CN101285081A - New process for preparing theaflavine - Google Patents
New process for preparing theaflavine Download PDFInfo
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- CN101285081A CN101285081A CNA2008100235815A CN200810023581A CN101285081A CN 101285081 A CN101285081 A CN 101285081A CN A2008100235815 A CNA2008100235815 A CN A2008100235815A CN 200810023581 A CN200810023581 A CN 200810023581A CN 101285081 A CN101285081 A CN 101285081A
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- IPMYMEWFZKHGAX-ZKSIBHASSA-N theaflavin Chemical compound C1=C2C([C@H]3OC4=CC(O)=CC(O)=C4C[C@H]3O)=CC(O)=C(O)C2=C(O)C(=O)C=C1[C@@H]1[C@H](O)CC2=C(O)C=C(O)C=C2O1 IPMYMEWFZKHGAX-ZKSIBHASSA-N 0.000 title abstract description 6
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- UXRMWRBWCAGDQB-UHFFFAOYSA-N Theaflavin Natural products C1=CC(C2C(CC3=C(O)C=C(O)C=C3O2)O)=C(O)C(=O)C2=C1C(C1OC3=CC(O)=CC(O)=C3CC1O)=CC(O)=C2O UXRMWRBWCAGDQB-UHFFFAOYSA-N 0.000 abstract 4
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- LNTHITQWFMADLM-UHFFFAOYSA-N anhydrous gallic acid Natural products OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 2
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- Medicines Containing Plant Substances (AREA)
- Tea And Coffee (AREA)
Abstract
The invention provides a new process for using the enzyme owned by tea to converting tea polyphenol in the tea into theaflavin through biotransformation. The preparation process is as follows: adding fermenting enzyme made from fresh tea into green tea extracted by ethyl acetate, carrying out stirring and fermentation under the condition of pure oxygen, then going through separation, concentration, washing, conversion dissolving and filtration, and at last carrying out vacuum freeze drying, crushing and screening to obtain qualified theaflavin product. The theaflavin product made through the process has a stable quality, high theaflavin content, high yield and low cost. In addition, the method adopts pure ester phase oxidative fermentation, thereby solving the problem that the three phases are incapable of being separated after the traditional ester, water and refuse mixed-phase fermentation, and consequently carrying out stable and controllable industrialized production.
Description
Technical field
The present invention relates to a kind of novel process for preparing theoflavin, particularly a kind of enzyme that utilizes tealeaves self prepares the tea-polyphenol in the tealeaves novel process of theoflavin by bio-transformation.
Background technology
Cardiovascular and cerebrovascular diseases is the serious disease of harm humans health, data presentation according to the modern medicine diseases monitoring, whole world every day, numbers such as the heart stalk that China causes because of hyperlipidemia every year, cerebral infarction, apoplexy rose with annual 12% speed because of more than nearly 3600 people of cardiovascular and cerebrovascular diseases death toll.Cardiovascular and cerebrovascular diseases has become first killer who engulfs human health, and people also more and more pay attention to prevention and the treatment to it, and studies show that, theoflavin has best prevention and result of treatment to these diseases.
Theoflavin is a kind of natural pigment of the big fragrant lopps that catechins forms through the fermentation oxidation in the tealeaves, is by finding in the black tea the earliest, is topmost active substance in the black tea, and concrete extremely strong physiologically active is described as the DHA (docosahexaenoic acid) in the tealeaves.Because the powerful effect of theoflavin, so the research of theoflavin is become the heat subject of countries in the world medical circle, China since the eighties in 20th century scientific worker just theoflavin is constantly studied, and carried out corresponding clinical trial, finally opened the pharmacological effect of theoflavin, and along with going deep into of studying, the increasing function of theoflavin is found.Its major function and Application Areas are:
One, to the effect of cardiovascular and cerebrovascular diseases aspect, show as mainly that regulating blood fat is unusual, anti-freezing, short fibrinolytic, reduce blood viscosity effect, lipoid peroxidization resistant, damage has provide protection, microcirculation improvement etc. to animal cardiac muscle cell acute ischemia.
