CN106278978A - The method preparing bata-carotene crystal - Google Patents
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Abstract
The method preparing bata-carotene crystal, comprise the steps: (1) by microorganism fungus kind inoculation fermentation, fermentation liquid is carried out solid-liquid separation by (2), obtains wet thallus；(3) wet thallus is obtained after drying dry mycelium；(4) use organic solvent that dry mycelium is extracted；(5) it is extracted liquid after solid-liquid separation；(6) extract obtains crystalline mother solution through evaporative crystallization；(7) crystalline mother solution is through solid-liquid separation, obtains thick wet crystal；(8) thick wet crystal is after organic solvent washing, and vacuum drying obtains bata-carotene crystal；In step (3), in wet thallus, first add antioxidant, then be dried.The present invention is in the step of dry, solid-liquid separation and evaporative crystallization, some or all of interpolation antioxidant, reduces the loss of bata-carotene during extraction, improves the yield of bata-carotene, the bata-carotene crystal purity simultaneously prepared is higher, and quality is more preferable.
Description
Technical field
The method that the present invention relates to prepare beta-carotene crystal, a kind of microbe-derived beta-carotene crystal
Preparation method.
Background technology
Carotenoid is that one is widely present in plant, animal, microorganism, the closely-related battalion with the health of human body
Supporting material, it mainly includes beta-carotene, lycopene, phylloxanthin etc..Carotenoid not only has anticancer, antioxidation etc. very
High medical value, but also be the important sources of body vitamin A.Carotenoid strengthens as food additive and nutrition
Agent, has obtained the accreditation of the international organizations such as FDA, the European Economic Community, WHO, has been widely used in medicine, food the most especially
The fields such as product, health product and cosmetics.
Natural carotenoid mostlys come from plant.But, vegetable raw material exists under-supply, and the low grade of content lacks
Point, it is impossible to utilize the most on a large scale.Microorganism has that growth and breeding is fast, content is high, unexcellent by seasonal effect etc.
Point, therefore, utilizing fermentable to produce carotenoid is a kind of preferably method.
At present, the main technique extracting the carotenoid in Blakeslea trispora includes: wet thallus mixes through high pressure with water
Homogenizing extracts, wet, dry mycelium and organic solvent extraction.After obtaining crude extract, the step such as isolated and purified obtains the crystal of high-load.
No. 01804173.6 separation disclosing a kind of carotenoid crystals of Chinese Patent No., through height after using wet thallus to mix with water
Pressure homogenizer homogenizing crushes the mixture extracting carotenoid, then with ethanol, saline purging compound.The method extracts class recklessly
Temperature during Radix Raphani element is high, easily causes carotenoid oxidative degradation, and isolated and purified difficulty, and yield is extremely low.Chinese patent Shen
Please No. 201210180281.4 disclose a kind of method using high steam extraction beta-carotene.But, the method
The temperature and pressure used is the highest, easily makes beta-carotene aoxidize, causes product yield low, and affects the quality of product.
Existing beta-carotene crystal of preparing in the way of fermentable mostly has the disadvantage in that dry or extracts
During need through high-temperature process, that easily causes carotenoid sees light, oxidative degradation, causes yield low, and product quality is poor.
Accordingly, it would be desirable to consider that the mode of a kind of improvement is to the loss avoiding carotenoid in preparation process.
Summary of the invention
It is an object of the invention to provide a kind of beta-carotene that can reduce to aoxidize, improve yield and the preparation β-Radix Dauci Sativae of quality
The method of cellulose crystal.
For achieving the above object, the method preparing beta-carotene crystal of the present invention, comprise the steps:
(1) by microorganism fungus kind inoculation fermentation,
(2) fermentation liquid is carried out solid-liquid separation, obtain wet thallus；
(3) wet thallus is obtained after drying dry mycelium；
(4) use organic solvent that dry mycelium is extracted
(5) it is extracted liquid after solid-liquid separation；
(6) extract obtains crystalline mother solution through evaporative crystallization；
(7) crystalline mother solution is through solid-liquid separation, obtains thick wet crystal；
(8) thick wet crystal is after organic solvent washing, and vacuum drying obtains beta-carotene crystal；
Step (3), (4), (6) at least one step in, add antioxidant.
The method preparing beta-carotene crystal foregoing, in step (1), microorganism fungus kind is Blakeslea trispora, Du
Family name's salt alga or yeast.
The method preparing beta-carotene crystal foregoing, in step (3), the addition of antioxidant is wet thallus
The 0.1%～5% of weight.
The method preparing beta-carotene crystal foregoing, in step (4) or (6), the addition of antioxidant is dry
The 0.1%～5% of thalline weight.
The method preparing beta-carotene crystal foregoing, in step (4), dry mycelium and organic solvent quality volume
Ratio is 1:3-1:30.
The method preparing beta-carotene crystal foregoing, in step (4), extraction uses the work of Mechanical Crushing simultaneously
Skill, after Mechanical Crushing, the mean diameter of thalline is not higher than 300 μm.
The method preparing beta-carotene crystal foregoing, in step (4), organic solvent be hexane, dichloromethane,
Petroleum ether, ethyl acetate or acetone.
