CN113548976A - Theanine extraction process - Google Patents
Theanine extraction process Download PDFInfo
- Publication number
- CN113548976A CN113548976A CN202110946294.7A CN202110946294A CN113548976A CN 113548976 A CN113548976 A CN 113548976A CN 202110946294 A CN202110946294 A CN 202110946294A CN 113548976 A CN113548976 A CN 113548976A
- Authority
- CN
- China
- Prior art keywords
- theanine
- extraction process
- supernatant
- later use
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Tea And Coffee (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a theanine extraction process, and belongs to the technical field of extraction processes. It comprises the following steps: (1) collecting fresh Pu' er tea leaves, and naturally drying in the shade for later use; (2) soaking the naturally dried Pu' er tea leaves in warm water to obtain a soaking solution for later use; (3) carrying out centrifugal precipitation treatment on the soak solution for later use; (4) chopping the precipitate after centrifugal precipitation, dissolving with ethyl acetate, filtering, and recovering the supernatant; (5) heating the supernatant after centrifugal precipitation, and cooling after heating to obtain cooled supernatant for later use; (6) mixing the recovered supernatant with the cooled supernatant, and concentrating under reduced pressure to obtain concentrated solution; (7) subjecting the obtained concentrated solution to column treatment, and recovering theanine. The theanine obtained by the extraction process is mainly used in laboratories or small factories, and the purity can meet the requirements.
Description
Technical Field
The invention belongs to the technical field of extraction processes, and particularly relates to a theanine extraction process.
Background
Theanine (L-Theanine) is a free amino acid peculiar to tea leaves, and is glutamic acid gamma-ethylamide, and has sweet taste. Theanine content varies depending on the variety and the site of tea. Theanine accounts for 1-2% of the weight of the dry tea. Theanine is similar to active matters in brain, namely glutamine and glutamic acid in chemical structure, and is a main component for promoting the secretion of body fluid and moistening and sweetening tea. The theanine content is about 1% -2% of the new tea, and the theanine content decreases with the fermentation process. The health-care function of theanine is manifold. Theanine has the basic functions of controlling excessive anxiety, improving learning efficiency, increasing the acuteness of nerves in vivo, improving attention, lowering blood pressure, improving the function of immune system, and the like. As a food additive, theanine is not only easily dissolved in water, but also has the characteristics of suppressing bitterness and improving food flavor. Can be widely used in foods such as snack, candy, jelly, beverage, chewing gum, etc. And after the edible vinegar is added into food, the problems of poor eating and drinking and reduced mouthfeel can be avoided.
Patent CN200310114694.3 discloses a comprehensive preparation process of effective components in tea. The process utilizes a reagent multi-step stepwise extraction method to extract 4 effective components of caffeine, tea polyphenol, tea polysaccharide and theanine from tea according to the physicochemical properties of tea polyphenol, caffeine, tea polysaccharide and theanine. It has the following problems: the three wastes are seriously polluted; large investment in supercritical extraction equipment and the like, and the natural resources cannot be effectively utilized by other single-component extraction methods.
Disclosure of Invention
1. Problems to be solved
Aiming at the problems in the prior art, the invention provides the theanine extraction process which is simple, and particularly, the prepared theanine meets the use requirement.
2. Technical scheme
In order to solve the above problems, the present invention adopts the following technical solutions.
A theanine extraction process comprises the following steps:
(1) collecting fresh Pu' er tea leaves, and naturally drying in the shade for later use;
(2) soaking the Pu' er tea naturally dried in the step (1) in warm water to obtain a soaking solution for later use;
(3) carrying out centrifugal precipitation treatment on the soak solution in the step (2) for later use;
(4) cutting the precipitate obtained after the centrifugal precipitation in the step (3), dissolving the precipitate by using ethyl acetate, and filtering the solution to recover supernatant for later use;
(5) heating the supernatant after centrifugal precipitation in the step (3), and cooling after heating to obtain cooled supernatant for later use;
(6) combining the supernatant recovered in the step (4) and the supernatant cooled in the step (5), and then concentrating under reduced pressure to obtain a concentrated solution;
(7) and (4) carrying out column treatment on the concentrated solution obtained in the step (6) and recovering theanine.
In the theanine extraction process, the tea plant type of the Pu' er tea leaves in the step (1) is Asahm, the product brand is 8582, and the manufacturer is Menghai tea industry, namely the company with limited responsibility.
In the theanine extraction process, the average water content of the naturally aired Pu' er tea leaves in the step (1) is 5%.
In the theanine extraction process, the temperature of the warm water in the step (2) is 46 ℃, and the soaking time is 6 hours;
the medium temperature water in the step (2) contains 20mM Tris.