Two, anti-mattress anti-inflammatory aspect, 4 monomers of theoflavin and theoflavin to meat poison gemma bar mattress, bacillus enteritidis, gold-coloured staphylococci, bacillus capsulatus, bacillus cercus, will is congratulated bacterium that significant inhibitory effect is all arranged.Theaflavine monogallate in the theoflavin under 1mg/mL concentration, can kill Whooping cough in 24 hours fully.
Three, powerful antioxidant can be used for removing free radical.
In addition, theoflavin also has the inhibition tumor growth, suppress the HIV (human immunodeficiency virus) effect, studies show that theoflavin and gallic acid ester have restraining effect to the reversed transcriptive enzyme of virus of AIDS (comprising HIV (human immunodeficiency virus) I type (HIV-1)) and the DNA and the rna polymerase activity of various cells.Theoflavin and gallic acid ester thereof not only suppress reversed transcriptive enzyme, and suppress human DNA Polymerase, β, γ and colibacillary RNA polymerase.The powerful pharmacological effect of theoflavin just is being applied to a plurality of fields, has occurred the health care medicine of theoflavin at present, the attached treatment articles that helps of anti-oxidant goods and tumour and AIDS.Along with the research of effect application and going deep into of clinical trial, theoflavin will be applied to more aspect.
Along with the raising of people's living standard, more and more pay attention to healthy.And theoflavin reducing blood-fat, anti-angiocardiopathy, anti-oxidant, effect such as delay senility obviously, the antitumor effect of Denging is arranged again, as the staple product that influences people's quality of life, will more and more be received by people, its market is huge.At present, in great demand to theoflavin on the domestic and international market estimates that the market annual requirement is 2000 tons, and along with the reception in market, demand will further enlarge.
Theoflavin production at present mainly concentrates on China, and the producer of domestic real production theoflavin also seldom, and production technique is very relatively backward, and the method for mainly producing theoflavin has: adopt traditional method from black tea, extracts refining and theoflavin, adopt chemical fermentation method that tea-polyphenol is converted into theoflavin, the traditional resolvase fermentative Production theoflavin of employing.The main drawback of these technology is: 1. technology industrialization poor ability, the theoflavin product content low (theoflavin content is below 20%) that a large amount of indeterminable problems 2. are produced appears in the technology process, of poor quality, demand 3. yields that at all can not satisfy market are low, big 4. production processes of production cost are difficult to use strong acid and strong base in control 5. production processes, and producing a large amount of waste water, environmental pollution is serious.
Summary of the invention
The objective of the invention is the shortcoming that exists in the technology at above-mentioned preparation theoflavin, a kind of novel process for preparing theoflavin is provided, the characteristics of this method are: 1. the PPO enzyme that uses in the tealeaves self, in special environment, active substance tea-polyphenol aerobic fermentation in the tealeaves is become theoflavin, the Product Green environmental protection, steady quality, the high 2. yield height of theoflavin content, do not use strong acid and strong base in low 3. production processes of cost, no processing wastewater produces, thoroughly solved the environmental issue 4. in the production process because the pure ester phase oxidation fermentation that present method adopts, solved traditional ester, water, problem (normal appearance can't be filtered and emulsification problem) that can't three phase separation after the slag mixed phase fermentation, thus can carry out the technology production of stable and controllable.
The technical scheme that realizes above-mentioned purpose is: a kind of novel process for preparing theoflavin, and processing step is as follows:
The preparation of a, fermenation raw liquid: green tea is joined in the extractor, add ethyl acetate then, stir extraction 30min down at 25 ℃～60 ℃, discharging, and then the adding ethyl acetate is extracted once with method again, united extraction liquid, last concentrated extracting solution to solid content is 0.5%～5%, it is standby as fermenation raw liquid to be cooled to room temperature;
The preparation of b, fermenting enzyme: is that 0.1%～1% aqueous citric acid solution is wetting with fresh tea leaf in its with pure water or concentration, through freezing, standby as fermenting enzyme after the pulverization process;
C, fermentation: the fermenation raw liquid in the above-mentioned a step is joined in the fermentation container, add the fermenting enzyme in the b step again, evenly feed gas and stir fermentation, temperature is controlled at 20 ℃～40 ℃, and wherein: the weight ratio of fermenation raw liquid and enzyme is 5～20: 1;
D, separation: the fermented liquid that the c step process is crossed is separated into filtrate and filter residue two portions by filter screen;
E, concentrate: the d step is separated the filtrate that obtains carries out temperature control and concentrate, to solid content be 5%～30%;
F, washing: the concentrated solution in the e step is placed water scrubber, add acidic aqueous solution, mix and wash, leave standstill then, divide the sub-cloud water after the layering, with method washing 1～20 time, wherein, the each acidic aqueous solution that adds and the volume ratio of concentrated solution are 0.1～1: 1, collect ester phase and water after the washing respectively, water gets byproduct behind concentrate drying, ester gives over to standby mutually;
G, change molten: the ester in the f step is added pure water in mutually, wherein the add-on of pure water and ester mutually in the weight ratio of add-on of fermented liquid be 1～1: 25, it is concentrated to carry out temperature control then;
H, filtration: the concentrated solution in the g step is cooled to 30 ℃～60 ℃, filters, collect filtrate;
I, concentrate drying: the filtrate in the above-mentioned h step is further concentrated, and is 15%～80% to containing solid filter, carries out vacuum lyophilization, pulverizes, and obtains qualified theoflavin product after sieving.
