CN105001234B - A kind of method for extraction and purification of biotin - Google Patents

A kind of method for extraction and purification of biotin Download PDF

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Publication number
CN105001234B
CN105001234B CN201510458041.XA CN201510458041A CN105001234B CN 105001234 B CN105001234 B CN 105001234B CN 201510458041 A CN201510458041 A CN 201510458041A CN 105001234 B CN105001234 B CN 105001234B
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biotin
filtrate
nanofiltration
extraction
purification
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CN105001234A (en
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王�义
周丽娜
王文超
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Ningxia Tairui Pharmaceutical Co Ltd
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Ningxia Tairui Pharmaceutical Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D495/00—Heterocyclic compounds containing in the condensed system at least one hetero ring having sulfur atoms as the only ring hetero atoms
    • C07D495/02—Heterocyclic compounds containing in the condensed system at least one hetero ring having sulfur atoms as the only ring hetero atoms in which the condensed system contains two hetero rings
    • C07D495/04—Ortho-condensed systems
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

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  • Organic Chemistry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The present invention relates to a kind of method that utilization biotin zymotic fluid prepares biotin, the method be by biotin zymotic fluid by pretreatment, ceramic membrane filter, ultrafiltration, nanofiltration, crystallize and be dried to obtain biotin.The achievable bulk drug biotin stabilization of the present invention, efficient production.The method is utilized simultaneously, biotin yield can be improved, with energy-conservation, to reduce environmental pollution, easy to operate, operating efficiency high etc. excellent.

Description

A kind of method for extraction and purification of biotin
Technical field
The invention belongs to vitamin extraction, synthesis technical field, more particularly to a kind of extraction purification side of biotin Method.
Background technology
Biotin is a kind of water-soluble B vitamin containing element sulphur, is sent out as the yeast growth factor before more than 100 years It is existing, then found in yolk and liver again.Biotin participates in carboxylation, decarboxylation and turns as the co-factor of enzyme in vivo Carboxylic reacts, and plays the carrier effect that carboxyl is transferred to acceptor from donor.The biological action of biotin is since discovery As foods and cosmetics additive, it is widely used in the multiple fields such as animal husbandry, medicine, biomedical detection, fermentation industry, World market is higher per annual requirement, has exceeded 200 tons.
At present, it is domestic using synthetic method and fermentation method production biotin, but using the extraction of fermentation method production biotin, Purifying process is without related document report.
The content of the invention
The purpose of the present invention is that offer one kind effectively improves extract yield, and reduces cost reduces environmental pollution, realizes The method for extraction and purification of stabilization, the efficiently biotin of production.
The technical scheme taken to achieve the above object is：
A kind of method for extraction and purification of biotin, it is characterised in that comprise the technical steps that：
1) pre-process：Biotin zymotic fluid is adjusted into pH to 7.1~7.5 first, 20~40min is stood, then heated to 60~80 DEG C, 40~60min is stood again, after be down to room temperature, add adsorbent, be sufficiently stirred for, continue to stand 80~100min, Stainless steel metal net filtration is used, biotin filtrate is obtained；
2) by process 1) obtained by the dilution of biotin filtrate, ceramic membrane filter, super is carried out after being warming up to 35~40 DEG C successively Filter and nanofiltration treatment, gained nanofiltration filtrate are warming up to 60~80 DEG C, then crystallisation by cooling, separation of solid and liquid, dry and sieve.
The process 1) in, regulation pH uses mass concentration for 10~30% sodium carbonate liquors.
The process 1) in, the stainless steel wire mesh deionized water rinsing after filtering is equal to hair to flushing liquor volume Stop rinsing during zymotic fluid volume, the flushing liquor mixes with biotin filtrate；The filtering accuracy of the stainless steel wire mesh is 300 ~500 μm.
The process 1) in, adsorbent is heavy metal absorbent, its addition for biotin zymotic fluid quality 0.01~ 0.05%.Heavy metal absorbent can select heavy metal absorbent H2061.
The process 2) in, dilution refer to biotin filtrate add deionized water, its dosage for filtrate volume 20~ 40%.
The process 2) in, during ceramic membrane filter, in 0.3~0.4MPa, ceramic membrane is that bundled tube is more to Stress control Hole ceramics membrane material is aluminum oxide, and molecular cut off is 5KD.