The present invention prepares the method for beta-carotene and has the advantages that owing to beta-carotene oxidative degradation is mainly given birth to
Become a series of volatility flavor matter, such as alpha, beta-lonone, dihydroactinidiolide, isophorone, oxidation isophorone etc..This
There is considerable influence to the purification of beta-carotene in a large amount of existence of a little oxidative breakdown products, can affect the purity of beta-carotene,
Therefore during dry, solid-liquid separation and evaporative crystallization, some or all of interpolation antioxidant, both reduced and extracted
The loss of beta-carotene in journey, improves the yield of beta-carotene, can prepare purity again higher, the more preferable β-Radix Dauci Sativae of quality
Cellulose crystal.
Detailed description of the invention
Below in conjunction with instantiation, the present invention is described in further detail.
Yield calculates and detects standard or the method for purity
1, the detection method of thalline weight content beta-carotene: accurately weigh 0.01～0.03g sample, accurate 0.0001g,
After glass homogenizer breaking cellular wall, extract by ethyl acetate, repeatedly extract to sample completely colorless, constant volume to 25ml.Use again
Pipet takes 1ml and is diluted to constant volume after certain multiple.With ethyl acetate as reference, pour the solution after constant volume into colorimetric
In ware, the maximum absorption wave strong point in the range of 455 nm ± 2 nm measures absorbance, then according to beta-carotene mark
Accurate
Curve calculates the content beta-carotene in thalline.
2, the computational methods of beta-carotene extraction ratio:
Extraction ratio (%)=m 1 / (m 2* w)
In formula:m 1 : obtain beta-carotene crystal weight；
m 2 : the weight of beta-carotene dry mycelium；
w: the content of beta-carotene in beta-carotene dry mycelium.
3, the detection method of beta-carotene crystal purity: with reference to GB 28310-2012 national food safety standard food
Additive beta-carotene (fermentation method).
Embodiment 1
With Dunaliella salina as fermented bacterium, follow these steps to successively operate:
1) by Dunaliella salina inoculation fermentation, to obtain the water yield be 75.7% wet thallus by centrifugal for fermentation liquid,
2) taking 1kg wet thallus, add 1g dibenzylatiooluene (antioxidant), and mix homogeneously in wet thallus, vacuum is done
The dry 269.3g dry mycelium that obtains, vacuum drying condition is: temperature 80 DEG C, negative pressure-0.085MPa.
3) take the above-mentioned dry thalline of 200g, join in the four-neck flask of 3L, and add 600mL dichloromethane, with height
It is 181um that speed cutter is crushed to thalline mean diameter, and sucking filtration obtains extraction extract and a wet bacteria slag, wet bacteria slag 2L dichloromethane
Alkane carries out reextraction, and sucking filtration obtains two extraction extracts.
4) twice extract is merged, at 50 DEG C, evaporative crystallization under the conditions of-0.08MPa, obtain crystalline mother solution.
5) crystalline mother solution sucking filtration obtaining wet crystal, wet crystal 20ml ethyl acetate is washed, and sucking filtration obtains wet crystalline substance again
Body, wet crystal is at 80 DEG C, under the conditions of-0.085MPa, is vacuum dried 2h, obtains finished product carotenoid crystals.After testing, β-recklessly
The extraction ratio of Radix Raphani cellulose crystal is 66.1%, and beta-carotene purity is 97.3% after testing.
6) by above-mentioned identical technique, carry out controlled trial without antioxidant, be computed carrying of beta-carotene crystal
The rate of taking is 60.9%, and beta-carotene purity is 95.9% after testing.
Embodiment 2
With yeast as fermented bacterium, follow these steps to successively operate:
1) yeast-inoculated is fermented, fermentation liquid is centrifuged and obtains the wet thallus that water content is 80.3%；
2) taking above-mentioned 10kg wet thallus, wet thallus heavily adds 75g vitamin E (antioxidant), is sufficiently mixed and stirs, through cold
Freezing and be dried to obtain 2.17kg dry mycelium, lyophilization condition is: vacuum 20Pa, and catcher temperature is-40 DEG C, is dried 18h.
3) take 1kg dry mycelium, put in the reactor of 50L, add 30L normal hexane, be crushed to sand mill circulation
Thalline mean diameter is 217um, is centrifugally separating to obtain extraction extract and a wet bacteria slag, and wet bacteria slag continuously adds 30L normal hexane,
55 DEG C of extraction 1h, are centrifuged and obtain two extraction extract and wet bacteria slags.
4) merge an extraction and two extraction extracts, at 43 DEG C, evaporative crystallization under conditions of-0.085MPa, obtain crystalline mother solution.
5) above-mentioned crystalline mother solution is centrifugally separating to obtain wet crystal, wet crystal 500ml normal hexane agitator treating, again from
Gains in depth of comprehension are to wet crystal, and wet crystal, at 80 DEG C, is vacuum dried 2h and obtains finished product carotenoid crystals under the conditions of-0.085MPa.Through meter
Calculating carotenoids crystal yield is 69.1%, and beta-carotene purity is 97.7% after testing.
6) by above-mentioned identical technique, carry out controlled trial without antioxidant, be computed the receipts of beta-carotene crystal
Rate is 62.1%, and beta-carotene purity is 96.1% after testing.