As the optimization to such scheme, the weight ratio of green tea and each ethyl acetate that adds is 1: 10～30 in the preparation process of described fermenation raw liquid.To pulverize the back Fresh Folium Camelliae sinensis more than 80 orders at freezing below 0 ℃ and freezing at least 2h in the preparation process of described enzyme.The gas that feeds in the described aerobic fermentation is pure oxygen.Describedly concentrate and change that temperature should be controlled at below 80 ℃ in the molten process.The acidic aqueous solution that adds in the described water-washing step is 0.05%～1% aqueous citric acid solution.Vacuum lyophilization is to freeze into ice cube below-35 ℃ in the described concentrate drying process, vacuum tightness is 0.6～1 mmhg, make moisture vaporization evaporation in the ice cube that the theoflavin concentrated solution freezes, be raised to 0 ℃ with 3 ℃ the speed of per hour heating up then, be raised to 25 ℃～30 ℃ with 5 ℃ speed per hour again, keep 1～2h, make the water content of product reach 3%～5%, remove vacuum state at last.
Take the beneficial effect after the technique scheme as follows:
1. adopt the raw materials for production of green tea, adopt ethyl acetate directly to extract as theoflavin, preparation proferment feed liquid, and organically combine with the biological fermentation of back, thereby farthest reduced production cost.
2. use Fresh Folium Camelliae sinensis as raw material, and the enzyme of preparing by above-mentioned enzyme technology of preparing, as the katalaze enzyme in the biological fermentation (mainly utilize in the tealeaves self PPO enzyme), on the one hand be that the fermenting process gentleness is easy to control, make the theoflavin product content of producing can reach more than 45% on the other hand, quality is good, be again real green product.
3. use pure ester phase oxidation fermentation, solved the problem (normal appearance can't be filtered and emulsification problem) that to carry out three phase separation after ester in traditional resolvase fermentation method, water, the fermentation of slag mixed phase, thereby can be very stable carry out suitability for industrialized production, and product yield and the content produced obviously increase, the generation of having stopped waste water in producing simultaneously.
4. after adopting WATER-WASHING METHOD to carry out purification process, the content of product is greatly improved, and caffeine has obtained removing, keeps away except remove the method for caffeine in the traditional technology with noxious solvent.
5. change the theoflavin aqueous solution after molten, thoroughly separate out through making the insoluble impurity of part after the cooling to a certain degree, again by strainer filtering, thereby make the water-soluble enhancing of theoflavin product of producing, it is bright that color and luster becomes.
6. employing vacuum lyophilization can prevent farthest that theoflavin from the drying process mesometamorphism, obviously improve quality index such as product content, mouthfeel, color and luster.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
The present invention is further detailed explanation below in conjunction with drawings and Examples.