In the theanine extraction process, the rotation speed of the centrifugal precipitation of the soaking solution in the step (3) is 6000 rpm;
the temperature of the centrifugal precipitation of the soak solution in the step (3) is 8 ℃.
In the above theanine extraction process, the mass ratio of ethyl acetate to precipitate in step (4) is 25: 3;
the temperature for dissolution in step (4) was 45 ℃.
In the theanine extraction process, the heating treatment temperature in the step (5) is 65 ℃;
the heating treatment time in the step (5) is 2 hours;
the temperature after cooling in step (5) was 15 ℃.
In the above theanine extraction process, the parameter conditions of the reduced pressure concentration in the step (6) are as follows:
the pressure reduction pressure is 0.08MPa, and the pressure reduction temperature is 55 ℃.
In the above-mentioned theanine extraction process, the column passing method in the step (7) is as follows:
firstly, treating with polyethylene resin, keeping the column for 45min, and then eluting with deionized water;
then, macroporous cation resin is adopted for processing, the retention time in the column is 30min, and then PBS buffer solution is used for elution;
and finally, carrying out vacuum freeze drying on the collected eluent, and recovering the powdery substance.
In the theanine extraction process, the macroporous cation resin in the step (7) is D113 type macroporous weak acid cation exchange resin.
3. Advantageous effects
Compared with the prior art, the invention has the beneficial effects that:
the theanine obtained by the extraction process is mainly used in laboratories or small factories, and the purity can meet the requirements. Compared with the traditional technology, the method has the advantages that the Pu' er tea is fully utilized, ethyl acetate is arranged for extraction, and the column passing treatment method is optimized, so that the prepared theanine meets the requirements.
Detailed Description
The invention is further described with reference to specific examples.
Example 1
The theanine extraction process of the embodiment comprises the following steps:
(1) collecting fresh Pu' er tea leaves, and naturally drying in the shade for later use;
(2) soaking the Pu' er tea naturally dried in the step (1) in warm water to obtain a soaking solution for later use;
(3) carrying out centrifugal precipitation treatment on the soak solution in the step (2) for later use;
(4) cutting the precipitate obtained after the centrifugal precipitation in the step (3), dissolving the precipitate by using ethyl acetate, and filtering the solution to recover supernatant for later use;
(5) heating the supernatant after centrifugal precipitation in the step (3), and cooling after heating to obtain cooled supernatant for later use;
(6) combining the supernatant recovered in the step (4) and the supernatant cooled in the step (5), and then concentrating under reduced pressure to obtain a concentrated solution;
(7) and (4) carrying out column treatment on the concentrated solution obtained in the step (6) and recovering theanine.
In the theanine extraction process, the tea plant type of the Pu' er tea leaves in the step (1) is Asahm, the product brand is 8582, and the manufacturer is Menghai tea industry, namely the company with limited responsibility.
In the theanine extraction process, the average water content of the naturally aired Pu' er tea leaves in the step (1) is 5%.
In the theanine extraction process, the temperature of the warm water in the step (2) is 46 ℃, and the soaking time is 6 hours;
the medium temperature water in the step (2) contains 20mM Tris.
In the theanine extraction process, the rotation speed of the centrifugal precipitation of the soaking solution in the step (3) is 6000 rpm;
the temperature of the centrifugal precipitation of the soak solution in the step (3) is 8 ℃.
In the above theanine extraction process, the mass ratio of ethyl acetate to precipitate in step (4) is 25: 3;
the temperature for dissolution in step (4) was 45 ℃.
In the theanine extraction process, the heating treatment temperature in the step (5) is 65 ℃;
the heating treatment time in the step (5) is 2 hours;
the temperature after cooling in step (5) was 15 ℃.
In the above theanine extraction process, the parameter conditions of the reduced pressure concentration in the step (6) are as follows:
the pressure reduction pressure is 0.08MPa, and the pressure reduction temperature is 55 ℃.
In the above-mentioned theanine extraction process, the column passing method in the step (7) is as follows:
firstly, treating with polyethylene resin, keeping the column for 45min, and then eluting with deionized water;
then, macroporous cation resin is adopted for processing, the retention time in the column is 30min, and then PBS buffer solution is used for elution;
and finally, carrying out vacuum freeze drying on the collected eluent, and recovering the powdery substance.
In the theanine extraction process, the macroporous cation resin in the step (7) is D113 type macroporous weak acid cation exchange resin.
