CN102140052A - Method for extracting lycopene continuously - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 64
- OAIJSZIZWZSQBC-GYZMGTAESA-N lycopene Chemical compound CC(C)=CCC\C(C)=C\C=C\C(\C)=C\C=C\C(\C)=C\C=C\C=C(/C)\C=C\C=C(/C)\C=C\C=C(/C)CCC=C(C)C OAIJSZIZWZSQBC-GYZMGTAESA-N 0.000 title claims abstract description 36
- UPYKUZBSLRQECL-UKMVMLAPSA-N Lycopene Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1C(=C)CCCC1(C)C)C=CC=C(/C)C=CC2C(=C)CCCC2(C)C UPYKUZBSLRQECL-UKMVMLAPSA-N 0.000 title claims abstract description 22
- JEVVKJMRZMXFBT-XWDZUXABSA-N Lycophyll Natural products OC/C(=C/CC/C(=C\C=C\C(=C/C=C/C(=C\C=C\C=C(/C=C/C=C(\C=C\C=C(/CC/C=C(/CO)\C)\C)/C)\C)/C)\C)/C)/C JEVVKJMRZMXFBT-XWDZUXABSA-N 0.000 title claims abstract description 22
- 229960004999 lycopene Drugs 0.000 title claims abstract description 22
- 235000012661 lycopene Nutrition 0.000 title claims abstract description 22
- 239000001751 lycopene Substances 0.000 title claims abstract description 22
- ZCIHMQAPACOQHT-ZGMPDRQDSA-N trans-isorenieratene Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/c1c(C)ccc(C)c1C)C=CC=C(/C)C=Cc2c(C)ccc(C)c2C ZCIHMQAPACOQHT-ZGMPDRQDSA-N 0.000 title claims abstract description 22
- 238000000605 extraction Methods 0.000 claims abstract description 83
- 239000002904 solvent Substances 0.000 claims abstract description 55
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000000284 extract Substances 0.000 claims abstract description 29
- 241000235553 Blakeslea trispora Species 0.000 claims abstract description 14
- 239000012046 mixed solvent Substances 0.000 claims abstract description 12
- 239000007791 liquid phase Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 27
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- 238000000855 fermentation Methods 0.000 claims description 15
- 230000004151 fermentation Effects 0.000 claims description 15
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 15
- 238000004587 chromatography analysis Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 230000013872 defecation Effects 0.000 claims description 6
- 238000000638 solvent extraction Methods 0.000 claims description 6
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Abstract
The invention belongs to the field of biological separation, and discloses a method for extracting lycopene continuously, which comprises the following steps of: adding blakeslea trispora fermented mycelia into ethanol for dehydrating, filtering and separating the mycelia from ethanol treating fluid; drying the wet mycelia under vacuum and crushing to obtain dried mycelia; adding the dried mycelia into mixed solvent to perform solid-liquid phase extraction; adding the mycelia into each extracting unit of a continuous extracting system, circulating continuously by mixed extraction solvent, and extracting for a certain time period, arranging all units according to the gradient of concentration, performing multi-stage countercurrent extraction until the lycopene is extracted completely, and collecting extract liquor; and concentrating the extract liquor under vacuum to obtain lycopene concentrated liquor. In the method, the lycopene is extracted by the mixed solvent, so that the dissolution effect of the solvent on the lycopene is played fully; the operation is continuous and can be performed in dark places; and the method consumes less solvent consumption, has large treatment capacity, short extraction time and low energy consumption, is low in cost and facilities industrial production.
Description
Technical field
The invention belongs to the bioseparation field, relate to a kind of continuous extraction lycopene method.Utilize this method from mucor fungi Blakeslea trispora (Blaleslea trispora) fermentation mycelium, to extract Lyeopene effectively.