Embodiment 3
With yeast as fermented bacterium, follow these steps to successively operate:
1) yeast-inoculated is fermented, fermentation liquid is centrifuged and obtains the wet thallus that water content is 80.1%；
2) taking above-mentioned 50kg wet thallus, wet thallus heavily adds 150g sodium L-ascorbate-2-phosphate (antioxidant), is sufficiently mixed stirring
Uniformly, carrying out spray drying and obtain 20.78kg dry mycelium, spray drying condition is: hot blast temperature 130 DEG C, temperature of charge 65 DEG C,
Blower fan frequency is 45Hz, and charging rate is 5kg/h.
3) take 5kg dry mycelium, put in the reactor of 100L, add 50L normal hexane, be crushed to sand mill circulation
Thalline mean diameter is 193um, is centrifugally separating to obtain extraction extract and a wet bacteria slag, and wet bacteria slag continuously adds 50L normal hexane,
55 DEG C of extraction 1h, are centrifuged and obtain two extraction extract and wet bacteria slags.
4) merge an extraction and two extraction extracts, at 43 DEG C, evaporative crystallization under conditions of-0.085MPa, obtain crystalline mother solution.
5) above-mentioned crystalline mother solution is centrifugally separating to obtain wet crystal, wet crystal 250ml ethanol agitator treating, recentrifuge
Obtaining wet crystal, wet crystal, at 80 DEG C, is vacuum dried 2h and obtains finished product carotenoid crystals under the conditions of-0.085MPa.It is computed
Carotenoids crystal yield is 69.1%, and beta-carotene purity is 97.7% after testing.
6) by above-mentioned identical technique, carry out controlled trial without antioxidant, be computed the receipts of beta-carotene crystal
Rate is 61.7%, and beta-carotene purity is 96.1% after testing.
Embodiment 4
Using Blakeslea trispora strain as fermented bacterium, follow these steps to successively operate:
1) by Blakeslea trispora inoculation fermentation, it is 55.1% wet thallus by obtaining water content after fermentation liquor filter press,
2) take 500kg wet thallus pulverizer to crush, add 25kg ethylparaben (antioxidant) mix homogeneously, then
Obtaining 241.1kg dry mycelium through airpillow-dry, airpillow-dry condition is: hot blast temperature 120 DEG C, temperature of charge 55 DEG C, blower fan frequency
50Hz。
3) take the above-mentioned dry thalline of 5kg, put in 200L reactor, and add 100L dichloromethane, use high shear
It is 300um that colloid mill circulation is crushed to thalline mean diameter, is warming up to 55 DEG C of stirring extraction 1h, and after settlement separate, upper strata extracts
Taking liquid 5um bag filter and 0.5um filter stick filter is filtrated to get an extraction extract, lower floor's wet bacteria slag continuously adds 100L
Petroleum ether, extracts 1.5h at 55 DEG C, and extraction mixed liquor 5um bag filter and 0.5um filter stick filter are filtrated to get two extractions
Extract and wet bacteria slag.
4) twice extract is merged, at 48 DEG C, evaporative crystallization under the conditions of-0.08MPa, obtain crystalline mother solution.
5) crystalline mother solution sucking filtration obtaining thick wet crystal, thick wet crystal 500ml petroleum ether, sucking filtration obtains wet again
Crystal, wet crystal is at 80 DEG C, under the conditions of-0.085MPa, is vacuum dried 2h, obtains finished product carotenoid crystals.It is computed class recklessly
The extraction ratio of Radix Raphani cellulose crystal is 73.3%, and beta-carotene purity is 98.1% after testing.
6) by above-mentioned identical technique, carry out controlled trial without antioxidant, be computed carrying of beta-carotene crystal
The rate of taking is 62.9%, and beta-carotene purity is 96.9% after testing.
Embodiment 5
With Dunaliella salina as fermented bacterium, follow these steps to successively operate:
1) by Dunaliella salina inoculation fermentation, to obtain the water yield be 75.7% wet thallus by centrifugal for fermentation liquid,
2) taking 1kg wet thallus, vacuum drying obtains 269.3g dry mycelium, and vacuum drying condition is: temperature 80 DEG C, and negative pressure-
0.085MPa。
3) take the above-mentioned dry thalline of 200g, be added thereto to 0.2g vitamin E (antioxidant), join four necks of 3L
In flask, and adding 600mL ethyl acetate, being crushed to thalline mean diameter with high-speed shearing machine is 151um, and sucking filtration obtains an extraction
Extract and wet bacteria slag, wet bacteria slag 2L ethyl acetate carries out reextraction, and sucking filtration obtains two extraction extracts.
4) twice extract is merged, at 50 DEG C, evaporative crystallization under the conditions of-0.08MPa, obtain crystalline mother solution.
5) crystalline mother solution sucking filtration obtaining wet crystal, wet crystal 20ml washing with alcohol, sucking filtration obtains wet crystal again, wet
Crystal is at 80 DEG C, under the conditions of-0.085MPa, is vacuum dried 2h, obtains finished product carotenoid crystals.After testing, beta-carotene
The extraction ratio of crystal is 64.1%, and beta-carotene purity is 97.3% after testing.
6) by above-mentioned identical technique, carry out controlled trial without antioxidant, be computed carrying of beta-carotene crystal
The rate of taking is 60.9%, and beta-carotene purity is 95.9% after testing.
