CN110183412A - The method of theaflavin is extracted from black tea - Google Patents

The method of theaflavin is extracted from black tea Download PDF

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Publication number
CN110183412A
CN110183412A CN201910496871.XA CN201910496871A CN110183412A CN 110183412 A CN110183412 A CN 110183412A CN 201910496871 A CN201910496871 A CN 201910496871A CN 110183412 A CN110183412 A CN 110183412A
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China
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black tea
theaflavin
distilled water
mixed liquor
obtains
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CN201910496871.XA
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Inventor
应少明
谢丹华
黄剑华
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Ningde Normal University
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Ningde Normal University
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D311/00Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/58Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
    • C07D311/60Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
    • C07D311/62Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Tea And Coffee (AREA)

Abstract

The method that the present invention provides a kind of from black tea extracts theaflavin, wherein the following steps are included: black tea powder and distilled water are mixed to form mixed liquor, the solid-to-liquid ratio of black tea powder and distilled water is 1:20-1:60;Heating and refluxing extraction is carried out to mixed liquor, reflux temperature is 50 DEG C -100 DEG C, return time 10min-60min, and decompression filters while hot, is cooled to room temperature and obtains filtrate;Different espeleton is added into filtrate or -2 pentanone of 4- methyl is extracted as extractant, obtains the ketone layer containing theaflavin, removal ketone layer obtains theaflavin.