Background technology
Lyeopene is a kind of fat-soluble natural pigment, belongs to carotenoid.Lyeopene has the performance more more superior than other carotenoid, the strongest in carotenoid as its oxidation-resistance, quencher singlet oxygen ability is 100 times of VE, is more than 2 times of β-Hu Luobusu, and the ability of removing free radical also is better than other carotenoid.It has extremely strong antioxygenation, but anticancer growth, the oxidation that slows down low-density lipoprotein (LDL) prevents and treats arteriosclerosis, protect cardiovascular, the toxic substance in removing cigarette and the automobile exhaust gas etc.
Production methods of lycopene mainly contains natural extract, chemosynthesis, microbial fermentation etc., and the Production by Microorganism Fermentation Lyeopene have cost low, pollute advantages such as little, safety and technology are simple, become one of research focus in recent years.At present, many researchists begin one's study and utilize the microorganisms producing Lyeopene, and wherein studying maximum is to utilize blakeslea trispora (Blakeslea trispora) fungi fermentation to obtain lycopene method (CN 1353765A; CN 1370241A; US 2005/0106657A1; US 3369974; GB 1008469).The extracting method overwhelming majority of report is an organic solvent extraction at present, and solvent consumption is big, and Lyeopene is subjected to illumination, air etc. in the leaching process influences very easily oxidation, and the Lyeopene loss is bigger.Patent CN1760282A reports supercritical CO
2The extraction Lyeopene, the extraction yield height, no solvent residue, extraction time is short, but because of apparatus expensive, and cost is high and can't realize suitability for industrialized production.
Summary of the invention
The objective of the invention is to be to overcome the deficiencies in the prior art, and a kind of suitability for industrialized production Lyeopene that is suitable for is provided, and production cost is low, easy and safe to operate, extraction yield is high utilizes Blakeslea trispora suitability for industrialized production lycopene method.
Purpose of the present invention can reach by following technical measures:
A kind of mixed solvent that utilizes extracts lycopene method continuously, it is characterized in that comprising following steps:
A. the Blakeslea trispora fermentation mycelium adds dewatering of ethanol processing, filtering separation mycelium and Ethanol Treatment liquid; Wet mycelium by vacuum-drying and pulverizing, is obtained dry mycelium;
B. the mycelium of handling through step a, add mixed solvent and carry out solid phase-liquid-phase extraction: in each extraction unit of system for continuously extracting, add the mycelium of handling through step a, adopt the mixed extraction solvent to circulate continuously to extract certain hour each unit is arranged by concentration gradient, stage countercurrent extraction to Lyeopene extracts totally again, collects extraction liquid;
C. extraction liquid obtains lycopene concentrated liquor through vacuum concentration in the step (b).
Described method, wherein among the step a alcohol concn between 50%-100%, the volume mass of ethanol and Blakeslea trispora fermentation mycelium than (L/Kg) 1: 1-10: 1, normal temperature was handled 5-180 minute down.
Described method, wherein Ethanol Treatment liquid is handled through low-pressure distillation and be can be recycled.
Described method, wherein the vacuum-drying temperature is at 30 ℃-80 ℃ among the step a, and the vacuum-drying time is at 1-24 hour, preferred 4-12 hour.
Described method, wherein used mixed extraction solvent is primary solvent with the normal hexane solid phase among the step b-liquid-phase extraction stage, with acetone, ethyl acetate or sherwood oil is secondary solvent, the volume ratio of primary solvent and secondary solvent is 1: 1-10: 1, preferred n-hexane/acetone mixed solvent, the volume ratio of normal hexane and acetone is 1: 1-5: 1, preferred 2: 1-5: 1.
Described method, wherein system for continuously extracting is made up of 6-16 root chromatography column, container for storing liquid, recycle pump, valve and pipeline among the step b; Each extraction unit is in series by 2-5 root chromatography column, comprises supporting container for storing liquid, recycle pump, valve and pipeline; System for continuously extracting can the lucifuge operation.
Described method, wherein each unit is arranged by following operation realization by concentration gradient among the step b: unit 1-5 adds the mycelium that equivalent is handled through step a respectively, unit 5 adds fresh mix and extracts solvent extraction t (extraction time in stage) back discharge extracting solution, and unit 2-4 carries out t respectively
1/4, t
2/4, t
3/4The extraction of (being for 1/4,2/4,3/4 extraction time in stage), the solvent of unit 2 and 4 is exchanged, 5 add fresh mix and extract solvents in the unit at last, the concentration gradient shown in when each unit is extracted at the beginning according to Fig. 2 process is arranged, and has promptly made concentration gradient.