The process 2) in, ultrafiltrate temperature is controlled at 30~35 DEG C, and Stress control is in 0.2~0.3MPa；During ultrafiltration is used Fibre ultrafiltration film, material is PVDF, and membrane aperture is 0.01 μm.
The process 2) in, in nanofiltration before processing, ultrafiltrate is first down to room temperature, add deionized water dilution dimension life Plain H, makes its chemical titer be down to 500~1000 μ/ml, then carries out nanofiltration.
The process 2) in, nanofiltration is using Tao Shi NF membrane NF90-400/34i desalination type NF membranes, nanofiltration pressure control System in 2~2.5MPa, nanofiltration 300~400L/h of flow velocity, the concentration volume multiple of nanofiltration is 3~5 times, and nanofiltration terminates, using going 8~10min is washed on ionized water top.
The process 2) in, crystallisation by cooling process is：Rate of temperature fall according to 10~12 DEG C/h is cooled down, period, even Continuous constant current at a slow speed imports the anti-solvent deionized water of the 5~10% of nanofiltration filtrate volume, when there is crystalline polamer, rapidly joins The crystal seed biotin of the 0.1~0.5% of nanofiltration filtrate total hundred million, cooling and deionized water are stopped when being down to -10~-5 DEG C to temperature Dose, continue stir 20~40min, then stand 2~4h.
The process 2) in, drying is that, using the mixed powder machine of bipyramid, to 120~130 DEG C, temperature of outgoing air is extremely for regulation EAT 50~80 DEG C.
The process 2) in, in ultra-filtration process, water-dialyzing being added, the water-dialyzing is the filtrate of ceramic membrane filter, when first When the filtrate volume of ceramic membrane filter reaches the 30% of fermentating liquid volume, 3 times are diluted as water-dialyzing, be continuously added to 2 times.
The process 2) in, chemical titer (the u/ml) × volume of crystal seed biotin consumption (g)=biotin filtrate (m3) × proportionality coefficient (%).
Technique effect of the invention is：
1) present invention establishes a kind of method that utilization biotin zymotic fluid prepares biotin.
2) total recovery is more than 85%.
3) final product quality meets relevant regulations.
Specific embodiment
The present invention is explained with example, it should be understood that example is for illustrating rather than to this below The limitation of invention.The scope of the present invention is determined with core content according to claims.
Biotin zymotic fluid is to use brevibacterium ammoniagene in following embodiments, and biotin is obtained by second order fermentation pattern Zymotic fluid, the carbon source in the fermentation medium is mainly grape sugar and starch, and nitrogen source is mainly beancake powder, peptone and yeast Powder.
Material source：Heavy metal absorbent H2061 is provided by Shanghai Hui Jian Industrial Co., Ltd.s.
Embodiment 1
Biotin zymotic fluid 10m3, potency is 2540u/ml.
1) pre-process：Speed of agitator is controlled in 30r/min；Zymotic fluid pH is adjusted to 7.1 with 10% sodium carbonate liquor first, Stand 20min；Secondly biotin zymotic fluid is warming up to 60 DEG C, then stands 40min；Last zymotic fluid is down to room temperature, adds The adsorbent H2061 of 1kg, speed of agitator is controlled in 100r/min；Stirring 1min, stands 80min, uses stainless steel wire mesh mistake Filter, filtering accuracy is 300 μm, obtains biotin filtrate 8.2m3；Use deionized water rinsing stainless steel wire mesh, flushing liquor and dimension Raw element H filtrates mixing, the volume of filtrate is 10m3, potency is 2497u/ml, and the yield of pretreatment is 98.3%.