Comparative example 1
The theanine extraction process of the embodiment comprises the following steps:
(1) collecting fresh Pu' er tea leaves, and naturally drying in the shade for later use;
(2) soaking the Pu' er tea naturally dried in the step (1) in warm water to obtain a soaking solution for later use;
(3) carrying out centrifugal precipitation treatment on the soak solution in the step (2) for later use;
(4) cutting the precipitate obtained after the centrifugal precipitation in the step (3), dissolving the precipitate by using ethyl acetate, and filtering the solution to recover supernatant for later use;
(5) heating the supernatant after centrifugal precipitation in the step (3), and cooling after heating to obtain cooled supernatant for later use;
(6) combining the supernatant recovered in the step (4) and the supernatant cooled in the step (5), and then concentrating under reduced pressure to obtain a concentrated solution;
(7) and (4) carrying out column treatment on the concentrated solution obtained in the step (6) and recovering theanine.
In the theanine extraction process, the tea plant type of the Pu' er tea leaves in the step (1) is Asahm, the product brand is 8582, and the manufacturer is Menghai tea industry, namely the company with limited responsibility.
In the theanine extraction process, the average water content of the naturally aired Pu' er tea leaves in the step (1) is 5%.
In the theanine extraction process, the temperature of the warm water in the step (2) is 46 ℃, and the soaking time is 6 hours;
the medium temperature water in the step (2) contains 20mM Tris.
In the theanine extraction process, the rotation speed of the centrifugal precipitation of the soaking solution in the step (3) is 6000 rpm;
the temperature of the centrifugal precipitation of the soak solution in the step (3) is 8 ℃.
In the above theanine extraction process, the mass ratio of ethyl acetate to precipitate in step (4) is 25: 1;
the temperature for dissolution in step (4) was 45 ℃.
In the theanine extraction process, the heating treatment temperature in the step (5) is 65 ℃;
the heating treatment time in the step (5) is 2 hours;
the temperature after cooling in step (5) was 15 ℃.
In the above theanine extraction process, the parameter conditions of the reduced pressure concentration in the step (6) are as follows:
the pressure reduction pressure is 0.08MPa, and the pressure reduction temperature is 55 ℃.
In the above-mentioned theanine extraction process, the column passing method in the step (7) is as follows:
firstly, treating with polyethylene resin, keeping the column for 45min, and then eluting with deionized water;
then, macroporous cation resin is adopted for processing, the retention time in the column is 30min, and then PBS buffer solution is used for elution;
and finally, carrying out vacuum freeze drying on the collected eluent, and recovering the powdery substance.
In the theanine extraction process, the macroporous cation resin in the step (7) is D113 type macroporous weak acid cation exchange resin.
Comparative example 2
The theanine extraction process of the embodiment comprises the following steps:
(1) collecting fresh Pu' er tea leaves, and naturally drying in the shade for later use;
(2) soaking the Pu' er tea naturally dried in the step (1) in warm water to obtain a soaking solution for later use;
(3) carrying out centrifugal precipitation treatment on the soak solution in the step (2) for later use;
(4) cutting the precipitate obtained after the centrifugal precipitation in the step (3), dissolving the precipitate by using ethyl acetate, and filtering the solution to recover supernatant for later use;
(5) heating the supernatant after centrifugal precipitation in the step (3), and cooling after heating to obtain cooled supernatant for later use;
(6) combining the supernatant recovered in the step (4) and the supernatant cooled in the step (5), and then concentrating under reduced pressure to obtain a concentrated solution;
(7) and (4) carrying out column treatment on the concentrated solution obtained in the step (6) and recovering theanine.
In the theanine extraction process, the tea plant type of the Pu' er tea leaves in the step (1) is Asahm, the product brand is 8582, and the manufacturer is Menghai tea industry, namely the company with limited responsibility.
In the theanine extraction process, the average water content of the naturally aired Pu' er tea leaves in the step (1) is 5%.
In the theanine extraction process, the temperature of the warm water in the step (2) is 46 ℃, and the soaking time is 6 hours;
the medium temperature water in the step (2) contains 20mM Tris.
In the theanine extraction process, the rotation speed of the centrifugal precipitation of the soaking solution in the step (3) is 6000 rpm;
the temperature of the centrifugal precipitation of the soak solution in the step (3) is 8 ℃.
In the above theanine extraction process, the mass ratio of ethyl acetate to precipitate in step (4) is 25: 5;
the temperature for dissolution in step (4) was 45 ℃.
In the theanine extraction process, the heating treatment temperature in the step (5) is 65 ℃;
the heating treatment time in the step (5) is 2 hours;
the temperature after cooling in step (5) was 15 ℃.
In the above theanine extraction process, the parameter conditions of the reduced pressure concentration in the step (6) are as follows:
the pressure reduction pressure is 0.08MPa, and the pressure reduction temperature is 55 ℃.
In the above-mentioned theanine extraction process, the column passing method in the step (7) is as follows:
firstly, treating with polyethylene resin, keeping the column for 45min, and then eluting with deionized water;
then, macroporous cation resin is adopted for processing, the retention time in the column is 30min, and then PBS buffer solution is used for elution;
and finally, carrying out vacuum freeze drying on the collected eluent, and recovering the powdery substance.