Described method, wherein each process of system for continuously extracting is all extracted t
1/4The back is carried out the deslagging charging to Lyeopene by the unit 5 of defecation, and the opposite direction that unsaturated solvent is successively decreased by lycopene concentration migrates to every a unit; Through six operating process, all unit are got back to the initial concentration state again, realize operate continuously, as shown in Figure 2.
Described method, wherein the mode of extracting continuously is a countercurrent extraction; Extract temperature and be 20-60 ℃, preferred 30-50 ℃; Extract solvent load and be the 5-40mL/g mycelium, preferred 5-20mL/g mycelium; Return velocity is 0.6-3.6BV/h (BV is a bed volume), preferred 0.6-1.8BV/h; The backflow number of times is preferred 2-3 time 3-6 time; Extraction time is 2-8h, is preferable over 2-4h; Extraction unit group number is the 3-6 group, preferred 5-6 group.
Described method wherein adds the mycelium that equivalent is handled through step a in each extraction unit.
Further, specific operation process is as follows:
(1) after Blakeslea trispora fermentation broth is handled after filtration, obtains wet mycelium.
(2) wet mycelium in the step (1) is carried out pre-treatment, its pretreatment condition is preferably:
A). wet mycelium and ethanol stir at normal temperatures, filter obtain dewatering mycelium and Ethanol Treatment liquid, and wet mycelium and ethanol mass volume ratio are 1: 1-1: between 10, be preferable over 1: 1-1: between 5;
B). Ethanol Treatment liquid is handled through low-pressure distillation and be can be recycled; The dehydration wet mycelium obtains dry mycelium by vacuum-drying and pulverizing.
(3) through the dry mycelium of step (2), add mixed solvent and carry out solid phase-liquid-phase extraction, in each extraction unit of system for continuously extracting, add the mycelium that equivalent is handled through step (2), adopt the mixed extraction solvent to circulate continuously to extract certain hour each unit is arranged by concentration gradient, stage countercurrent extraction to Lyeopene extracts totally again, collects extraction liquid.Its extraction conditions is preferable over:
A). each unit concentration gradient array realizes by following operation: unit 5 adds discharges extracting solution after fresh mix is extracted solvent extraction t (extraction time in stage), and unit 2-4 carries out t respectively
1/4, t
2/4, t
3/4The solvent of unit 2 and 4 is exchanged in the extraction of extraction time in stage, 5 adds fresh mix and extracts solvents in the unit at last, and the concentration gradient shown in when each unit is extracted at the beginning according to Fig. 2 process is arranged, and has promptly made concentration gradient;
B). leaching process is realized by following operation continuously: each process is all extracted t
1/4The back is carried out the deslagging charging to Lyeopene by the unit 5 of defecation, and the opposite direction that unsaturated solvent is successively decreased by lycopene concentration migrates to every a unit; Through six operating process, all unit are got back to the initial concentration state again, realize operate continuously, as shown in Figure 2;
C). the mixed extraction solvent is primary solvent with the normal hexane, and acetone is secondary solvent, and its volume ratio is 1: 1-10: between 1, be preferable over 2: 1-5: between 1;
D). the mode of extracting is a countercurrent extraction continuously;
E). extract temperature and be between 20-60 ℃, be preferable between 30-50 ℃;
F). extract solvent load and be between the 5-40mL/g mycelium, be preferable between the 5-20mL/g mycelium;
G). return velocity is between the flow velocity of 0.6-3.6BV/h, is preferable between the 0.6-1.8BV/h;
H). the backflow number of times is between 2-6 time, is preferable between 2-3 time;
I). extraction unit group number is the 3-6 group, is preferable between the 5-6 group;
J). extraction time is 2-8h, is preferable between the 2-4h.