Embodiment 6
With yeast as fermented bacterium, follow these steps to successively operate:
1) yeast-inoculated is fermented, fermentation liquid is centrifuged and obtains the wet thallus that water content is 80.5%；
2) take above-mentioned 10kg wet thallus, be sufficiently mixed and stir, the freeze-dried 2.07kg dry mycelium that obtains, lyophilization bar
Part is: vacuum 20Pa, and catcher temperature is-40 DEG C, is dried 20h.
3) take 1kg dry mycelium, put in the reactor of 30L, add 50g dibenzylatiooluene (antioxidant), then
Adding 30L normal hexane, with sand mill circulation, to be crushed to thalline mean diameter be 133um, be centrifugally separating to obtain an extraction extract and
Wet bacteria slag, wet bacteria slag continuously adds 30L normal hexane, extracts 1h at 55 DEG C, is centrifuged and obtains two extraction extract and wet bacteria slags.
4) merge an extraction and two extraction extracts, at 43 DEG C, evaporative crystallization under conditions of-0.085MPa, obtain crystalline mother solution.
5) above-mentioned crystalline mother solution is centrifugally separating to obtain wet crystal, wet crystal 250ml normal hexane agitator treating, again from
Gains in depth of comprehension are to wet crystal, and wet crystal, at 80 DEG C, is vacuum dried 2h and obtains finished product carotenoid crystals under the conditions of-0.085MPa.Through meter
Calculating carotenoids crystal yield is 69.1%, and beta-carotene purity is 97.7% after testing.
6) by above-mentioned identical technique, carry out controlled trial without antioxidant, be computed the receipts of beta-carotene crystal
Rate is 63.3%, and beta-carotene purity is 96.1% after testing.
Embodiment 7
With yeast as fermented bacterium, follow these steps to successively operate:
1) yeast-inoculated is fermented, fermentation liquid is centrifuged and obtains the wet thallus that water content is 80.1%；
2) take above-mentioned 50kg wet thallus, be sufficiently mixed and stir, carry out spray drying and obtain 20.78kg dry mycelium, spray dried
Dry condition is: hot blast temperature 130 DEG C, temperature of charge 65 DEG C, and blower fan frequency is 45Hz, and charging rate is 5kg/h.
3) take 5kg dry mycelium, put in the reactor of 100L, add 100g sodium L-ascorbate-2-phosphate (antioxidant),
Adding 50L normal hexane, being crushed to thalline mean diameter with sand mill circulation is 153um, is centrifugally separating to obtain an extraction extract
And wet bacteria slag, wet bacteria slag continuously adds 50L normal hexane, extracts 1h at 55 DEG C, is centrifuged and obtains two extraction extract and wet bacteria slags.
4) merge an extraction and two extraction extracts, at 43 DEG C, evaporative crystallization under conditions of-0.085MPa, obtain crystalline mother solution.
5) above-mentioned crystalline mother solution is centrifugally separating to obtain wet crystal, wet crystal 250ml ethyl acetate agitator treating, again
Being centrifuged and obtain wet crystal, wet crystal, at 80 DEG C, is vacuum dried 2h and obtains finished product carotenoid crystals under the conditions of-0.085MPa.Warp
Calculating carotenoids crystal yield is 69.1%, and beta-carotene purity is 97.7% after testing.
6) by above-mentioned identical technique, carry out controlled trial without antioxidant, be computed the receipts of beta-carotene crystal
Rate is 63.3%, and beta-carotene purity is 96.1% after testing.
Embodiment 8
Using Blakeslea trispora strain as fermented bacterium, follow these steps to successively operate:
1) by Blakeslea trispora inoculation fermentation, it is 55.1% wet thallus by obtaining water content after fermentation liquor filter press,
2) taking 500kg wet thallus pulverizer to crush, obtain 233.1kg dry mycelium through airpillow-dry, airpillow-dry condition is: hot blast
Temperature 120 DEG C, temperature of charge 55 DEG C, blower fan frequency 50Hz.
3) take the above-mentioned dry thalline of 50kg, put in 1000L reactor, add 1kg Herba Rosmarini Officinalis (antioxidant), and
Adding 500L petroleum ether, being crushed to thalline mean diameter with high-shear colloid mill circulation is 231um, is warming up to 55 DEG C of stirring extractions
1h, after settlement separate, upper layer of extraction liquid 5um bag filter and 0.5um filter stick filter are filtrated to get an extraction extract,
Lower floor's wet bacteria slag continuously adds 500L petroleum ether, extracts 1.5h at 55 DEG C, extracts mixed liquor 5um bag filter and 0.5um
Filter stick filter is filtrated to get two extraction extract and wet bacteria slags.
4) twice extract is merged, at 48 DEG C, evaporative crystallization under the conditions of-0.08MPa, obtain crystalline mother solution.
5) crystalline mother solution sucking filtration obtaining thick wet crystal, thick wet crystal 5L ethanol, sucking filtration obtains wet crystal, wet crystalline substance again
Body is at 80 DEG C, under the conditions of-0.085MPa, is vacuum dried 2h, obtains finished product carotenoid crystals.It is computed carotenoid crystals
Extraction ratio be 73.3%, beta-carotene purity is 98.1% after testing.