2) dilute：Biotin filtrate is added into deionized water 2m3, the volume of filtrate is 12m3。
3) ceramic membrane filter：By process 2) the biotin solution that obtains is warming up to 35 DEG C, using bundled tube porous ceramic film Filtering.In filter process, Stress control is in 0.3~0.4MPa.Ceramic membrane filter terminates, and the volume of filtrate is 11.8m3。
4) ultrafiltration：By process 3) the biotin solution that obtains controlled at 30 DEG C, carries out ultrafiltration, Stress control 0.2~ 0.3MPa, ultrafiltration terminates, and the volume of filtrate is 11.6m3。
5) nanofiltration：By process 4) the filtrate temperature that obtains is down to room temperature, adds deionized water dilution biotin, makes it Chemical titer is down to 500u/ml, then carries out nanofiltration, and nanofiltration terminates, and the volume of filtrate is 19.3m3。
6) crystallisation by cooling：Speed of agitator is controlled in 30r/min；By process 5) gained filtrate be warming up to 60 DEG C, then start Cooling, the speed control of cooling stops cooling in 10~12 DEG C/h when being cooled to -10 DEG C；In temperature-fall period, continuously constant current at a slow speed Anti-solvent deionized water is imported, dosage is 1m3, temperature is down to -10 DEG C, stops adding deionized water.In temperature-fall period, there is knot During brilliant phenomenon, crystal seed biotin 24.9g is rapidly joined.Temperature is down to -10 DEG C, continues to stir 20min, then stands 2h.
7) dry
Filtrate is dried through separation of solid and liquid, gained solid biotin.Enable the mixed powder machine of bipyramid, regulation EAT to 120~130 DEG C, temperature of outgoing air to 50~80 DEG C, humidification powder in charge door, through 8~12 mesh stainless steel mesh after, with air-flow to revolve Wind separator, reaches sieving machine and obtains biotin 21.53kg through sieving.
Total recovery is 85.3%.
Embodiment 2
Biotin zymotic fluid 10m3, potency is 2365u/ml.
1) pre-process：Speed of agitator is controlled in 35r/min；Zymotic fluid pH is adjusted to 7.2 with 15% sodium carbonate liquor first, Stand 25min；Secondly biotin zymotic fluid is warming up to 65 DEG C, then stands 45min；Last zymotic fluid is down to room temperature, adds The adsorbent H2061 of 2kg, speed of agitator is controlled in 105r/min；Stirring 2min, stands 85min, uses stainless steel wire mesh mistake Filter, filtering accuracy is 350 μm, obtains biotin filtrate 8.3m3；Use deionized water rinsing stainless steel wire mesh, flushing liquor and dimension Raw element H filtrates mixing, the volume of filtrate is 10m3, potency is 2327u/ml, and the yield of pretreatment is 98.4%.
2) dilute：Biotin filtrate is added into deionized water 2.5m3, the volume of filtrate is 12.5m3。
3) ceramic membrane filter：By process 2) the biotin solution that obtains is warming up to 36 DEG C, using bundled tube porous ceramic film Filtering.In filter process, Stress control is in 0.3~0.4MPa.Ceramic membrane filter terminates, and the volume of filtrate is 12.3m3。
4) ultrafiltration：By process 3) the biotin solution that obtains controlled at 31 DEG C, carries out ultrafiltration, Stress control 0.2~ 0.3MPa, ultrafiltration terminates, and the volume of filtrate is 12.1m3。
5) nanofiltration：By process 4) the filtrate temperature that obtains is down to room temperature, adds deionized water dilution biotin, makes it Chemical titer is down to 600u/ml, then carries out nanofiltration, and nanofiltration terminates, and the volume of filtrate is 13.4m3。
6) crystallisation by cooling：Speed of agitator is controlled in 35r/min；By process 5) gained filtrate be warming up to 65 DEG C, then start Cooling, the speed control of cooling stops cooling in 10~12 DEG C/h when being cooled to -9 DEG C；In temperature-fall period, continuously constant current at a slow speed Anti-solvent deionized water is imported, dosage is 0.8m3, temperature is down to -9 DEG C, stops adding deionized water.In temperature-fall period, occur During crystalline polamer, crystal seed biotin 46.54g is rapidly joined.Temperature is down to -9 DEG C, continues to stir 25min, then stands 2.5h.
7) dry
Filtrate is dried through separation of solid and liquid, gained solid biotin.Enable the mixed powder machine of bipyramid, regulation EAT to 120~130 DEG C, temperature of outgoing air to 50~80 DEG C, humidification powder in charge door, through 8~12 mesh stainless steel mesh after, with air-flow to revolve Wind separator, reaches sieving machine and obtains PABA 9.87kg through sieving.
Total recovery is 85.6%.