(4) with extraction liquid in the step (3) through vacuum concentration, obtain lycopene concentrated liquor.
System for continuously extracting mainly comprises chromatography column, container for storing liquid, recycle pump, control valve, pipeline.
Chromatography column in the system for continuously extracting is meant and can loads the column shape container that mycelium extracts.
The invention has the advantages that:
1, the present invention adopts mixed solvent to extract Lyeopene, gives full play to the solvency action of each solvent to Lyeopene.
2, technical superiority of the present invention is operating continuity, but and the lucifuge operation, reduced periodical operation to the unsettled influence of Lyeopene.
3, the present invention and conventional solvent extraction method ratio, solvent consumption is few, and treatment capacity is big, and extraction time is short, and energy consumption is low, and cost is relatively low, easily suitability for industrialized production.
Description of drawings
Fig. 1 is the system for continuously extracting device sketch among the embodiment, and this system is made up of 5 extraction units, and each extraction unit comprises chromatography column, container for storing liquid, recycle pump, control valve, pipeline.Among the figure: 1 pipeline, 2 chromatography columns, 3 container for storing liquids, 4 control valves, 5 recycle pumps, 6 total pipelines (connecting each unit).
Fig. 2 is continuous extraction process schematic flow sheet.
Embodiment
The invention will be further elaborated by the following examples.
Blakeslea trispora fermentation mycelium of the present invention adopts following method to prepare:
The present invention adopts Blakeslea trispora (Blaleslea trispora) (+) (-) to be fermented bacterium, obtains Blakeslea trispora fermentation broth through shaking a bottle first order seed cultivation, secondary seed fermentation culture and the cultivation of fermentor tank three grade fermemtation; Adopt the filter press method to remove too much moisture in the fermented liquid after fermentation is finished, wet mycelium is through 95% ethanol stir process 2h, and through the dry pre-treatment mycelium that gets of filter press, the alcohol treatment solution is recycled through rectifying tower again.
The leaching process that the present invention adopts:
In conjunction with Fig. 1 and Fig. 2, extract " process one " to " process five " each extraction unit solvent migratory route, charging and operation rules such as deslagging, adding fresh solvent and extracting solution derivation (being to set up through after a plurality of processes), " process six " and four later leaching process are " process one " repetition to " process five ".
Concrete operations comprise:
A. make gradient: mycelium after the pre-treatment of being packed in unit 1 and 5 respectively earlier, unit 5 add discharges extracting solution after fresh mix is extracted a solvent extraction extraction time in stage t, and unit 2-4 carries out t respectively
1/4, t
2/4, t
3/4The solvent of unit 2 and 4 is exchanged in the extraction of extraction time in stage, 5 adds fresh mix and extracts solvents in the unit at last, and the concentration gradient shown in when each unit is extracted at the beginning according to Fig. 2 process is arranged, and promptly makes good concentration gradient shown in Figure 2;
B. deslagging charging: each process is all extracted t again
1/4The back is carried out deslagging to Lyeopene by the unit 5 of defecation, charging;
C. saturated solvent migration: the saturated solvent of unit 1 is transferred in the container for storing liquid, and this process only relates to the saturated unit of solvent (promptly by the next unit of defecation unit 5);
D. unsaturated solvent migration: 1. 3 → 1; 2. 5 → 3; 3. 2 → 5; 4. 4 → 2, this process relates to 4 unit, and it moves follow regularity: promptly the opposite direction of successively decreasing by lycopene concentration migrates to every a unit;
E. fill solvent: fresh mix is inserted in unit 4 extract solvent;
F. through six operating process, all unit are got back to the initial concentration state again, realize operate continuously.
Embodiment 1
The former bacterial strain list bacterium colony of Blakeslea trispora (Blaleslea trispora) is inoculated into 500mL shakes and carry out shake-flask seed in the bottle and cultivate from the inclined-plane, liquid amount 10%, 30 ℃ of culture temperature, rotating speed 200r/min cultivates 30h.The one-level shake-flask seed liquid is seeded to 2.5L shakes and carry out secondary seed in the bottle and cultivate, culture temperature maintains 30 ℃, and rotating speed 200r/min cultivates 30h.Seed culture finishes it is inoculated into and carries out fermentation culture in the 50L fermentor tank, coefficient 60%, and charge amount 30L, culture temperature maintains 30 ℃, rotating speed 200r/min, air flow 0.2-0.5L/min cultivates 120h.