In the theanine extraction process, the macroporous cation resin in the step (7) is D113 type macroporous weak acid cation exchange resin.
Comparative example 3
The theanine extraction process of the embodiment comprises the following steps:
(1) collecting fresh Pu' er tea leaves, and naturally drying in the shade for later use;
(2) soaking the Pu' er tea naturally dried in the step (1) in warm water to obtain a soaking solution for later use;
(3) carrying out centrifugal precipitation treatment on the soak solution in the step (2) for later use;
(4) cutting the precipitate obtained after the centrifugal precipitation in the step (3), dissolving the precipitate by using ethyl acetate, and filtering the solution to recover supernatant for later use;
(5) heating the supernatant after centrifugal precipitation in the step (3), and cooling after heating to obtain cooled supernatant for later use;
(6) combining the supernatant recovered in the step (4) and the supernatant cooled in the step (5), and then concentrating under reduced pressure to obtain a concentrated solution;
(7) and (4) carrying out column treatment on the concentrated solution obtained in the step (6) and recovering theanine.
In the theanine extraction process, the tea plant type of the Pu' er tea leaves in the step (1) is Asahm, the product brand is 8582, and the manufacturer is Menghai tea industry, namely the company with limited responsibility.
In the theanine extraction process, the average water content of the naturally aired Pu' er tea leaves in the step (1) is 5%.
In the theanine extraction process, the temperature of the warm water in the step (2) is 46 ℃, and the soaking time is 6 hours;
in the step (2), the medium temperature water contains 20mM PBS buffer solution.
In the theanine extraction process, the rotation speed of the centrifugal precipitation of the soaking solution in the step (3) is 6000 rpm;
the temperature of the centrifugal precipitation of the soak solution in the step (3) is 8 ℃.
In the above theanine extraction process, the mass ratio of ethyl acetate to precipitate in step (4) is 25: 3;
the temperature for dissolution in step (4) was 45 ℃.
In the theanine extraction process, the heating treatment temperature in the step (5) is 65 ℃;
the heating treatment time in the step (5) is 2 hours;
the temperature after cooling in step (5) was 15 ℃.
In the above theanine extraction process, the parameter conditions of the reduced pressure concentration in the step (6) are as follows:
the pressure reduction pressure is 0.08MPa, and the pressure reduction temperature is 55 ℃.
In the above-mentioned theanine extraction process, the column passing method in the step (7) is as follows:
firstly, treating with polyethylene resin, keeping the column for 45min, and then eluting with deionized water;
then, macroporous cation resin is adopted for processing, the retention time in the column is 30min, and then PBS buffer solution is used for elution;
and finally, carrying out vacuum freeze drying on the collected eluent, and recovering the powdery substance.
In the theanine extraction process, the macroporous cation resin in the step (7) is D113 type macroporous weak acid cation exchange resin.
Comparative example 4
The theanine extraction process of the embodiment comprises the following steps:
(1) collecting fresh Pu' er tea leaves, and naturally drying in the shade for later use;
(2) soaking the Pu' er tea naturally dried in the step (1) in warm water to obtain a soaking solution for later use;
(3) carrying out centrifugal precipitation treatment on the soak solution in the step (2) for later use;
(4) cutting the precipitate obtained after the centrifugal precipitation in the step (3), dissolving the precipitate by using ethyl acetate, and filtering the solution to recover supernatant for later use;
(5) heating the supernatant after centrifugal precipitation in the step (3), and cooling after heating to obtain cooled supernatant for later use;
(6) combining the supernatant recovered in the step (4) and the supernatant cooled in the step (5), and then concentrating under reduced pressure to obtain a concentrated solution;
(7) and (4) carrying out column treatment on the concentrated solution obtained in the step (6) and recovering theanine.
In the theanine extraction process, the tea plant type of the Pu' er tea leaves in the step (1) is Asahm, the product brand is 8582, and the manufacturer is Menghai tea industry, namely the company with limited responsibility.
In the theanine extraction process, the average water content of the naturally aired Pu' er tea leaves in the step (1) is 5%.
In the theanine extraction process, the temperature of the warm water in the step (2) is 46 ℃, and the soaking time is 6 hours;
the medium temperature water in the step (2) contains 20mM Tris.
In the theanine extraction process, the rotation speed of the centrifugal precipitation of the soaking solution in the step (3) is 6000 rpm;
the temperature of the centrifugal precipitation of the soak solution in the step (3) is 8 ℃.
In the above theanine extraction process, the mass ratio of ethyl acetate to precipitate in step (4) is 25: 3;
the temperature for dissolution in step (4) was 45 ℃.