6) by above-mentioned identical technique, carry out controlled trial without antioxidant, be computed carrying of beta-carotene crystal
The rate of taking is 62.9%, and beta-carotene purity is 96.9% after testing.
Embodiment 9
With Dunaliella salina as fermented bacterium, follow these steps to successively operate:
1) by Dunaliella salina inoculation fermentation, to obtain the water yield be 75.9% wet thallus by centrifugal for fermentation liquid,
2) taking 1kg wet thallus, vacuum drying obtains 267.3g dry mycelium, and vacuum drying condition is: temperature 80 DEG C, and negative pressure-
0.085MPa。
3) take the above-mentioned dry thalline of 200g, join in the four-neck flask of 3L, and add 600mL dichloromethane, with height
It is 181um that speed cutter is crushed to thalline mean diameter, and sucking filtration obtains extraction extract and a wet bacteria slag, wet bacteria slag 2L dichloromethane
Alkane carries out reextraction, and sucking filtration obtains two extraction extracts.
4) merge twice extract, be added thereto to 0.2g vitamin E (antioxidant), at 50 DEG C ,-0.08MPa condition
Lower evaporative crystallization, obtains crystalline mother solution.
5) crystalline mother solution sucking filtration obtaining wet crystal, wet crystal 50ml washing with alcohol, sucking filtration obtains wet crystal again, wet
Crystal is at 80 DEG C, under the conditions of-0.085MPa, is vacuum dried 2h, obtains finished product carotenoid crystals.After testing, beta-carotene
The extraction ratio of crystal is 64.1%, and beta-carotene purity is 97.3% after testing.
6) by above-mentioned identical technique, carry out controlled trial without antioxidant, be computed carrying of beta-carotene crystal
The rate of taking is 60.9%, and beta-carotene purity is 95.9% after testing.
Embodiment 10
With yeast as fermented bacterium, follow these steps to successively operate:
1) yeast-inoculated is fermented, fermentation liquid is centrifuged and obtains the wet thallus that water content is 80.3%；
2) take above-mentioned 10kg wet thallus, be sufficiently mixed and stir, the freeze-dried 2.1kg dry mycelium that obtains, lyophilization bar
Part is: vacuum 20Pa, and catcher temperature is-40 DEG C, is dried 20h.
3) take 1kg dry mycelium, put in the reactor of 30L, add 30L normal hexane, be crushed to sand mill circulation
Thalline mean diameter is 300um, is centrifugally separating to obtain extraction extract and a wet bacteria slag, and wet bacteria slag continuously adds 30L normal hexane,
55 DEG C of extraction 1h, are centrifuged and obtain two extraction extract and wet bacteria slags.
4) merge an extraction and two extraction extracts, add 50g dibenzylatiooluene (antioxidant), at 43 DEG C ,-
Evaporative crystallization under conditions of 0.085MPa, obtains crystalline mother solution.
5) above-mentioned crystalline mother solution is centrifugally separating to obtain wet crystal, wet crystal 250ml ethyl acetate agitator treating, again
Being centrifuged and obtain wet crystal, wet crystal, at 80 DEG C, is vacuum dried 2h and obtains finished product carotenoid crystals under the conditions of-0.085MPa.Warp
Calculating carotenoids crystal yield is 69.1%, and beta-carotene purity is 97.7% after testing.
6) by above-mentioned identical technique, carry out controlled trial without antioxidant, be computed the receipts of beta-carotene crystal
Rate is 63.3%, and beta-carotene purity is 96.1% after testing.
Embodiment 11
With yeast as fermented bacterium, follow these steps to successively operate:
1) yeast-inoculated is fermented, fermentation liquid is centrifuged and obtains the wet thallus that water content is 80.9%；
2) take above-mentioned 50kg wet thallus, be sufficiently mixed and stir, carry out spray drying and obtain 20.78kg dry mycelium, spray dried
Dry condition is: hot blast temperature 130 DEG C, temperature of charge 65 DEG C, and blower fan frequency is 45Hz, and charging rate is 5kg/h.
3) take 5kg dry mycelium, put in the reactor of 100L, add 50L normal hexane, be crushed to sand mill circulation
Thalline mean diameter is 300um, is centrifugally separating to obtain extraction extract and a wet bacteria slag, and wet bacteria slag continuously adds 50L normal hexane,
55 DEG C of extraction 1h, are centrifuged and obtain two extraction extract and wet bacteria slags.
4) merge an extraction and two extraction extracts, add 100g sodium L-ascorbate-2-phosphate (antioxidant), at 43 DEG C ,-
Evaporative crystallization under conditions of 0.085MPa, obtains crystalline mother solution.
5) above-mentioned crystalline mother solution is centrifugally separating to obtain wet crystal, wet crystal 250ml normal hexane agitator treating, again from
Gains in depth of comprehension are to wet crystal, and wet crystal, at 80 DEG C, is vacuum dried 2h and obtains finished product carotenoid crystals under the conditions of-0.085MPa.Through meter
Calculating carotenoids crystal yield is 69.1%, and beta-carotene purity is 97.7% after testing.