After finishing, fermentation gets the 28L fermented liquid, adopt centrifuging to remove too much moisture in the fermented liquid, obtain the 3kg wet mycelium, add 3L 95% ethanol then and mix stirring 2h, obtain the 0.8kg mycelium through filter press again, wet mycelium is by vacuum-drying (vacuum-drying temperature between 30 ℃-80 ℃, preferred 4-12 of vacuum-drying time hour) and pulverize, obtain pretreated dry mycelium, Ethanol Treatment liquid is handled through low-pressure distillation and be can be recycled; (volume ratio is 1 to the pre-treatment mycelium: 1-10: 1 with the n-hexane/acetone mixed solvent, preferred 3: 1) adopt system for continuously extracting to carry out countercurrent extraction (leaching process is as previously mentioned), extraction conditions is: extract 30 ℃ of temperature, extract solvent load 10mL/g mycelium, return velocity 1.2BV/h, backflow 2-3 time, extraction time 2-4h, several 5 groups of extraction unit group; Extracting solution obtains lycopene concentrated liquor through vacuum concentration.
Embodiment 2
It is described through pretreated mycelium 10g to get embodiment 1, puts in the 500mL round-bottomed flask, adds 400mL n-hexane/acetone mixed extraction solvent, and 40 ℃ are stirred extraction 1h, extract the extraction rate reached 81.42% of Lyeopene under this operational condition three times.
It is described in pretreated mycelium 50g packs chromatography column into to get embodiment 1, adds 500mL n-hexane/acetone mixed solvent, and the flow velocity circulated in countercurrent with 1.2BV/h under 30 ℃ is extracted 1.5h, refluxes the extraction rate reached 88% of Lyeopene under this operational condition three times.
It is described through pretreated mycelium 250g to get embodiment 1, equivalent adds in each chromatography column of the system for continuously extracting with 5 extraction units as shown in Figure 1, extracting solution is discharged after adding a stage extraction of fresh solvent 1.5h in unit 5, unit 2-4 carries out the stage of 22.5min, 45min, 67.5min respectively and extracts, the solvent of unit 2 and 4 is exchanged, the 5 adding fresh solvents in the unit make each unit arrange according to concentration gradient shown in Figure 2 at last; Continue to extract behind the 22.5min being carried out the deslagging charging by the unit 5 of defecation, the saturated solvent of unit 1 is transferred in the container for storing liquid; The opposite direction that unsaturated solvent is successively decreased by lycopene concentration migrates to every a unit; Moved the back fresh solvent has been inserted in unit 4.Each unit extraction conditions is: 30 ℃ of temperature, and 5 groups of extraction unit groups, every group of mycelial solvent of 10mL/g extracts 1.5h with the flow velocity circulated in countercurrent of 1.2BV/h.Other are with embodiment 1, and the extraction yield of Lyeopene can reach 94.76% under this operational condition.
Polytechnic extraction the results are shown in Table 1:
Table 1 extraction process relatively
The Lyeopene extraction yield of dynamic countercurrent extraction is the highest continuously, respectively than paddling process and single-column method height 13.34% and 6.76%, extraction time has shortened 1/3rd than single-column method, solvent load only is 1/6 of a paddling process, extract temperature and be close to normal temperature, demonstrated the superiority of Continuous Countercurrent Extraction.