Embodiment 3
Biotin zymotic fluid 10m3, potency is 2410u/ml.
1) pre-process：Speed of agitator is controlled in 40r/min；Zymotic fluid pH is adjusted to 7.3 with 20% sodium carbonate liquor first, Stand 30min；Secondly biotin zymotic fluid is warming up to 70 DEG C, then stands 50min；Last zymotic fluid is down to room temperature, adds The adsorbent H2061 of 3kg, speed of agitator is controlled in 110r/min；Stirring 3min, stands 90min, uses stainless steel wire mesh mistake Filter, filtering accuracy is 400 μm, obtains biotin filtrate 8.1m3；Use deionized water rinsing stainless steel wire mesh, flushing liquor and dimension Raw element H filtrates mixing, the volume of filtrate is 10m3, potency is 2379u/ml, and the yield of pretreatment is 98.7%.
2) dilute：Biotin filtrate is added into deionized water 3m3, the volume of filtrate is 13m3。
3) ceramic membrane filter：By process 2) the biotin solution that obtains is warming up to 37 DEG C, using bundled tube porous ceramic film Filtering.In filter process, Stress control is in 0.3~0.4MPa.Ceramic membrane filter terminates, and the volume of filtrate is 12.9m3。
4) ultrafiltration：By process 3) the biotin solution that obtains controlled at 32 DEG C, carries out ultrafiltration, Stress control 0.2~ 0.3MPa, ultrafiltration terminates, and the volume of filtrate is 12.7m3。
5) nanofiltration：By process 4) the filtrate temperature that obtains is down to room temperature, adds deionized water dilution biotin, makes it Chemical titer is down to 750u/ml, then carries out nanofiltration, and nanofiltration terminates, and the volume of filtrate is 10m3。
6) crystallisation by cooling：Speed of agitator is controlled in 40r/min；By process 5) gained filtrate be warming up to 70 DEG C, then start Cooling, the speed control of cooling stops cooling in 10~12 DEG C/h when being cooled to -8 DEG C；In temperature-fall period, continuously constant current at a slow speed Anti-solvent deionized water is imported, dosage is 0.7m3, temperature is down to -8 DEG C, stops adding deionized water.In temperature-fall period, occur During crystalline polamer, crystal seed biotin 71.4g is rapidly joined.Temperature is down to -8 DEG C, continues to stir 30min, then stands 3h.
7) dry：Filtrate is dried through separation of solid and liquid, gained solid biotin.The mixed powder machine of bipyramid is enabled, air intake is adjusted Temperature to 120~130 DEG C, temperature of outgoing air to 50~80 DEG C, humidification powder in charge door, through 8~12 mesh stainless steel mesh after, with gas Cyclone separator is flow to, sieving machine is reached and is obtained biotin 20.43kg through sieving.
Total recovery is 86.2%.
Embodiment 4
Biotin zymotic fluid 10m3, potency is 2150u/ml.
1) pre-process：Speed of agitator is controlled in 45r/min；Zymotic fluid pH is adjusted to 7.4 with 25% sodium carbonate liquor first, Stand 35min；Secondly biotin zymotic fluid is warming up to 75 DEG C, then stands 55min；Last zymotic fluid is down to room temperature, adds The adsorbent H2061 of 4kg, speed of agitator is controlled in 115r/min；Stirring 4min, stands 95min, uses stainless steel wire mesh mistake Filter, filtering accuracy is 450 μm, obtains biotin filtrate 8.2m3；Use deionized water rinsing stainless steel wire mesh, flushing liquor and dimension Raw element H filtrates mixing, the volume of filtrate is 10m3, potency is 2118u/ml, and the yield of pretreatment is 98.5%.