6) by above-mentioned identical technique, carry out controlled trial without antioxidant, be computed the receipts of beta-carotene crystal
Rate is 63.3%, and beta-carotene purity is 96.1% after testing.
Embodiment 12
Using Blakeslea trispora strain as fermented bacterium, follow these steps to successively operate:
1) by Blakeslea trispora inoculation fermentation, it is 55.1% wet thallus by obtaining water content after fermentation liquor filter press,
2) taking 500kg wet thallus pulverizer to crush, obtain 233.1kg dry mycelium through airpillow-dry, airpillow-dry condition is: hot blast
Temperature 120 DEG C, temperature of charge 55 DEG C, blower fan frequency 50Hz.
3) take the above-mentioned dry thalline of 50kg, put in 2000L reactor, and add 1000L petroleum ether, use high shear
It is 231um that colloid mill circulation is crushed to thalline mean diameter, then heats to 55 DEG C, extracts 1h, and after settlement separate, upper strata extracts
Take mixed liquor 5um bag filter and 0.5um filter stick filter is filtrated to get an extraction extract, continue in lower floor's wet bacteria slag
Adding 600L petroleum ether, extract 1.5h at 55 DEG C, extraction mixed liquor 5um bag filter and 0.5um filter stick filter filter
Obtain two extraction extract and wet bacteria slags.
4) merge twice extract, add 2kg Herba Rosmarini Officinalis (antioxidant), at 48 DEG C, evaporation knot under the conditions of-0.08MPa
Crystalline substance, obtains crystalline mother solution.
5) crystalline mother solution sucking filtration obtaining thick wet crystal, thick wet crystal 10L ethyl acetate is washed, and sucking filtration obtains wet again
Crystal, wet crystal is at 80 DEG C, under the conditions of-0.085MPa, is vacuum dried 2h, obtains finished product carotenoid crystals.It is computed class recklessly
The extraction ratio of Radix Raphani cellulose crystal is 73.1%, and beta-carotene purity is 98.1% after testing.
6) by above-mentioned identical technique, carry out controlled trial without antioxidant, be computed carrying of beta-carotene crystal
The rate of taking is 61.9%, and beta-carotene purity is 96.9% after testing.
Embodiment 13
Using Blakeslea trispora strain as fermented bacterium, follow these steps to successively operate:
1) by Blakeslea trispora inoculation fermentation, it is 55.1% wet thallus by obtaining water content after fermentation liquor filter press,
2) taking 500kg wet thallus pulverizer to crush, obtain 233.1kg dry mycelium through airpillow-dry, airpillow-dry condition is: hot blast
Temperature 120 DEG C, temperature of charge 55 DEG C, blower fan frequency 50Hz.
7) take the above-mentioned dry thalline of 200kg, put in 5000L reactor, and add 2000L petroleum ether, cut with height
Cutting colloid mill circulation and being crushed to thalline mean diameter is 231um, then heats to 55 DEG C, extracts 1h, after settlement separate, upper strata
Extraction mixed liquor 5um bag filter and 0.5um filter stick filter are filtrated to get an extraction extract, to lower floor's wet bacteria slag relaying
Continuous addition 2000L petroleum ether, extracts 1.5h at 55 DEG C, extracts mixed liquor 5um bag filter and 0.5um filter stick filter mistake
Filter obtains two extraction extract and wet bacteria slags.
3) merge twice extract, add 5kg ethylparaben (antioxidant), at 48 DEG C ,-0.08MPa bar
Evaporative crystallization under part, obtains crystalline mother solution.
4) crystalline mother solution sucking filtration obtaining thick wet crystal, thick wet crystal 500ml dichloromethane washs, and sucking filtration obtains again
Wet crystal, wet crystal is at 80 DEG C, under the conditions of-0.085MPa, is vacuum dried 2h, obtains finished product carotenoid crystals.It is computed class
The extraction ratio of carotene crystals is 73.3%, and beta-carotene purity is 98.1% after testing.
5) by above-mentioned identical technique, carry out controlled trial without antioxidant, be computed carrying of beta-carotene crystal
The rate of taking is 62.9%, and beta-carotene purity is 96.9% after testing.
Embodiment 14
With Dunaliella salina as fermented bacterium, follow these steps to successively operate:
1) by Dunaliella salina inoculation fermentation, to obtain the water yield be 75.7% wet thallus by centrifugal for fermentation liquid,
2) taking 1kg wet thallus, add 0.5g dibenzylatiooluene (antioxidant), mix homogeneously, vacuum drying obtains
261.3g dry mycelium, vacuum drying condition is: temperature 80 DEG C, negative pressure-0.085MPa.
3) take the above-mentioned dry thalline of 200g, join in the four-neck flask of 3L, add 0.5g vitamin E (antioxidation
Agent), add 600mL dichloromethane, being crushed to thalline mean diameter with high-speed shearing machine is 181um, and sucking filtration obtains an extraction extraction
Liquid and wet bacteria slag, wet bacteria slag 2L dichloromethane carries out reextraction, and sucking filtration obtains two extraction extracts.
4) twice extract is merged, at 50 DEG C, evaporative crystallization under the conditions of-0.08MPa, obtain crystalline mother solution.