In the theanine extraction process, the heating treatment temperature in the step (5) is 65 ℃;
the heating treatment time in the step (5) is 2 hours;
the temperature after cooling in step (5) was 15 ℃.
In the above theanine extraction process, the parameter conditions of the reduced pressure concentration in the step (6) are as follows:
the pressure reduction pressure is 0.08MPa, and the pressure reduction temperature is 55 ℃.
In the above-mentioned theanine extraction process, the column passing method in the step (7) is as follows:
firstly, treating with polyethylene resin, keeping the column for 45min, and then eluting with deionized water;
then, macroporous cation resin is adopted for processing, the retention time in the column is 30min, and then PBS buffer solution is used for elution;
and finally, carrying out vacuum freeze drying on the collected eluent, and recovering the powdery substance.
In the theanine extraction process, the macroporous cation resin in the step (7) is D113 type macroporous weak acid cation exchange resin.
Comparative example 5
The theanine extraction process of the embodiment comprises the following steps:
(1) collecting fresh Pu' er tea leaves, and naturally drying in the shade for later use;
(2) soaking the Pu' er tea naturally dried in the step (1) in warm water to obtain a soaking solution for later use;
(3) carrying out centrifugal precipitation treatment on the soak solution in the step (2) for later use;
(4) cutting the precipitate obtained after the centrifugal precipitation in the step (3), dissolving the precipitate by using ethyl acetate, and filtering the solution to recover supernatant for later use;
(5) heating the supernatant after centrifugal precipitation in the step (3), and cooling after heating to obtain cooled supernatant for later use;
(6) combining the supernatant recovered in the step (4) and the supernatant cooled in the step (5), and then concentrating under reduced pressure to obtain a concentrated solution;
(7) and (4) carrying out column treatment on the concentrated solution obtained in the step (6) and recovering theanine.
In the theanine extraction process, the tea plant type of the Pu' er tea leaves in the step (1) is Asahm, the product brand is 8582, and the manufacturer is Menghai tea industry, namely the company with limited responsibility.
In the theanine extraction process, the average water content of the naturally aired Pu' er tea leaves in the step (1) is 5%.
In the theanine extraction process, the temperature of the warm water in the step (2) is 46 ℃, and the soaking time is 6 hours;
the medium temperature water in the step (2) contains 20mM Tris.
In the theanine extraction process, the rotation speed of the centrifugal precipitation of the soaking solution in the step (3) is 6000 rpm;
the temperature of the centrifugal precipitation of the soak solution in the step (3) is 8 ℃.
In the above theanine extraction process, the mass ratio of ethyl acetate to precipitate in step (4) is 25: 3;
the temperature for dissolution in step (4) was 45 ℃.
In the theanine extraction process, the heating treatment temperature in the step (5) is 65 ℃;
the heating treatment time in the step (5) is 2 hours;
the temperature after cooling in step (5) was 15 ℃.
In the above theanine extraction process, the parameter conditions of the reduced pressure concentration in the step (6) are as follows:
the pressure reduction pressure is 0.08MPa, and the pressure reduction temperature is 55 ℃.
In the above-mentioned theanine extraction process, the column passing method in the step (7) is as follows:
firstly, treating with polyethylene resin, keeping the column for 25min, and then eluting with deionized water;
then, macroporous cation resin is adopted for processing, the retention time in the column is 10min, and then PBS buffer solution is used for elution;
and finally, carrying out vacuum freeze drying on the collected eluent, and recovering the powdery substance.
In the theanine extraction process, the macroporous cation resin in the step (7) is D113 type macroporous weak acid cation exchange resin.
Comparative example 6
The theanine extraction process of the embodiment comprises the following steps:
(1) collecting fresh Pu' er tea leaves, and naturally drying in the shade for later use;
(2) soaking the Pu' er tea naturally dried in the step (1) in warm water to obtain a soaking solution for later use;
(3) carrying out centrifugal precipitation treatment on the soak solution in the step (2) for later use;
(4) cutting the precipitate obtained after the centrifugal precipitation in the step (3), dissolving the precipitate by using ethyl acetate, and filtering the solution to recover supernatant for later use;
(5) heating the supernatant after centrifugal precipitation in the step (3), and cooling after heating to obtain cooled supernatant for later use;
(6) combining the supernatant recovered in the step (4) and the supernatant cooled in the step (5), and then concentrating under reduced pressure to obtain a concentrated solution;
(7) and (4) carrying out column treatment on the concentrated solution obtained in the step (6) and recovering theanine.
In the theanine extraction process, the tea plant type of the Pu' er tea leaves in the step (1) is Asahm, the product brand is 8582, and the manufacturer is Menghai tea industry, namely the company with limited responsibility.