2) dilute：Biotin filtrate is added into deionized water 3.5m3, the volume of filtrate is 13.5m3。
3) ceramic membrane filter：By process 2) the biotin solution that obtains is warming up to 38 DEG C, using bundled tube porous ceramic film Filtering.In filter process, Stress control is in 0.3~0.4MPa.Ceramic membrane filter terminates, and the volume of filtrate is 13.2m3。
4) ultrafiltration：By process 3) the biotin solution that obtains controlled at 33 DEG C, carries out ultrafiltration, Stress control 0.2~ 0.3MPa, ultrafiltration terminates, and the volume of filtrate is 13m3。
5) nanofiltration：By process 4) the filtrate temperature that obtains is down to room temperature, adds deionized water dilution biotin, makes it Chemical titer is down to 900u/ml, then carries out nanofiltration, and nanofiltration terminates, and the volume of filtrate is 6.8m3。
6) crystallisation by cooling：Speed of agitator is controlled in 40r/min；By process 5) gained filtrate be warming up to 75 DEG C, then start Cooling, the speed control of cooling stops cooling in 10~12 DEG C/h when being cooled to -7 DEG C；In temperature-fall period, continuously constant current at a slow speed Anti-solvent deionized water is imported, dosage is 0.54m3, temperature is down to -7 DEG C, stops adding deionized water.In temperature-fall period, occur During crystalline polamer, crystal seed biotin 84.72g is rapidly joined.Temperature is down to -7 DEG C, continues to stir 35min, then stands 3.5h.
7) dry：Filtrate is dried through separation of solid and liquid, gained solid biotin.The mixed powder machine of bipyramid is enabled, air intake is adjusted Temperature to 120~130 DEG C, temperature of outgoing air to 50~80 DEG C, humidification powder in charge door, through 8~12 mesh stainless steel mesh after, with gas Cyclone separator is flow to, sieving machine is reached and is obtained PABA 8.43kg through sieving.
Total recovery is 85.9%.
Embodiment 5
Biotin zymotic fluid 10m3, potency is 2248u/ml.
1) pre-process：Speed of agitator is controlled in 50r/min；Zymotic fluid pH is adjusted to 7.5 with 30% sodium carbonate liquor first, Stand 40min；Secondly biotin zymotic fluid is warming up to 80 DEG C, then stands 60min；Last zymotic fluid is down to room temperature, adds The adsorbent H2061 of 5kg, speed of agitator is controlled in 120r/min；Stirring 5min, stands 100min, uses stainless steel wire mesh mistake Filter, filtering accuracy is 500 μm, obtains biotin filtrate 8.4m3；Use deionized water rinsing stainless steel wire mesh, flushing liquor and dimension Raw element H filtrates mixing, the volume of filtrate is 10m3, potency is 2205u/ml, and the yield of pretreatment is 98.1%.
2) dilute：Biotin filtrate is added into deionized water 4m3, the volume of filtrate is 14m3。
3) ceramic membrane filter：By process 2) the biotin solution that obtains is warming up to 40 DEG C, using bundled tube porous ceramic film Filtering.In filter process, Stress control is in 0.3~0.4MPa.Ceramic membrane filter terminates, and the volume of filtrate is 13.9m3。
4) ultrafiltration：By process 3) the biotin solution that obtains controlled at 35 DEG C, carries out ultrafiltration, Stress control 0.2~ 0.3MPa, ultrafiltration terminates, and the volume of filtrate is 13.7m3。
5) nanofiltration：By process 4) the filtrate temperature that obtains is down to room temperature, adds deionized water dilution biotin, makes it Chemical titer is down to 1000u/ml, then carries out nanofiltration, and nanofiltration terminates, and the volume of filtrate is 6m3。
6) crystallisation by cooling：Speed of agitator is controlled in 40r/min；By process 5) gained filtrate be warming up to 80 DEG C, then start Cooling, the speed control of cooling stops cooling in 10~12 DEG C/h when being cooled to -5 DEG C；In temperature-fall period, continuously constant current at a slow speed Anti-solvent deionized water is imported, dosage is 0.6m3, temperature is down to -5 DEG C, stops adding deionized water.In temperature-fall period, occur During crystalline polamer, crystal seed PABA 10.25g is rapidly joined.Temperature is down to -5 DEG C, continues to stir 40min, then stands 4h.
7) dry：Filtrate is dried through separation of solid and liquid, gained solid biotin.The mixed powder machine of bipyramid is enabled, air intake is adjusted Temperature to 120~130 DEG C, temperature of outgoing air to 50~80 DEG C, humidification powder in charge door, through 8~12 mesh stainless steel mesh after, with gas Cyclone separator is flow to, sieving machine is reached and is obtained PABA 9.14kg through sieving.