Embodiment 1: as shown in Figure 1, a kind of novel process for preparing theoflavin, processing step is as follows: 100g green tea is joined in the extractor, add the ethyl acetate of 1000mL again, 25～60 ℃ of temperature controls, stir and extract 30min, discharging adds ethyl acetate 1000mL again and extracts once with method again, united extraction liquid, concentrating said extracted liquid to solid content is 1%, and it is standby as fermenation raw liquid to be cooled to room temperature; Select fresh Fresh Folium Camelliae sinensis 120g, raw material as enzyme, is that 0.1% aqueous citric acid solution is wetting with Fresh Folium Camelliae sinensis with pure water or concentration, be placed on below 0 ℃, more than during freezing 2h, pulverize immediately after the taking-up, pulverize and below room temperature, carry out, Fresh Folium Camelliae sinensis after control is pulverized is more than 80 orders, and the enzyme after disposing is as fermenting enzyme standby (storage time must not surpass 2h at normal temperatures); Above-mentioned fermenation raw liquid 1000g is joined in the fermentation container, add the 100g fermenting enzyme again, evenly feed pure oxygen, stir fermentation, temperature is controlled to be 25 ℃ in the fermenting process, stirring velocity 30～150r/min carries out the timing sampling monitoring to fermented liquid, and every 1h sampling once, when question response reaches terminal point, stop logical oxygen immediately, and stop to stir, thus termination reaction; Immediately fermented feed liquid is filtered by 120 mesh filter screens then, collect filtrate respectively, filter residue, filter residue comprehensive treating process; Filtrate is carried out temperature control concentrate, temperature is controlled at below 80 ℃, and being concentrated into solid content is 8%; Concentrated solution (ethyl acetate solution) is placed water scrubber, wash 8 times with 0.1% aqueous citric acid solution of 0.2 times of amount of concentrated solution volume, collect ester phase and water after washing finishes respectively, ester is mutually pending, and water obtains byproduct behind concentrate drying; With the middle mutually water that adds 100mL of above-mentioned ester, further concentrate, the control thickening temperature is below 80 ℃, finishes until the ethyl acetate recovery, collects remaining water; The above-mentioned theoflavin aqueous solution is cooled to 40 ℃, filters, remove insoluble impurities, collect filtrate by 100 mesh filter screens; Above-mentioned filtrate is further concentrated, to solid content be 40%, carry out vacuum lyophilization, freezing into ice cube below-35 ℃, vacuum tightness is 0.6～1 mmhg, make moisture vaporization evaporation in the ice cube that the theoflavin concentrated solution freezes, be raised to 0 ℃ with 3 ℃ the speed of per hour heating up then, be raised to 25 ℃～30 ℃ with 5 ℃ speed per hour again, keep 1～2h, make the water content of product reach 3%～5%, remove vacuum state, pulverize, obtain the theoflavin product of 6.2g after sieving, theoflavin content 46.2% after testing.
Embodiment 2: as shown in Figure 1, a kind of novel process for preparing theoflavin, processing step is as follows: 100g green tea is joined in the extractor, add the ethyl acetate of 1500mL again, 25 ℃～60 ℃ of temperature controls, stir and extract 30min, discharging adds ethyl acetate 1500mL again and extracts once with method again, united extraction liquid, concentrating said extracted liquid to solid content is 0.8%, and it is standby as fermenation raw liquid to be cooled to room temperature; Select fresh Fresh Folium Camelliae sinensis 180g, raw material as enzyme, is that 0.5% aqueous citric acid solution is wetting with Fresh Folium Camelliae sinensis with pure water or concentration, be placed on below 0 ℃, more than during freezing 2h, pulverize immediately after the taking-up, pulverize and below room temperature, carry out, Fresh Folium Camelliae sinensis after control is pulverized is more than 80 orders, and the enzyme after disposing is as fermenting enzyme standby (storage time must not surpass 2h at normal temperatures); Above-mentioned fermenation raw liquid 1500g is joined in the fermentation container, add the 150g fermenting enzyme again, evenly feed pure oxygen, stir fermentation, temperature is controlled to be 20 ℃ in the fermenting process, stirring velocity 30～150r/min carries out the timing sampling monitoring to fermented liquid, and every 1h sampling once, when question response reaches terminal point, stop logical oxygen immediately, and stop to stir, thus termination reaction; Immediately fermented feed liquid is filtered by 120 mesh filter screens then, collect filtrate respectively, filter residue, filter residue comprehensive treating process, filtrate is carried out temperature control to be concentrated, temperature is controlled at below 80 ℃, and being concentrated into solid content is 5%, and concentrated solution (ethyl acetate solution) is placed water scrubber, 0.05% aqueous citric acid solution with 0.1 times of amount of concentrated solution volume is washed 8 times, collect ester phase and water after washing finishes respectively, ester is mutually pending, and water obtains byproduct behind concentrate drying; With the middle mutually water that adds 150mL of above-mentioned ester, further concentrate, the control thickening temperature is below 80 ℃, finishes until the ethyl acetate recovery, collects remaining water; The above-mentioned theoflavin aqueous solution is cooled to 40 ℃, filters, remove insoluble impurities, collect filtrate by 100 mesh filter screens; Above-mentioned filtrate is further concentrated, to solid content be 40%, carry out vacuum lyophilization, freezing into ice cube below-35 ℃, vacuum tightness is 0.6～1 mmhg, make moisture vaporization evaporation in the ice cube that the theoflavin concentrated solution freezes, be raised to 0 ℃ with 3 ℃ the speed of per hour heating up then, be raised to 25 ℃～30 ℃ with 5 ℃ speed per hour again, keep 1～2h, make the water content of product reach 3%～5%, remove vacuum state, pulverize, obtain the theoflavin product of 6.4g after sieving, theoflavin content 45.8% after testing.
