Resin adsorption synthesis technology for extracting tea polyphenols from discarded fresh tea leaves

A technology of resin adsorption and fresh tea leaves, which is applied in the direction of drug combination, medical preparations containing active ingredients, antidote, etc., can solve the problem of low extraction efficiency, strict technical requirements for separation and purification of tea polyphenols, incomplete extraction of tea polyphenols, etc. problem to achieve efficient extraction

Active Publication Date: 2018-01-23

雅安市云茶供应链管理有限公司

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AI-Extracted Technical Summary

Problems solved by technology

However, only relying on one extraction method can easily lead to low extraction efficiency, incomplete extraction of tea polyphenols, or more residues and impurities, especially for the technology of extracting...

Abstract

The invention discloses a resign adsorption synthesis technology for extracting tea polyphenols from discarded fresh tea leaves. Extraction of the tea polyphenols is performed by combining solvent purification with a resin adsorption technique, processes of impurity removal, resin extracting, solvent cleaning, low-temperature static impurity removing and the like are performed via coarse separation of slag, using of more than 95% of chloroform and 5% or less than 5% of a petroleum ether mixture, impurities are removed maximumly finally, effective content and purity of the tea polyphenols are effectively increased, and the effect of low residues of harmful solvents is achieved.

Application Domain

Antinoxious agentsDermatological disorder +1

Technology Topic

SlagSolvent +5

Image

Examples

Experimental program(3)
Effect test(1)

Example Embodiment

[0039] Example 1:

[0040] A comprehensive resin adsorption technology for extracting tea polyphenols from waste fresh tea leaves, including the following steps:

[0041] (1) Rough separation of impurities:

[0042] A1: Use a tea washing machine to clean the discarded fresh tea leaves, and then heat the tea leaves to 280°C by microwave and keep them for 3 minutes to kill enzymes;

[0043] A2: Extract discarded fresh tea leaves in boiling water, use a dumb jaw crusher to crush, cut and crush the tea leaves to 110-120 meshes, filter, repeat more than twice, and combine the filtrate;

[0044] A3: Use a mixture of 95% chloroform and 5% petroleum ether to extract the filtrate, separate the layers, remove the chloroform petroleum ether extraction layer, and retain the aqueous layer;

[0045] A4: Repeat step A3 twice to combine the aqueous solution layers;

[0046] A5: Maintain the temperature of 35~40℃ to stir and evaporate the aqueous solution layer under negative pressure;

[0047] (2) Resin extraction: Circulate the liquid obtained in step A5 twice through the macroporous adsorption resin for adsorption. The macroporous adsorption resin is AB-8 macroporous adsorption resin with a pore size of 60~90nm and a porosity of 25%~40%. The temperature of the system is 16~20℃, and the flow rate is 3.8~4.0BV/h;

[0048] (3) Elution: Use an ethanol solution with a concentration of 10%-95% to elute the resin from a low concentration to a high concentration to obtain an eluate;

[0049] (4) Place the eluent in a 35~40℃ water bath to evaporate the solvent;

[0050] (5) Use a mixture of 85% chloroform and 15% petroleum ether to extract and remove impurities from the solution in step (4). During this time, shake the mixture, and then let it stand for more than 10 minutes, separating the solution, and retaining the aqueous layer. The chloroform and petroleum in this step The amount of ether does not need to be too large, it needs to be determined based on sampling and determination of impurity content;

[0051] (6) Repeat step (5) twice or more to combine the aqueous solution layers;

[0052] (7) Maintain the temperature of 35~45℃ to stir and evaporate the aqueous solution layer under negative pressure;

[0053] (8) Maintain the temperature of 60~65℃ to stir and evaporate the aqueous layer under negative pressure. The maintenance time is based on the following formula: T=Hm/2S, where T: time (h), H: solution height (m), m: solution Mass (kg), S: solution surface area (m 2 );

[0054] (9) Standing: After the temperature of the solution obtained in step (8) naturally drops to room temperature, place it in an environment of 4 to 6°C and stand for more than 1 hour;

[0055] (10) Filtration: filter the solid-liquid mixture obtained in step (9), recycle the filter residue, and take the filtrate;

[0056] (11) The filtrate obtained in step (10) is adsorbed on activated carbon, the mesh of which is 230-250 mesh;

[0057] (12) Concentration: vacuum the filtrate obtained in step (11), and evaporate the solvent in a water bath at 30-35°C;

[0058] (13) Place the resultant in step (12) in a vacuum drying oven and dry at 65-70°C for 2 to 4 hours.