Total recovery is 85.5%.

Claims (9)

1. a kind of method for extraction and purification of biotin, it is characterised in that comprise the technical steps that：
1）Pretreatment：Biotin zymotic fluid is adjusted into pH to 7.1~7.5 first, 20~40min is stood, then heat to 60~ 80 DEG C, 40~60min is stood again, after be down to room temperature, add adsorbent, be sufficiently stirred for, continue to stand 80~100min, with not Rust steel metal net filtration, obtains biotin filtrate, and the adsorbent is heavy metal absorbent, and its addition is fermented for biotin The 0.01~0.05% of liquid quality；
2）By process 1）Gained biotin filtrate dilution, carried out successively after being warming up to 35~40 DEG C ceramic membrane filter, ultrafiltration and Nanofiltration is processed, and gained nanofiltration filtrate is warming up to 60~80 DEG C, then crystallisation by cooling, separation of solid and liquid, is dried and is sieved；
During the ceramic membrane filter, in 0.3~0.4MPa, ceramic membrane is bundled tube porous ceramic film, material to Stress control It is aluminum oxide, molecular cut off is 5KD；
Ultrafiltrate temperature control at 30~35 DEG C, Stress control 0.2~0.3MPa；
It is described that ultrafiltrate is first down to room temperature in nanofiltration before processing, deionized water dilution biotin is added, make its chemistry Potency is down to 500~1000 μ/ml, then carries out nanofiltration, and nanofiltration pressure is controlled in 2~2.5MPa, 300~400L/ of nanofiltration flow velocity H, the concentration volume multiple of nanofiltration is 3~5 times, and nanofiltration terminates, and 8~10min is washed using deionized water top；
The crystallisation by cooling process is：Rate of temperature fall according to 10~12 DEG C/h is cooled down, period, and continuously constant current is imported at a slow speed The anti-solvent deionized water of the 5~10% of nanofiltration filtrate volume, when there is crystalline polamer, rapidly joins nanofiltration filtrate total hundred million 0.1~0.5% crystal seed biotin, stops cooling and deionized water is dosed when being down to -10~-5 DEG C to temperature, continues to stir 20~40min, then stands 2~4h.
2. according to the method for extraction and purification of the biotin described in claim 1, it is characterised in that the process 1）In, adjust pH Mass concentration is used for 10~30% sodium carbonate liquors.
3. according to the method for extraction and purification of the biotin described in claim 1, it is characterised in that the process 1）In, after filtering Stainless steel wire mesh deionized water rinsing, when being equal to fermentating liquid volume to flushing liquor volume stop rinse, the flushing liquor Mix with biotin filtrate；The filtering accuracy of the stainless steel wire mesh is 300~500 μm.
4. according to the method for extraction and purification of the biotin described in claim 1, it is characterised in that the process 2）In, dilution is Refer to and add deionized water in biotin filtrate, its dosage is the 20~40% of filtrate volume.
5. according to the method for extraction and purification of the biotin described in claim 1, it is characterised in that the process 2）In, ultrafiltration is adopted With hollow fiber ultrafiltration membrane, material is PVDF, and membrane aperture is 0.01 μm.
6. according to the method for extraction and purification of the biotin described in claim 1, it is characterised in that the process 2）In, nanofiltration is Using Tao Shi NF membrane NF90-400/34i desalination type NF membranes.
7. according to the method for extraction and purification of the biotin described in claim 1, it is characterised in that the process 2）In, drying is Using the mixed powder machine of bipyramid, to 120~130 DEG C, temperature of outgoing air is to 50~80 DEG C for regulation EAT.
8. according to the method for extraction and purification of the biotin described in claim 1, it is characterised in that the process 2）In, ultra filtration Cheng Zhong, adds water-dialyzing, and the water-dialyzing is the filtrate of ceramic membrane filter, when the filtrate volume of ceramic membrane filter first reaches fermentation Liquid product 30% when, diluted 3 times as water-dialyzing, be continuously added to 2 times.
9. according to the method for extraction and purification of the biotin described in claim 1, it is characterised in that the process 2）In, crystal seed dimension Raw element H consumptions（g）The chemical titer of=biotin filtrate（u/ml）× volume（m3）× proportionality coefficient（%）.
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