Embodiment 3: as shown in Figure 1, a kind of novel process for preparing theoflavin, processing step is as follows: 100g green tea is joined in the extractor, add the ethyl acetate of 3000mL again, 25～60 ℃ of temperature controls, stir and extract 30min, discharging adds ethyl acetate 3000mL again and extracts once with method again, united extraction liquid, concentrating said extracted liquid to solid content is 0.5%, and it is standby as fermenation raw liquid to be cooled to room temperature; Select fresh Fresh Folium Camelliae sinensis 180g, raw material as enzyme, is that 1% aqueous citric acid solution is wetting with Fresh Folium Camelliae sinensis with pure water or concentration, be placed on below 0 ℃, more than during freezing 2h, pulverize immediately after the taking-up, pulverize and below room temperature, carry out, Fresh Folium Camelliae sinensis after control is pulverized is more than 80 orders, and the enzyme after disposing is as fermenting enzyme standby (storage time must not surpass 2h at normal temperatures); Above-mentioned fermenation raw liquid 3000g is joined in the fermentation container, add the 150g fermenting enzyme again, evenly feed pure oxygen, stir fermentation, temperature is controlled to be 40 ℃ in the fermenting process, stirring velocity 30～150r/min carries out the timing sampling monitoring to fermented liquid, and every 1h sampling once, when question response reaches terminal point, stop logical oxygen immediately, and stop to stir, thus termination reaction; Immediately fermented feed liquid is filtered by 120 mesh filter screens then, collect filtrate respectively, filter residue, filter residue comprehensive treating process; Filtrate is carried out temperature control concentrate, temperature is controlled at below 80 ℃, and being concentrated into solid content is 15%; Concentrated solution (ethyl acetate solution) is placed water scrubber, wash 8 times with 1% aqueous citric acid solution of concentrated solution volume equivalent, collect ester phase and water after washing finishes respectively, ester is mutually pending, and water obtains byproduct behind concentrate drying; With the middle mutually water that adds 50mL of above-mentioned ester, further concentrate, the control thickening temperature is below 80 ℃, finishes until the ethyl acetate recovery, collects remaining water; The above-mentioned theoflavin aqueous solution is cooled to 30 ℃, filters, remove insoluble impurities, collect filtrate by 100 mesh filter screens; Above-mentioned filtrate is further concentrated, to solid content be 25%, carry out vacuum lyophilization, freezing into ice cube below-35 ℃, vacuum tightness is 0.6～1 mmhg, make moisture vaporization evaporation in the ice cube that the theoflavin concentrated solution freezes, be raised to 0 ℃ with 3 ℃ the speed of per hour heating up then, be raised to 25 ℃～30 ℃ with 5 ℃ speed per hour again, keep 1～2h, make the water content of product reach 3%～5%, remove vacuum state, pulverize, obtain the theoflavin product of 6.3g after sieving, theoflavin content 46.1% after testing.