In the theanine extraction process, the average water content of the naturally aired Pu' er tea leaves in the step (1) is 5%.
In the theanine extraction process, the temperature of the warm water in the step (2) is 46 ℃, and the soaking time is 6 hours;
the medium temperature water in the step (2) contains 20mM Tris.
In the theanine extraction process, the rotation speed of the centrifugal precipitation of the soaking solution in the step (3) is 6000 rpm;
the temperature of the centrifugal precipitation of the soak solution in the step (3) is 8 ℃.
In the above theanine extraction process, the mass ratio of ethyl acetate to precipitate in step (4) is 25: 3;
the temperature for dissolution in step (4) was 45 ℃.
In the theanine extraction process, the heating treatment temperature in the step (5) is 65 ℃;
the heating treatment time in the step (5) is 2 hours;
the temperature after cooling in step (5) was 15 ℃.
In the above theanine extraction process, the parameter conditions of the reduced pressure concentration in the step (6) are as follows:
the pressure reduction pressure is 0.08MPa, and the pressure reduction temperature is 55 ℃.
In the above-mentioned theanine extraction process, the column passing method in the step (7) is as follows:
firstly, treating with polyethylene resin, keeping the column for 45min, and then eluting with deionized water;
and finally, carrying out vacuum freeze drying on the collected eluent, and recovering the powdery substance.
In the theanine extraction process, the macroporous cation resin in the step (7) is D113 type macroporous weak acid cation exchange resin.
Comparative example 7
The theanine extraction process of the embodiment comprises the following steps:
(1) collecting fresh Pu' er tea leaves, and naturally drying in the shade for later use;
(2) soaking the Pu' er tea naturally dried in the step (1) in warm water to obtain a soaking solution for later use;
(3) carrying out centrifugal precipitation treatment on the soak solution in the step (2) for later use;
(4) cutting the precipitate obtained after the centrifugal precipitation in the step (3), dissolving the precipitate by using ethyl acetate, and filtering the solution to recover supernatant for later use;
(5) heating the supernatant after centrifugal precipitation in the step (3), and cooling after heating to obtain cooled supernatant for later use;
(6) combining the supernatant recovered in the step (4) and the supernatant cooled in the step (5), and then concentrating under reduced pressure to obtain a concentrated solution;
(7) and (4) carrying out column treatment on the concentrated solution obtained in the step (6) and recovering theanine.
In the theanine extraction process, the tea plant type of the Pu' er tea leaves in the step (1) is Asahm, the product brand is 8582, and the manufacturer is Menghai tea industry, namely the company with limited responsibility.
In the theanine extraction process, the average water content of the naturally aired Pu' er tea leaves in the step (1) is 5%.
In the theanine extraction process, the temperature of the warm water in the step (2) is 46 ℃, and the soaking time is 6 hours;
the medium temperature water in the step (2) contains 20mM Tris.
In the theanine extraction process, the rotation speed of the centrifugal precipitation of the soaking solution in the step (3) is 6000 rpm;
the temperature of the centrifugal precipitation of the soak solution in the step (3) is 8 ℃.
In the above theanine extraction process, the mass ratio of ethyl acetate to precipitate in step (4) is 25: 3;
the temperature for dissolution in step (4) was 45 ℃.
In the theanine extraction process, the heating treatment temperature in the step (5) is 65 ℃;
the heating treatment time in the step (5) is 2 hours;
the temperature after cooling in step (5) was 15 ℃.
In the above theanine extraction process, the parameter conditions of the reduced pressure concentration in the step (6) are as follows:
the pressure reduction pressure is 0.08MPa, and the pressure reduction temperature is 55 ℃.
In the above-mentioned theanine extraction process, the column passing method in the step (7) is as follows:
firstly, processing by adopting macroporous cation resin, keeping the retention time in a column for 30min, and then eluting by using PBS buffer solution;
and finally, carrying out vacuum freeze drying on the collected eluent, and recovering the powdery substance.
In the theanine extraction process, the macroporous cation resin in the step (7) is D113 type macroporous weak acid cation exchange resin.
Comparative example 8
The theanine extraction process of the embodiment comprises the following steps:
(1) collecting fresh Pu' er tea leaves, and naturally drying in the shade for later use;
(2) soaking the Pu' er tea naturally dried in the step (1) in warm water to obtain a soaking solution for later use;
(3) carrying out centrifugal precipitation treatment on the soak solution in the step (2) for later use;
(4) cutting the precipitate obtained after the centrifugal precipitation in the step (3), dissolving the precipitate by using ethyl acetate, and filtering the solution to recover supernatant for later use;
(5) heating the supernatant after centrifugal precipitation in the step (3), and cooling after heating to obtain cooled supernatant for later use;
(6) combining the supernatant recovered in the step (4) and the supernatant cooled in the step (5), and then concentrating under reduced pressure to obtain a concentrated solution;
(7) and (4) carrying out column treatment on the concentrated solution obtained in the step (6) and recovering theanine.