Claims (10)
1. one kind is utilized mixed solvent to extract lycopene method continuously, it is characterized in that comprising following steps:
A. the Blakeslea trispora fermentation mycelium adds dewatering of ethanol processing, filtering separation mycelium and Ethanol Treatment liquid; Wet mycelium by vacuum-drying and pulverizing, is obtained dry mycelium;
B. the mycelium of handling through step a, add mixed solvent and carry out solid phase-liquid-phase extraction: in each extraction unit of system for continuously extracting, add the mycelium of handling through step a, adopt the mixed extraction solvent to circulate continuously to extract certain hour each unit is arranged by concentration gradient, stage countercurrent extraction to Lyeopene extracts totally again, collects extraction liquid;
C. extraction liquid obtains lycopene concentrated liquor through vacuum concentration in the step (b).
2. method according to claim 1 is characterized in that alcohol concn is between 50%-100% among the step a, and ethanol compares 1 with the volume mass of Blakeslea trispora fermentation mycelium: 1-10: 1, and normal temperature was handled 5-180 minute down.
3. method according to claim 1 and 2 is characterized in that Ethanol Treatment liquid can be recycled through the low-pressure distillation processing.
4. method according to claim 1 is characterized in that among the step a vacuum-drying temperature at 30 ℃-80 ℃, and the vacuum-drying time is at 1-24 hour, preferred 4-12 hour.
5. method according to claim 1, it is characterized in that used mixed extraction solvent of solid phase among the step b-liquid-phase extraction stage is primary solvent with the normal hexane, with acetone, ethyl acetate or sherwood oil is secondary solvent, the volume ratio of primary solvent and secondary solvent is 1: 1-10: 1, preferred n-hexane/acetone mixed solvent, the volume ratio of normal hexane and acetone is 1: 1-5: 1, preferred 2: 1-5: 1.
6. method according to claim 1 is characterized in that system for continuously extracting is made up of 6-16 root chromatography column, container for storing liquid, recycle pump, valve and pipeline among the step b; Each extraction unit is in series by 2-5 root chromatography column, comprises supporting container for storing liquid, recycle pump, valve and pipeline; System for continuously extracting can the lucifuge operation.
7. method according to claim 1, it is characterized in that each unit is arranged by following operation realization by concentration gradient among the step b: unit 1-5 adds the mycelium that equivalent is handled through step a respectively, unit 5 adds fresh mix and extracts solvent extraction t (extraction time in stage) back discharge extracting solution, and unit 2-4 carries out t respectively
1/4, t
2/4, t
3/4The extraction of (being for 1/4,2/4,3/4 extraction time in stage), the solvent of unit 2 and 4 is exchanged, 5 add fresh mix and extract solvents in the unit at last, the concentration gradient shown in when each unit is extracted at the beginning according to Fig. 2 process is arranged, and has promptly made concentration gradient.
8. according to right 7 described methods, it is characterized in that each process of system for continuously extracting all extracts t
1/4The back is carried out the deslagging charging to Lyeopene by the unit 5 of defecation, and the opposite direction that unsaturated solvent is successively decreased by lycopene concentration migrates to every a unit; Through six operating process, all unit are got back to the initial concentration state again, realize operate continuously, as shown in Figure 2.
9. method according to claim 1 is characterized in that the mode of extracting continuously is a countercurrent extraction; Extract temperature and be 20-60 ℃, preferred 30-50 ℃; Extract solvent load and be the 5-40mL/g mycelium, preferred 5-20mL/g mycelium; Return velocity is 0.6-3.6BV/h (BV is a bed volume), preferred 0.6-1.8BV/h; The backflow number of times is preferred 2-3 time 3-6 time; Extraction time is 2-8h, is preferable over 2-4h; Extraction unit group number is the 3-6 group, preferred 5-6 group.
10. method according to claim 1 is characterized in that adding in each extraction unit the mycelium that equivalent is handled through step a.
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CN108017505A (en) * | 2016-11-04 | 2018-05-11 | 嘉必优生物技术(武汉)股份有限公司 | The method for extracting lycopene |
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Application publication date: 20110803 Assignee: Nanjing Siddartha medical science and Technology Co.,Ltd. Assignor: Nanjing Tech University Contract record no.: 2017320000159 Denomination of invention: Method for extracting lycopene continuously Granted publication date: 20131218 License type: Exclusive License Record date: 20170711 |