Embodiment 4: as shown in Figure 1, a kind of novel process for preparing theoflavin, processing step is as follows: 100g green tea is joined in the extractor, add the ethyl acetate of 1000mL again, 25～60 ℃ of temperature controls, stir and extract 30min, discharging adds ethyl acetate 1000mL again and extracts once with method again, united extraction liquid, concentrating said extracted liquid to solid content is 1%, and it is standby as fermenation raw liquid to be cooled to room temperature; Select fresh Fresh Folium Camelliae sinensis 220g, raw material as enzyme, is that 0.1% aqueous citric acid solution is wetting with Fresh Folium Camelliae sinensis with pure water or concentration, be placed on below 0 ℃, more than during freezing 2h, pulverize immediately after the taking-up, pulverize and below room temperature, carry out, Fresh Folium Camelliae sinensis after control is pulverized is more than 80 orders, and the enzyme after disposing is as fermenting enzyme standby (storage time must not surpass 2h at normal temperatures); Above-mentioned fermenation raw liquid 1000g is joined in the fermentation container, add the 200g fermenting enzyme again, evenly feed pure oxygen, stir fermentation, temperature is controlled to be 25 ℃ in the fermenting process, stirring velocity 30～150r/min carries out the timing sampling monitoring to fermented liquid, and every 1h sampling once, when question response reaches terminal point, stop logical oxygen immediately, and stop to stir, thus termination reaction; Immediately fermented feed liquid is filtered by 120 mesh filter screens then, collect filtrate respectively, filter residue, filter residue comprehensive treating process; Filtrate is carried out temperature control concentrate, temperature is controlled at below 80 ℃, and being concentrated into solid content is 8%; Concentrated solution (ethyl acetate solution) is placed water scrubber, wash 8 times with 0.1% aqueous citric acid solution of 0.2 times of amount of concentrated solution volume, collect ester phase and water after washing finishes respectively, ester is mutually pending, and water obtains byproduct behind concentrate drying; With the middle mutually water that adds 100mL of above-mentioned ester, further concentrate, the control thickening temperature is below 80 ℃, finishes until the ethyl acetate recovery, collects remaining water; The above-mentioned theoflavin aqueous solution is cooled to 60 ℃, filters, remove insoluble impurities, collect filtrate by 100 mesh filter screens; Above-mentioned filtrate is further concentrated, to solid content be 80%, carry out vacuum lyophilization, freezing into ice cube below-35 ℃, vacuum tightness is 0.6～1 mmhg, make moisture vaporization evaporation in the ice cube that the theoflavin concentrated solution freezes, be raised to 0 ℃ with 3 ℃ the speed of per hour heating up then, be raised to 25 ℃～30 ℃ with 5 ℃ speed per hour again, keep 1～2h, make the water content of product reach 3%～5%, remove vacuum state, pulverize, obtain the theoflavin product of 6.2g after sieving, theoflavin content 47.8% after testing.
Embodiment 5: as shown in Figure 1, a kind of novel process for preparing theoflavin, processing step is as follows: 200g green tea is joined in the extractor, add the ethyl acetate of 2000mL again, 25～60 ℃ of temperature controls, stir and extract 30min, discharging adds ethyl acetate 2000mL again and extracts once with method again, united extraction liquid, concentrating said extracted liquid to solid content is 1%, and it is standby as fermenation raw liquid to be cooled to room temperature; Select fresh Fresh Folium Camelliae sinensis 220g, raw material as enzyme, is that 0.1% aqueous citric acid solution is wetting with Fresh Folium Camelliae sinensis with pure water or concentration, be placed on below 0 ℃, more than during freezing 2h, pulverize immediately after the taking-up, pulverize and below room temperature, carry out, Fresh Folium Camelliae sinensis after control is pulverized is more than 80 orders, and the enzyme after disposing is as fermenting enzyme standby (storage time must not surpass 2h at normal temperatures); Above-mentioned fermenation raw liquid 2000g is joined in the fermentation container, add the 200g fermenting enzyme again, evenly feed pure oxygen, stir fermentation, temperature is controlled to be 25 ℃ in the fermenting process, stirring velocity 30～150r/min carries out the timing sampling monitoring to fermented liquid, and every 1h sampling once, when question response reaches terminal point, stop logical oxygen immediately, and stop to stir, thus termination reaction; Immediately fermented feed liquid