In the theanine extraction process, the tea plant type of the Pu' er tea leaves in the step (1) is Asahm, the product brand is 8582, and the manufacturer is Menghai tea industry, namely the company with limited responsibility.
In the theanine extraction process, the average water content of the naturally aired Pu' er tea leaves in the step (1) is 5%.
In the theanine extraction process, the temperature of the warm water in the step (2) is 46 ℃, and the soaking time is 6 hours;
the medium temperature water in the step (2) contains 20mM Tris.
In the theanine extraction process, the rotation speed of the centrifugal precipitation of the soaking solution in the step (3) is 6000 rpm;
the temperature of the centrifugal precipitation of the soak solution in the step (3) is 8 ℃.
In the above theanine extraction process, the mass ratio of ethyl acetate to precipitate in step (4) is 25: 3;
the temperature for dissolution in step (4) was 45 ℃.
In the theanine extraction process, the heating treatment temperature in the step (5) is 65 ℃;
the heating treatment time in the step (5) is 2 hours;
the temperature after cooling in step (5) was 15 ℃.
In the above theanine extraction process, the parameter conditions of the reduced pressure concentration in the step (6) are as follows:
the pressure reduction pressure is 0.08MPa, and the pressure reduction temperature is 45 ℃.
In the above-mentioned theanine extraction process, the column passing method in the step (7) is as follows:
firstly, treating with polyethylene resin, keeping the column for 45min, and then eluting with deionized water;
then, macroporous cation resin is adopted for processing, the retention time in the column is 30min, and then PBS buffer solution is used for elution;
and finally, carrying out vacuum freeze drying on the collected eluent, and recovering the powdery substance.
In the theanine extraction process, the macroporous cation resin in the step (7) is D113 type macroporous weak acid cation exchange resin.
Example 2
The product prepared in example 1 and the products prepared in comparative examples 1 to 8 were selected and subjected to the following tests:
the measurement is carried out by referring to QB/T4263-2011L-theanine; it needs to be reminded that in the prior art, the purity of theanine can be improved in various ways, but an ultrafiltration membrane or chromatographic separation mode is adopted, so that the production cost is high, and continuous processing is difficult.
Wherein the purity of theanine prepared in example 1 was 92.0%;
wherein the purity of theanine prepared in comparative example 1 was 90.1%;
wherein the purity of theanine prepared in comparative example 2 was 89.7%;
wherein the purity of theanine prepared in comparative example 3 was 91.4%;
wherein the purity of theanine prepared in comparative example 4 was 90.8%;
wherein the purity of theanine prepared in comparative example 5 was 80.5%;
wherein the purity of theanine prepared in comparative example 6 was 78.4%;
wherein the purity of theanine prepared in comparative example 7 was 74.1%;
wherein the purity of theanine prepared in comparative example 8 was 91.6%.
While the invention has been described in further detail in connection with specific embodiments thereof, it will be understood that the invention is not limited thereto, and that various other modifications and substitutions may be made by those skilled in the art without departing from the spirit of the invention, which should be considered to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A theanine extraction process comprises the following steps:
(1) collecting fresh Pu' er tea leaves, and naturally drying in the shade for later use;
(2) soaking the Pu' er tea naturally dried in the step (1) in warm water to obtain a soaking solution for later use;
(3) carrying out centrifugal precipitation treatment on the soak solution in the step (2) for later use;
(4) cutting the precipitate obtained after the centrifugal precipitation in the step (3), dissolving the precipitate by using ethyl acetate, and filtering the solution to recover supernatant for later use;
(5) heating the supernatant after centrifugal precipitation in the step (3), and cooling after heating to obtain cooled supernatant for later use;
(6) combining the supernatant recovered in the step (4) and the supernatant cooled in the step (5), and then concentrating under reduced pressure to obtain a concentrated solution;
(7) and (4) carrying out column treatment on the concentrated solution obtained in the step (6) and recovering theanine.
2. The theanine extraction process as set forth in claim 1, wherein:
the tea plant type of the Pu' er tea in the step (1) is Asahm, the brand model of the product is 8582, and the manufacturer is Menghai tea industry, namely a company with limited responsibility.
3. The theanine extraction process as set forth in claim 1, wherein:
the average water content of the Pu' er tea naturally dried in the step (1) is 5%.
4. The theanine extraction process as set forth in claim 1, wherein:
in the step (2), the temperature of the warm water is 46 ℃, and the soaking time is 6 hours;
the medium temperature water in the step (2) contains 20mM Tris.