Description

The method of theaflavin is extracted from black tea
Technical field
The present invention relates to a kind of plant extraction process, in particular to a kind of method that theaflavin is extracted from black tea.
Background technique
An important factor for theaflavin is influence black tea quality, and there is multiple pharmacological effect and health-care efficacy, it is main to wrap The effects of including anti-oxidant, cancer-resisting, reducing blood lipid, prevention cardiovascular disease, anti-bacteria and anti-virus.With very big potentiality to be exploited, As people's lives level increasingly improves and environmentally protective theory is rooted in the hearts of the people, people increasingly praise highly green living, tea The pharmacological function of flavine is also more valued by people, and theaflavin is protected as a kind of natural active constituent in food, medicine Strong equal fields have broad application prospects, so the extraction of theaflavin and being prepared into research hot topic in recent years.
Currently, the method for extracting theaflavin from black tea mainly has: (1) Collier method: this method is extracted using hot water Theaflavin is concentrated after removal of impurities, and concentrate is extracted with ethyl acetate, and finally crude product can be obtained in dehydration and drying.This The advantages of method is that extraction process is simple, the disadvantage is that the amount that organic solvent uses is more, operation is comparatively laborious, and extraction yield It is less, from an economic point of view, it is unsuitable for large-scale production.(2) Ullah method: this method uses sodium dihydrogen phosphate and acetic acid second Ester carries out hybrid extraction to extracting solution.Using extracting in boiling water theaflavin, hybrid extraction is carried out after removal of impurities, ester layer after extraction is taken to carry out It is concentrated and dried, theaflavin crude product can be obtained.The method is easy to operate, as long as carrying out 1 extraction, can be very good to extract simultaneously Theaflavin is isolated, but the usage amount of organic solvent is still more, extraction efficiency is also not very high.(3) prepared by enzymatic oxidation Method: promoting the preparation of theaflavin using biological enzyme, and principle is mainly the polyphenol oxidase contained using tealeaves itself.Pass through Select suitable substrate, and the condition of strict control reaction system, the theaflavin of the extractable more amount out of enzymatic oxidation method;But Enzymatic oxidation method is more demanding to the selection of substrate and the control of condition, and reaction is complicated, not easy to control.(4) prepared by chemical oxidation Method: the reaction mechanism that chemical oxidation prepares theaflavin is that theaflavin, chemical oxidation is made using chemical oxidizing agent oxidation catechin Method can be divided into alkaline oxygenated and acidic oxidation again.Chemical oxidization method can eliminate the restriction of various influence factors, make to react into Journey is easily controllable, and controllability is stronger, but due to joined chemical oxidizing agent, preparation and purification process relative to direct extraction method compared with It is complicated.
Summary of the invention
The present invention provides a kind of methods for extracting theaflavin as Extraction solvent using distilled water, can effectively solve State problem.
The present invention is implemented as follows:
A method of extracting theaflavin from black tea, wherein the following steps are included: black tea powder is mixed with distilled water The solid-to-liquid ratio of formation mixed liquor, black tea powder and distilled water is 1:20-1:60;Heating and refluxing extraction, reflux are carried out to mixed liquor Temperature is 50 DEG C -100 DEG C, return time 10min-60min, and decompression filters while hot, is cooled to room temperature and obtains filtrate;To Different espeleton is added in filtrate or -2 pentanone of 4- methyl is extracted as extractant, obtains the ketone layer containing theaflavin, goes Except ketone layer obtains theaflavin.
As further improved, the solid-to-liquid ratio (g:mL) of the black tea powder and distilled water is 1:20-1:40.
As further improved, the reflux temperature is 80 DEG C -100 DEG C.
As further improved, the return time is 20min-40min.
The beneficial effects of the present invention are: feasible and environmentally protective as Extraction solvent raw material economics using water;Using directly extraction Method extracts theaflavin from black tea, and simple process is suitable for large-scale production.
Detailed description of the invention
It, below will be to use required in embodiment in order to illustrate more clearly of the technical solution of embodiment of the present invention Attached drawing be briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not to be seen as It is the restriction to range, it for those of ordinary skill in the art, without creative efforts, can be with root Other relevant attached drawings are obtained according to these attached drawings.
Fig. 1 is the flow chart of the method provided in an embodiment of the present invention that theaflavin is extracted from black tea.
Fig. 2 is the variation schematic diagram of absorbance value provided in an embodiment of the present invention Yu solid-to-liquid ratio parameter.
Fig. 3 is the variation schematic diagram of absorbance value provided in an embodiment of the present invention Yu reflux temperature parameter.
Fig. 4 is the variation schematic diagram of absorbance value provided in an embodiment of the present invention Yu return time parameter.
Specific embodiment
To keep the purposes, technical schemes and advantages of embodiment of the present invention clearer, implement below in conjunction with the present invention The technical solution in embodiment of the present invention is clearly and completely described in attached drawing in mode, it is clear that described reality The mode of applying is some embodiments of the invention, rather than whole embodiments.Based on the embodiment in the present invention, ability Domain those of ordinary skill every other embodiment obtained without creative efforts, belongs to the present invention The range of protection.Therefore, the detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit below and is wanted The scope of the present invention of protection is sought, but is merely representative of selected embodiment of the invention.Based on the embodiment in the present invention, Every other embodiment obtained by those of ordinary skill in the art without making creative efforts belongs to this Invent the range of protection.
In the description of the present invention, term " first ", " second " are used for description purposes only, and should not be understood as instruction or dark Show relative importance or implicitly indicates the quantity of indicated technical characteristic.The feature of " first ", " second " is defined as a result, It can explicitly or implicitly include one or more of the features.In the description of the present invention, the meaning of " plurality " is two It is a or more than two, unless otherwise specifically defined.
Shown in referring to Fig.1, the present invention provides a kind of method that theaflavin is extracted from black tea, comprising the following steps:
Black tea powder and distilled water are mixed to form mixed liquor by S1, and the solid-to-liquid ratio of black tea powder and distilled water is 1:20-1: 60;
S2 carries out heating and refluxing extraction to mixed liquor, and reflux temperature is 50 DEG C -100 DEG C, return time 10min- 60min, and decompression filters while hot, is cooled to room temperature and obtains filtrate;
Different espeleton or -2 pentanone of 4- methyl (IBMK) are added into filtrate and is extracted as extractant, obtains by S3 Ketone layer containing theaflavin, removal ketone layer obtain theaflavin.
In step sl, the black tea powder is carried out after removing tea branch with mortar by drying black tea in an oven Grinding, then the tea-leaf power after grinding is sieved to obtain with sieve.Specifically, the black tea powder is by black tea at 40 DEG C Baking oven in suitably dry, ground after removing tea branch with mortar, then by the sieve of 20 mesh of the tea-leaf power after grinding into Row sieving obtains.The solid-to-liquid ratio (g:mL) of the black tea powder and distilled water is 1:20-1:60.Preferably, the black tea powder Solid-to-liquid ratio (g:mL) with distilled water is 1:20-1:40.In the present embodiment, the solid-to-liquid ratio of the black tea powder and distilled water (g: It mL) is 1:20.
In step s 2, it when carrying out heating and refluxing extraction to mixed liquor, is heated using thermostat water bath.The reflux The range of temperature is 50 DEG C -100 DEG C, it is preferable that the range of the reflux temperature is 80 DEG C -100 DEG C.The return time is 10min-60min, it is preferable that the return time is 20min-40min.In the present embodiment, the reflux temperature is 100 DEG C, The return time is 30min.
In step s3, the method for removing ketone layer is the method for conventional removal ketone layer, is not described in detail herein.
In order to illustrate influence of each preparation parameter to theaflavin content in said extracted method, further using includes to tea The measuring method of flavine content, comprising the following steps: 0.05mol/L is added in the ketone layer into S3 step containing theaflavin AlCl3: dehydrated alcohol (1:2) mixed liquor makes its fully reacting after mixing;It is molten for the mixing of 1:2 with ethyl alcohol volume ratio with IBMK Liquid is reference solution, detects its absorbance with visible spectrophotometer at wavelength 525nm.
The preparation parameter influence extracted in theaflavin method is illustrated below with reference to specific embodiment.Except non-specifically Illustrate, reagent used in following embodiment and material are commercially available.
Experimental raw: the commercially available black tea in Ningde;Distilled water;Experimental drug is as shown in table 1;Laboratory apparatus is as shown in table 2.
1 experimental drug list of table
Nomenclature of drug Purity Producer
Ethyl alcohol AR Sinopharm Chemical Reagent Co., Ltd.
Aluminum trichloride (anhydrous) AR Tianjin Zhi Yuan chemical reagent Co., Ltd
- 2 pentanone of 4- methyl AR Beijing lark prestige Science and Technology Ltd.
2 laboratory apparatus list of table
Instrument title Model Producer
Visible spectrophotometer V-1200 U.S. spectrum in Shanghai reaches Instrument Ltd.
Instrument thermostat water bath Four hole of biserial Establish instrument and meter Co., Ltd in Shanghai
Constant Temp. Oven DHG-9071A The upper macro experimental facilities Co., Ltd of Nereid
Electronic balance YP202N Shanghai Precision Scientific Apparatus Co., Ltd
Multiplex vavuum pump of circulating water type SHZ-D(III) Zhengzhou Boke experimental instruments and equipment limited
Embodiment 1
1. providing the solid-to-liquid ratio parameter of five kinds of different black tea powder and distilled water, i.e. 1:20,1:30,1:40,1:50,1: 60。
2. experiment flow: weigh grind after black tea powder 1.000g, be separately added into 20mL, 30mL, 40mL, 50mL, 60mL distilled water, distillation coolant-temperature gage be 80 DEG C, with thermostat water bath at 80 DEG C refluxing extraction 20 minutes, while hot decompression filter, It is cooled to room temperature;It takes filtrate 5mL in test tube with liquid-transfering gun, IBMK 5mL, concussion layering is added into test tube;It is taken with liquid-transfering gun 0.05mol/L AlCl is added in test tube in the ketone layer solution 2mL on upper layer3: the mixed liquor 6ml of dehydrated alcohol volume ratio 1:2 is mixed Even postposition is sealed with preservative film, and placing 15min makes its fully reacting;Using the mixed solution of IBMK and ethyl alcohol 1:2 as reference solution, Absorbance is detected with visible spectrophotometer at wavelength 525nm, testing result joins table 3 and Fig. 2.Figure it is seen that working as When solid-to-liquid ratio is 1:20, absorbance is maximum.
The influence that theaflavin is extracted when 3 different solid of table is than parameter
Embodiment 2
1. providing six kinds of different reflux temperature parameters, i.e., 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, 100 DEG C.
2. experiment flow: weighing black tea powder 1.000g, the distilled water that 20mL is added extracts, respectively in 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, extract at 100 DEG C 20 minutes, decompression filters while hot, is cooled to room temperature;It takes filtrate 5mL in test tube, is added IBMK 5mL extraction;It takes the ketone layer solution 2mL of extraction in test tube, 0.05mol/L AlCl is added3: dehydrated alcohol volume ratio 1: 2 mixed liquor 6ml makes it react 15min, using the mixed solution of IBMK and ethyl alcohol 1:2 as reference solution, at wavelength 525nm Its absorbance is detected with visible spectrophotometer, testing result joins table 4 and Fig. 3.From figure 3, it can be seen that when reflux temperature is At 100 DEG C, absorbance is maximum.
The influence that 4 reflux temperature of table extracts theaflavin
Embodiment 3
1. providing six kinds of different return time parameters, i.e. 10min, 20min, 30min, 40min, 50min, 60min.
2. experiment flow: weighing black tea powder 1.000g, the distilled water that 20mL is added extracts, and extracts respectively at 80 DEG C 10min, 20min, 30min, 40min, 50min, 60min, decompression filters while hot, is cooled to room temperature;Take filtrate 5mL in test tube In, IBMK 5mL extraction is added;It takes the ketone layer solution 2mL of extraction in test tube, 0.05mol/L AlCl is added3: dehydrated alcohol The mixed liquor 6ml of volume ratio 1:2 makes it react 15min;Using the mixed solution of IBMK and ethyl alcohol 1:2 as reference solution, in wavelength Its absorbance is detected with visible spectrophotometer at 525nm, testing result joins table 5 and Fig. 4.From fig. 4, it can be seen that when reflux When time is 30 minutes, absorbance is maximum.
The influence that 5 return time of table extracts theaflavin
Further, when extracting theaflavin, select solid-to-liquid ratio parameter for 1:20, reflux temperature is 100 DEG C, and return time is When 30min, the absorbance detected is 0.167.
The method provided by the invention for extracting theaflavin from black tea has the advantage that using direct extraction method from black tea Theaflavin is extracted, simple process is suitable for large-scale production;It is feasible and environmentally protective as Extraction solvent raw material economics using water.
The foregoing is merely the preferred embodiment of the present invention, are not intended to restrict the invention, for this field For technical staff, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any Modification, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.