is filtered by 120 mesh filter screens then, collect filtrate respectively, filter residue, filter residue comprehensive treating process; Filtrate is carried out temperature control concentrate, temperature is controlled at below 80 ℃, and being concentrated into solid content is 8%; Concentrated solution (ethyl acetate solution) is placed water scrubber, wash 20 times with 0.1% aqueous citric acid solution of 0.2 times of amount of concentrated solution volume, collect ester phase and water after washing finishes respectively, ester is mutually pending, and water obtains byproduct behind concentrate drying; With the middle mutually water that adds 100mL of above-mentioned ester, further concentrate, the control thickening temperature is below 80 ℃, finishes until the ethyl acetate recovery, collects remaining water; The above-mentioned theoflavin aqueous solution is cooled to 40 ℃, filters, remove insoluble impurities, collect filtrate by 100 mesh filter screens; Above-mentioned filtrate is further concentrated, to solid content be 40%, carry out vacuum lyophilization, freezing into ice cube below-35 ℃, vacuum tightness is 0.6～1 mmhg, make moisture vaporization evaporation in the ice cube that the theoflavin concentrated solution freezes, be raised to 0 ℃ with 3 ℃ the speed of per hour heating up then, be raised to 25 ℃～30 ℃ with 5 ℃ speed per hour again, keep 1～2h, make the water content of product reach 3%～5%, remove vacuum state, pulverize, obtain the theoflavin product of 13.12g after sieving, theoflavin content 47% after testing.
Embodiment 6: as shown in Figure 1, a kind of novel process for preparing theoflavin, processing step is as follows: 100g green tea is joined in the extractor, add the ethyl acetate of 1000mL again, 25～60 ℃ of temperature controls, stir and extract 30min, discharging adds ethyl acetate 1000mL again and extracts once with method again, united extraction liquid, concentrating said extracted liquid to solid content is 1%, and it is standby as fermenation raw liquid to be cooled to room temperature; Select fresh Fresh Folium Camelliae sinensis 220g, raw material as enzyme, is that 0.1% aqueous citric acid solution is wetting with Fresh Folium Camelliae sinensis with pure water or concentration, be placed on below 0 ℃, more than during freezing 2h, pulverize immediately after the taking-up, pulverize and below room temperature, carry out, Fresh Folium Camelliae sinensis after control is pulverized is more than 80 orders, and the enzyme after disposing is as fermenting enzyme standby (storage time must not surpass 2h at normal temperatures); Above-mentioned fermenation raw liquid 1000g is joined in the fermentation container, add the 200g fermenting enzyme again, evenly feed pure oxygen, stir fermentation, temperature is controlled to be 25 ℃ in the fermenting process, stirring velocity 30～150r/min carries out the timing sampling monitoring to fermented liquid, and every 1h sampling once, when question response reaches terminal point, stop logical oxygen immediately, and stop to stir, thus termination reaction; Immediately fermented feed liquid is filtered by 120 mesh filter screens then, collect filtrate respectively, filter residue, filter residue comprehensive treating process; Filtrate is carried out temperature control concentrate, temperature is controlled at below 80 ℃, and being concentrated into solid content is 8%; Concentrated solution (ethyl acetate solution) is placed water scrubber, wash 1 time with 0.1% aqueous citric acid solution of 0.2 times of amount of concentrated solution volume, collect ester phase and water after washing finishes respectively, ester is mutually pending, and water obtains byproduct behind concentrate drying; With the middle mutually water that adds 100mL of above-mentioned ester, further concentrate, the control thickening temperature is below 80 ℃, finishes until the ethyl acetate recovery, collects remaining water; The above-mentioned theoflavin aqueous solution is cooled to 60 ℃, filters, remove insoluble impurities, collect filtrate by 100 mesh filter screens; Above-mentioned filtrate is further concentrated, to solid content be 50%, carry out vacuum lyophilization, freezing into ice cube below-35 ℃, vacuum tightness is 0.6～1 mmhg, make moisture vaporization evaporation in the ice cube that the theoflavin concentrated solution freezes, be raised to 0 ℃ with 3 ℃ the speed of per hour heating up then, be raised to 25 ℃～30 ℃ with 5 ℃ speed per hour again, keep 1～2h, make the water content of product reach 3%～5%, remove vacuum state, pulverize, obtain the theoflavin product of 6.1g after sieving, theoflavin content 46% after testing.