5. The theanine extraction process as set forth in claim 1, wherein:
the rotating speed of the centrifugal precipitation of the soaking solution in the step (3) is 6000 rpm;
the temperature of the centrifugal precipitation of the soak solution in the step (3) is 8 ℃.
6. The theanine extraction process as set forth in claim 1, wherein:
the mass ratio of the ethyl acetate to the precipitate in the step (4) is 25: 3;
the temperature for dissolution in step (4) was 45 ℃.
7. The theanine extraction process as set forth in claim 1, wherein:
the temperature of the heating treatment in the step (5) is 65 ℃;
the heating treatment time in the step (5) is 2 hours;
the temperature after cooling in step (5) was 15 ℃.
8. The theanine extraction process as set forth in claim 1, wherein:
the parameter conditions of the reduced pressure concentration in the step (6) are as follows:
the pressure reduction pressure is 0.08MPa, and the pressure reduction temperature is 55 ℃.
9. The theanine extraction process as set forth in claim 1, wherein:
the column passing treatment in the step (7) is as follows:
firstly, treating with polyethylene resin, keeping the column for 45min, and then eluting with deionized water;
then, macroporous cation resin is adopted for processing, the retention time in the column is 30min, and then PBS buffer solution is used for elution;
and finally, carrying out vacuum freeze drying on the collected eluent, and recovering the powdery substance.
10. The theanine extraction process of claim 9, wherein:
and (4) the macroporous cation resin in the step (7) is D113 type macroporous weak-acidic cation exchange resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110946294.7A CN113548976A (en) | 2021-08-18 | 2021-08-18 | Theanine extraction process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110946294.7A CN113548976A (en) | 2021-08-18 | 2021-08-18 | Theanine extraction process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113548976A true CN113548976A (en) | 2021-10-26 |
Family
ID=78133963
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110946294.7A Withdrawn CN113548976A (en) | 2021-08-18 | 2021-08-18 | Theanine extraction process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113548976A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114960218A (en) * | 2022-06-30 | 2022-08-30 | 常州美胜生物材料有限公司 | Theanine fabric and preparation method thereof |
-
2021
- 2021-08-18 CN CN202110946294.7A patent/CN113548976A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114960218A (en) * | 2022-06-30 | 2022-08-30 | 常州美胜生物材料有限公司 | Theanine fabric and preparation method thereof |
| CN114960218B (en) * | 2022-06-30 | 2024-03-15 | 常州美胜生物材料有限公司 | Theanine fabric and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106822196B (en) | Method for simultaneously extracting ginkgo leaf polysaccharide and ginkgo leaf flavone from ginkgo leaves | |
| CN111296708A (en) | Method for producing fructus momordicae extract by adopting immobilized enzyme technology | |
| CN105053952B (en) | A kind of processing technology of the dried orange peel extracts of no bitter taste | |
| CN103462133A (en) | Fructose roxburgh rose juice beverage and production method thereof | |
| CN107188911B (en) | Method for extracting soybean oligosaccharide and soybean isoflavone by using soybean molasses | |
| CN112616966A (en) | Preparation method of strong-flavor instant tea and product thereof | |
| CN113548976A (en) | Theanine extraction process | |
| CN109457008B (en) | Preparation method of ginseng chelating peptide | |
| CN109757600B (en) | Preparation method of perilla peptide | |
| CN102613352B (en) | Method for preparing high gamma-amino butyric acid instant tea powder | |
| CN1128151C (en) | Method for extracting soy bean oligosaccharide from soy bean whey water | |
| CN103980335A (en) | Mogroside V preparation method | |
| CN102127128A (en) | New process for extracting stevioside by utilizing enzyme coupling membrane separation technology | |
| CN205409475U (en) | Solid sugarcane juice processingequipment is strained to multistage mixed membrane | |
| CN115581266B (en) | Clean production method of momordica grosvenori dry powder and momordica grosvenori concentrated juice | |
| CN101597635B (en) | Method for preparing high purity stachyose | |
| CN114539330B (en) | Extraction method and application of mogroside | |
| CN103965153B (en) | Utilize rutin to prepare the method for Quercetin and rhamnose | |
| CN112442136A (en) | Method for extracting functional components from tremella | |
| CN111377898A (en) | Preparation process of cranberry extract procyanidine | |
| CN115176845A (en) | Fermentation preparation process of phycocyanin coconut-flavor sucrose-free yoghurt powder | |
| CN86105966A (en) | The method of extracting pectin from beencard firewood leaves | |
| CN107467283B (en) | Method for regulating and controlling tea juice taste quality | |
| CN110669095B (en) | Extraction method of high-purity mogroside V | |
| CN115124585B (en) | Clean production method of momordica grosvenori extract |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20211026 |