5) crystalline mother solution sucking filtration obtaining wet crystal, wet crystal 20ml dichloromethane washs, and sucking filtration obtains wet crystalline substance again
Body, wet crystal is at 80 DEG C, under the conditions of-0.085MPa, is vacuum dried 2h, obtains finished product carotenoid crystals.After testing, β-recklessly
The extraction ratio of Radix Raphani cellulose crystal is 64.1%, and beta-carotene purity is 97.3% after testing.
6) by above-mentioned identical technique, carry out controlled trial without antioxidant, be computed carrying of beta-carotene crystal
The rate of taking is 60.9%, and beta-carotene purity is 95.9% after testing.
Embodiment 15
With yeast as fermented bacterium, follow these steps to successively operate:
1) yeast-inoculated is fermented, fermentation liquid is centrifuged and obtains the wet thallus that water content is 80.9%；
2) take above-mentioned 10kg wet thallus, add 50gVc cetylate (antioxidant), be sufficiently mixed and stir, spray
Being dried to obtain 2.18kg dry mycelium, spray drying condition is: hot blast temperature 130 DEG C, temperature of charge 65 DEG C, and blower fan frequency is
45Hz, charging rate is 5kg/h.
3) take 2kg dry mycelium, put in the reactor of 50L, add 20L normal hexane, be crushed to sand mill circulation
Thalline mean diameter is 300um, then at 550 stirring extraction 1h, is centrifugally separating to obtain extraction extract and a wet bacteria slag, and wet bacteria slag continues
Continuous addition 20L normal hexane, extracts 1h at 55 DEG C, is centrifuged and obtains two extraction extract and wet bacteria slags.
4) merge an extraction and two extraction extracts, add 50g Herba Rosmarini Officinalis (antioxidant), at 43 DEG C, the condition of-0.085MPa
Lower evaporative crystallization, obtains crystalline mother solution.
5) above-mentioned crystalline mother solution is centrifugally separating to obtain wet crystal, wet crystal 250ml normal hexane agitator treating, again from
Gains in depth of comprehension are to wet crystal, and wet crystal, at 80 DEG C, is vacuum dried 2h and obtains finished product carotenoid crystals under the conditions of-0.085MPa.Through meter
Calculating carotenoids crystal yield is 69.1%, and beta-carotene purity is 97.7% after testing.
6) by above-mentioned identical technique, carry out controlled trial without antioxidant, be computed the receipts of beta-carotene crystal
Rate is 63.3%, and beta-carotene purity is 96.1% after testing.
Embodiment 16
Using Blakeslea trispora strain as fermented bacterium, follow these steps to successively operate:
1) by Blakeslea trispora inoculation fermentation, it is 55.1% wet thallus by obtaining water content after fermentation liquor filter press,
2) taking 50kg wet thallus pulverizer to crush, obtain 23.1kg dry mycelium through airpillow-dry, airpillow-dry condition is: hot blast temperature
Spend 120 DEG C, temperature of charge 55 DEG C, blower fan frequency 50Hz.
3) take the above-mentioned dry thalline of 10kg, put in 200L reactor, add 250g ethylparaben
(antioxidant), and add 100L petroleum ether, being crushed to thalline mean diameter with high-shear colloid mill circulation is 231um, then
It is warming up to 55 DEG C, extracts 1h, after settlement separate, upper strata extraction mixed liquor 5um bag filter and 0.5um filter stick filter
It is filtrated to get an extraction extract, in lower floor's wet bacteria slag, continuously adds 100L petroleum ether, extract 1.5h at 55 DEG C, extract mixed liquor
It is filtrated to get two extraction extract and wet bacteria slags with 5um bag filter and 0.5um filter stick filter.
4) merge twice extract, add 250g vitamin E (antioxidant), at 48 DEG C, evaporate under the conditions of-0.08MPa
Crystallization, obtains crystalline mother solution.
5) crystalline mother solution sucking filtration obtaining thick wet crystal, thick wet crystal 2L dichloromethane washs, and sucking filtration obtains wet again
Crystal, wet crystal is at 80 DEG C, under the conditions of-0.085MPa, is vacuum dried 2h, obtains finished product carotenoid crystals.It is computed class recklessly
The extraction ratio of Radix Raphani cellulose crystal is 73.3%, and beta-carotene purity is 98.1% after testing.
6) by above-mentioned identical technique, carry out controlled trial without antioxidant, be computed carrying of beta-carotene crystal
The rate of taking is 62.9%, and beta-carotene purity is 96.9% after testing.
Embodiment 17
Using Blakeslea trispora strain as fermented bacterium, follow these steps to successively operate:
7) by Blakeslea trispora inoculation fermentation, it is 55.1% wet thallus by obtaining water content after fermentation liquor filter press,
8) take 500kg wet thallus pulverizer to crush, add 2.5kg dibutyl strong basis toluene (antioxidant), mix homogeneously, warp
Airpillow-dry obtains 233.1kg dry mycelium, and airpillow-dry condition is: hot blast temperature 120 DEG C, temperature of charge 55 DEG C, blower fan frequency
50Hz。
8) take the above-mentioned dry thalline of 200kg, put in 5000L reactor, add 1kg vitamin E (antioxidant),
And add 2000L petroleum ether, being crushed to thalline mean diameter with high-shear colloid mill circulation is 231um, then heats to 55 DEG C,
Extraction 1h, after settlement separate, upper strata extraction mixed liquor 5um bag filter and 0.5um filter stick filter are filtrated to get one
Extraction extract, continuously adds 2000L petroleum ether in lower floor's wet bacteria slag, extracts 1.5h at 55 DEG C, extracts mixed liquor 5um pocket type
Filter and 0.5um filter stick filter are filtrated to get two extraction extract and wet bacteria slags.
