotograph among the embodiment 1 obtains crystal morphology as shown in Figure 2,
CrystalThe size heterogeneity, coalescent and parcel impurity, pattern is poor than embodiment 1.
Comparative illustration by embodiment 1-3 and embodiment 4: in the crystallisation process of tennecetin, adopt the growing the grain technology of the smart extracting solution of acidifying tennecetin stage by stage can improve the size distribution of tabular crystal, improve tennecetin crystalline purity.
Contrast experiment's group
As embodiment 1 method, only change the ratio of methyl alcohol and water in the mixing solutions of methyl alcohol and water, the tennecetin in the mycelium is extracted in grouping, and the filtration time (liquid-solid separation) of the tennecetin crystalline crystal solution that makes is as shown in table 1 with time of drying:
Table 1 different ratios mixing solutions filtration time and contrast time of drying
Group 9 crystal that make get crystal morphology as shown in Figure 3 by photomicrography method among the embodiment 1, and brilliant the habit is needle-like.
The result shows that the content of methyl alcohol is practised crystalline substance very big influence, and brilliant tennecetin crystal filtration time of practising of sheet and time of drying are all short than the brilliant tennecetin crystal of practising of needle-like, more help the solid-liquid separation in the tennecetin leaching process.
Claims (4)
1. the preparation method of a tennecetin tabular crystal, it is characterized in that: it may further comprise the steps:
A, get in the mixed solution that the tennecetin mycelium adds methyl alcohol and water; In the mixed solution of described methyl alcohol and water, the volume ratio of methyl alcohol and water is 60-90: 40-10; The mixed solution of every 1L methyl alcohol and water adds 90-110g tennecetin mycelium;
The pH value of b, the solution that obtains with the even stirring and adjusting step of alkaline matter a is to 10-12;
C, the solution that step b is obtained carry out liquid-solid separation, collect the extracting solution that filtrate obtains tennecetin;
The extracting solution of the tennecetin that d, enrichment step c obtain to tennecetin content between 18～26mg/ml, and flocculation removes the insolubles of separating out in this process, obtain the smart extracting solution of tennecetin;
The smart extracting solution of the tennecetin of e, acidification step d acquisition in two stages:
Fs slowly drips acid while stirring the smart extracting solution of tennecetin, makes the pH value of the smart extracting solution of tennecetin progressively be reduced to 8-9, and under the situation that the pH value is no longer gone up, restir is more than 1 hour;
Subordinate phase continues slowly to drip acid while stirring the smart extracting solution of tennecetin, make the pH value of the smart extracting solution of tennecetin progressively be reduced to 6-7, under the situation that the pH value is no longer gone up, restir obtained flaky tennecetin crystalline crystal solution more than 3 hours;
F, the tennecetin crystalline crystal solution that step e is obtained are carried out liquid-solid separation, and vacuum-drying obtains sheet tennecetin crystal then.
2. the preparation method of tennecetin tabular crystal according to claim 1 is characterized in that: the described tennecetin mycelium of step a is the dry mycelium of moisture content≤5%.
3. the preparation method of tennecetin tabular crystal according to claim 1 is characterized in that: the volume ratio of described methyl alcohol of step a and water is 73: 27, and the mixed solution of every 1L methyl alcohol and water adds 100g tennecetin mycelium.
4. the preparation method of tennecetin tabular crystal according to claim 1 is characterized in that: among the step e, and the fs, under the situation that the pH value is no longer gone up, restir 1 hour; Subordinate phase, under the situation that the pH value is no longer gone up, restir 3-5 hour.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104876989A (en) * | 2015-05-14 | 2015-09-02 | 浙江新银象生物工程有限公司 | Preparation method of natamycin acicular crystal |
| CN108659075A (en) * | 2018-06-19 | 2018-10-16 | 苏州汉德瑞生物工程有限公司 | A kind of preparation method of novel polymolecularity Natamycin |
| CN110790801A (en) * | 2019-11-19 | 2020-02-14 | 浙江新银象生物工程有限公司 | Preparation method of high-purity white natamycin |
| CN112585150A (en) * | 2018-08-16 | 2021-03-30 | 帝斯曼知识产权资产管理有限公司 | Novel epolyonic amphomacrolides and process for purifying natamycin |
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| US3892850A (en) * | 1956-03-13 | 1975-07-01 | Gist Brocades Nv | Pimaricin and process of producing same |
| US5942611A (en) * | 1995-01-19 | 1999-08-24 | Cultor Ltd. | Process for natamycin recovery |
| CN1515678A (en) * | 2003-08-25 | 2004-07-28 | 天津科技大学 | Preparation method of natamycin |
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2011
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| US3892850A (en) * | 1956-03-13 | 1975-07-01 | Gist Brocades Nv | Pimaricin and process of producing same |
| US5942611A (en) * | 1995-01-19 | 1999-08-24 | Cultor Ltd. | Process for natamycin recovery |
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| 殷昊等: "纳他霉素分离技术的研究进展", 《食品工业科技》, vol. 28, no. 07, 25 July 2007 (2007-07-25), pages 244 - 246 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104876989A (en) * | 2015-05-14 | 2015-09-02 | 浙江新银象生物工程有限公司 | Preparation method of natamycin acicular crystal |
| CN104876989B (en) * | 2015-05-14 | 2017-10-20 | 浙江新银象生物工程有限公司 | A kind of preparation method of natamycin acicular crystal |
| CN108659075A (en) * | 2018-06-19 | 2018-10-16 | 苏州汉德瑞生物工程有限公司 | A kind of preparation method of novel polymolecularity Natamycin |
| CN112585150A (en) * | 2018-08-16 | 2021-03-30 | 帝斯曼知识产权资产管理有限公司 | Novel epolyonic amphomacrolides and process for purifying natamycin |
| CN112585150B (en) * | 2018-08-16 | 2024-03-29 | 帝斯曼知识产权资产管理有限公司 | New epoxypolyene ampholytic macrolides and process for purifying natamycin |
| CN110790801A (en) * | 2019-11-19 | 2020-02-14 | 浙江新银象生物工程有限公司 | Preparation method of high-purity white natamycin |
| CN110790801B (en) * | 2019-11-19 | 2021-05-04 | 浙江新银象生物工程有限公司 | Preparation method of high-purity white natamycin |
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