Theoflavin product sanitary index by prepared of the present invention meets state food additive quality standard fully.The theoflavin quality standard is as follows:
| Project | Standard | Remarks |
| Proterties | Yellowish to reddish-brown powder, puckery | |
| Content % | ≥40.0 | HPLC detects |
| Moisture content % | ≤6.0 | |
| Ash content % | ≤2.0 | |
| Heavy metal ppm | ≤10 | |
| Arsenic ppm | ≤2 | |
| Caffeine % | ≤4 |
Claims (7)
1. novel process for preparing theoflavin is characterized in that processing step is as follows:
The preparation of a, fermenation raw liquid: green tea is joined in the extractor, add ethyl acetate then, stir extraction 30min down at 25 ℃～60 ℃, discharging, and then the adding ethyl acetate is extracted once with method again, united extraction liquid, last concentrated extracting solution to solid content is 0.5%～5%, it is standby as fermenation raw liquid to be cooled to room temperature;
The preparation of b, fermenting enzyme: is that 0.1%～1% aqueous citric acid solution is wetting with fresh tea leaf in its with pure water or concentration, through freezing, standby as fermenting enzyme after the pulverization process;
C, fermentation: the fermenation raw liquid in the above-mentioned a step is joined in the fermentation container, add the fermenting enzyme in the b step again, evenly feed gas and stir fermentation, temperature is controlled at 20 ℃～40 ℃, and wherein: the weight ratio of fermenation raw liquid and enzyme is 5～20: 1;
D, separation: the fermented liquid that the c step process is crossed is separated into filtrate and filter residue two portions by filter screen;
E, concentrate: the d step is separated the filtrate that obtains carries out temperature control and concentrate, to solid content be 5%～30%;
F, washing: the concentrated solution in the e step is placed water scrubber, add acidic aqueous solution, mix and wash, leave standstill then, divide the sub-cloud water after the layering, with method washing 1～20 time, wherein, the each acidic aqueous solution that adds and the volume ratio of concentrated solution are 0.1～1: 1, collect ester phase and water after the washing respectively, water gets byproduct behind concentrate drying, ester gives over to standby mutually;
G, change molten: the ester in the f step is added pure water in mutually, wherein the add-on of pure water and ester mutually in the weight ratio of add-on of fermented liquid be 1～1: 25, it is concentrated to carry out temperature control then;
H, filtration: the concentrated solution in the g step is cooled to 30 ℃～60 ℃, filters, collect filtrate;
I, concentrate drying: the filtrate in the above-mentioned h step is further concentrated, and is 15%～80% to containing solid filter, carries out vacuum lyophilization, pulverizes, and obtains qualified theoflavin product after sieving.
2. a kind of novel process for preparing theoflavin according to claim 1 is characterized in that: the weight ratio of green tea and each ethyl acetate that adds is 1: 10～30 in the preparation process of described fermenation raw liquid.
3. a kind of novel process for preparing theoflavin according to claim 1 is characterized in that: will pulverize the back Fresh Folium Camelliae sinensis more than 80 orders at freezing below 0 ℃ and freezing at least 2h in the preparation process of described enzyme.
4. a kind of novel process for preparing theoflavin according to claim 1 is characterized in that: the gas that feeds in the described fermenting process is pure oxygen.
5. a kind of novel process for preparing theoflavin according to claim 1 is characterized in that: describedly concentrate and change that temperature should be controlled at below 80 ℃ in the molten process.
6. a kind of novel process for preparing theoflavin according to claim 1 is characterized in that: the acidic aqueous solution that adds in the described water-washing step is 0.05%～1% aqueous citric acid solution.
7. a kind of novel process for preparing theoflavin according to claim 1, it is characterized in that: vacuum lyophilization is to freeze into ice cube below-35 ℃ in the described concentrate drying process, vacuum tightness is 0.6～1 mmhg, make moisture vaporization evaporation in the ice cube that the theoflavin concentrated solution freezes, be raised to 0 ℃ with 3 ℃ the speed of per hour heating up then, be raised to 25 ℃～30 ℃ with 5 ℃ speed per hour again, keep 1～2h, make the water content of product reach 3%～5%, remove vacuum state at last.
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