9) merge twice extract, add 1kg ethylparaben (antioxidant), at 48 DEG C ,-0.08MPa bar
Evaporative crystallization under part, obtains crystalline mother solution.
10) crystalline mother solution sucking filtration obtaining thick wet crystal, thick wet crystal 500ml dichloromethane washs, and sucking filtration obtains again
To wet crystal, wet crystal is at 80 DEG C, under the conditions of-0.085MPa, is vacuum dried 2h, obtains finished product carotenoid crystals.It is computed
The extraction ratio of carotenoid crystals is 80.1%, and beta-carotene purity is 99.1% after testing.
11) by above-mentioned identical technique, carry out controlled trial without antioxidant, be computed beta-carotene crystal
Extraction ratio is 61.9%, and beta-carotene purity is 96.9% after testing.
The present invention prepare the method for beta-carotene have the advantages that being dried, solid-liquid separation and evaporative crystallization
In step, some or all of interpolation antioxidant, reduce the loss of beta-carotene during extraction, improve β-Radix Dauci Sativae
The yield of element, the beta-carotene crystal purity simultaneously prepared is higher, and quality is more preferable.
Antioxidant mentioned in the present invention, is not limited in embodiment cited type, and other in use have
The product having same effect belongs to protection scope of the present invention.
Claims (8)
1. the method preparing beta-carotene crystal, comprises the steps:
(1) by microorganism fungus kind inoculation fermentation,
(2) fermentation liquid is carried out solid-liquid separation, obtain wet thallus；
(3) wet thallus is obtained after drying dry mycelium；
(4) use organic solvent that dry mycelium is extracted；
(5) it is extracted liquid after solid-liquid separation；
(6) extract obtains crystalline mother solution through evaporative crystallization；
(7) crystalline mother solution is through solid-liquid separation, obtains thick wet crystal；
(8) thick wet crystal is after organic solvent washing, and vacuum drying obtains beta-carotene crystal；
It is characterized in that: in step (3), in wet thallus, first add antioxidant, then be dried.
The method preparing beta-carotene crystal the most according to claim 1, it is characterised in that: in step (1), microorganism
Strain is Blakeslea trispora, Dunaliella salina or yeast.
The method preparing beta-carotene crystal the most according to claim 1, it is characterised in that: in step (3), antioxidation
The addition of agent is the 0.1%～5% of wet thallus weight.
The method preparing beta-carotene crystal the most according to claim 1, it is characterised in that: described antioxidant is two
Butylated hydroxytoluene, ethylparaben, sodium L-ascorbate-2-phosphate, vitamin E or Herba Rosmarini Officinalis.
The method preparing beta-carotene crystal the most according to claim 1, it is characterised in that: in step (4), dry mycelium
It is 1:3-1:30 with organic solvent mass volume ratio.
The method preparing beta-carotene crystal the most according to claim 1, it is characterised in that: in step (4), extraction is same
Time use Mechanical Crushing, after Mechanical Crushing, the mean diameter of thalline is not higher than 300 μm.
The method preparing beta-carotene crystal the most according to claim 1, it is characterised in that: in step (4), You Jirong
Agent is hexane, dichloromethane, petroleum ether, ethyl acetate or acetone.
The method preparing beta-carotene crystal the most according to claim 1, it is characterised in that: in step (5), by solid-liquid
The wet bacteria slag that obtains after separation is repeated is obtained by extraction extract, is merged by all extracts.
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| PCT/CN2017/093527 WO2018028406A1 (en) | 2016-08-09 | 2017-07-19 | Method for preparing beta carotene crystals |
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| WO2018028404A1 (en) * | 2016-08-09 | 2018-02-15 | 嘉必优生物技术（武汉）股份有限公司 | Method for preparing β-carotene crystal |
| WO2018028406A1 (en) * | 2016-08-09 | 2018-02-15 | 嘉必优生物技术（武汉）股份有限公司 | Method for preparing beta carotene crystals |
| WO2018028402A1 (en) * | 2016-08-09 | 2018-02-15 | 嘉必优生物技术（武汉）股份有限公司 | Method for preparing beta carotene crystals |
| WO2018028405A1 (en) * | 2016-08-09 | 2018-02-15 | 嘉必优生物技术（武汉）股份有限公司 | Method for preparing beta carotene crystals |
| CN110407659A (en) * | 2019-08-05 | 2019-11-05 | 嘉必优生物技术（武汉）股份有限公司 | A kind of Extraction of carotenoid pigment method |
| CN114133348A (en) * | 2021-11-09 | 2022-03-04 | 湖北广济药业股份有限公司 | Method for extracting high-purity all-trans beta-carotene |
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| CN114133348A (en) * | 2021-11-09 | 2022-03-04 | 湖北广济药业股份有限公司 | Method for extracting high-purity all-trans beta-carotene |
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