Claims (6)

1. a kind of method for extracting theaflavin from black tea, which comprises the following steps:
Black tea powder and distilled water are mixed to form mixed liquor, the solid-to-liquid ratio of black tea powder and distilled water is 1:20-1:60;
Heating and refluxing extraction is carried out to mixed liquor, reflux temperature is 50 DEG C -100 DEG C, return time 10min-60min, and is taken advantage of Heat decompression filters, and is cooled to room temperature and obtains filtrate;
Different espeleton is added into filtrate or -2 pentanone of 4- methyl is extracted as extractant, obtains the ketone containing theaflavin Layer, removal ketone layer obtain theaflavin.
2. the method according to claim 1 for extracting theaflavin from black tea, which is characterized in that the black tea powder is logical It crosses and dries black tea in an oven, ground after removing tea branch with mortar, then the tea-leaf power after grinding is carried out with sieve Sieving obtains.
3. the method according to claim 1 for extracting theaflavin from black tea, which is characterized in that the black tea powder and steaming The solid-to-liquid ratio (g:mL) of distilled water is 1:20-1:40.
4. the method according to claim 1 for extracting theaflavin from black tea, which is characterized in that heated to mixed liquor It is to be heated using thermostat water bath.
5. the method according to claim 1 for extracting theaflavin from black tea, which is characterized in that the reflux temperature is 80 ℃-100℃。
6. the method according to claim 1 for extracting theaflavin from black tea, which is characterized in that the return time is 20min-40min。
CN201910496871.XA 2019-06-10 2019-06-10 The method of theaflavin is extracted from black tea Pending CN110183412A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111732566A (en) * 2020-08-04 2020-10-02 大湾汉唯(广州)医药科技集团有限公司 Method for extracting theaflavin

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111732566A (en) * 2020-08-04 2020-10-02 大湾汉唯(广州)医药科技集团有限公司 Method for extracting theaflavin
CN111732566B (en) * 2020-08-04 2020-11-27 大湾汉唯(广州)医药科技集团有限公司 Method for extracting theaflavin

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Application publication date: 20190830