Example Embodiment

[0059] Example 2

[0060] A comprehensive resin adsorption technology for extracting tea polyphenols from waste fresh tea leaves, including the following steps:

[0061] (1) Rough separation of impurities:

[0062] A1: Use a tea washing machine to clean the discarded fresh tea leaves, and then heat the tea leaves to 260°C with microwaves and keep them for 4 minutes to inactivate enzymes;

[0063] A2: Extract waste fresh tea leaves in boiling water, crush them with a hammer mill, cut and crush the tea leaves to a mesh size of 180-230 meshes, filter, repeat more than twice, and combine the filtrate;

[0064] A3: Use a mixture of 97% chloroform and 3% petroleum ether to extract the filtrate, separate the layers, remove the chloroform petroleum ether extraction layer, and retain the aqueous layer;

[0065] A4: Repeat step A3 twice to combine the aqueous solution layers;

[0066] A5: Maintain the temperature of 35~40℃ to stir and evaporate the aqueous solution layer under negative pressure;

[0067] (2) Resin extraction: Circulate the liquid obtained in step A5 twice through the macroporous adsorption resin for adsorption. The macroporous adsorption resin is AB-8 macroporous adsorption resin with a pore size of 60~90nm and a porosity of 25%~40%. The system temperature is 18~22℃, and the flow rate is 4.2~4.6BV/h;

[0068] (3) Elution: Use an ethanol solution with a concentration of 10%-95% to elute the resin from a low concentration to a high concentration to obtain an eluate;

[0069] (4) Place the eluent in a 35~40℃ water bath to evaporate the solvent;

[0070] (5) Use a mixture of 83% chloroform and 17% petroleum ether to extract and remove impurities from the solution in step (4). During this period, shake the mixture, and then let it stand for more than 10 minutes, separate the liquid, and retain the aqueous layer. The chloroform and petroleum in this step The amount of ether does not need to be too large, it needs to be determined based on sampling and determination of impurity content;

[0071] (6) Repeat step (5) twice or more to combine the aqueous solution layers;

[0072] (7) Maintain the temperature of 35~45℃ to stir and evaporate the aqueous solution layer under negative pressure;

[0073] (8) Maintain the temperature of 60~65℃ to stir and evaporate the aqueous layer under negative pressure. The maintenance time is based on the following formula: T=Hm/2S, where T: time (h), H: solution height (m), m: solution Mass (kg), S: solution surface area (m 2 );

[0074] (9) Standing: After the temperature of the solution obtained in step (8) naturally drops to room temperature, place it in an environment of 5 to 7°C and stand for more than 1 hour;

[0075] (10) Filtration: filter the solid-liquid mixture obtained in step (9), recycle the filter residue, and take the filtrate;

[0076] (11) The filtrate obtained in step (10) is adsorbed on activated carbon, the mesh of which is 260-280;

[0077] (12) Concentration: vacuum the filtrate obtained in step (11), and evaporate the solvent in a water bath at 35-38°C;

[0078] (13) Place the resultant in step (12) in a vacuum drying oven and dry at 70-75°C for 2 to 4 hours.

Example Embodiment

[0079] Example 3

[0080] A comprehensive resin adsorption technology for extracting tea polyphenols from waste fresh tea leaves, including the following steps:

[0081] (1) Rough separation of impurities:

[0082] A1: Use a tea washing machine to clean the discarded fresh tea leaves, and then heat the tea leaves to 270°C with a microwave for 3.5 minutes to inactivate enzymes;

[0083] A2: Extract discarded fresh tea leaves in boiling water, crush them with an ultrafine pulverizer, cut and crush the tea leaves to 240-280 meshes, filter, repeat more than twice, and combine the filtrate;

[0084] A3: Use a mixture of 99% chloroform and 1% petroleum ether to extract the filtrate, separate the layers, remove the chloroform petroleum ether extraction layer, and retain the aqueous layer;

[0085] A4: Repeat step A3 twice to combine the aqueous solution layers;

[0086] A5: Maintain the temperature of 35~40℃ to stir and evaporate the aqueous solution layer under negative pressure;

[0087] (2) Resin extraction: Circulate the liquid obtained in step A5 twice through the macroporous adsorption resin for adsorption. The macroporous adsorption resin is AB-8 macroporous adsorption resin with a pore size of 60~90nm and a porosity of 25%~40%. The system temperature is 23~24℃, and the flow rate is 4.8~5.2BV/h;

[0088] (3) Elution: Use an ethanol solution with a concentration of 10%-95% to elute the resin from a low concentration to a high concentration to obtain an eluate;

[0089] (4) Place the eluent in a 35~40℃ water bath to evaporate the solvent;

[0090] (5) Use a mixture of 80% chloroform and 20% petroleum ether to extract and remove impurities from the solution in step (4). During this process, shake the mixed solution, and then let it stand for more than 10 minutes for separation. The aqueous layer is retained. The chloroform and petroleum in this step The amount of ether does not need to be too large, it needs to be determined based on sampling and determination of impurity content;

[0091] (6) Repeat step (5) twice or more to combine the aqueous solution layers;

[0092] (7) Maintain the temperature of 35~45℃ to stir and evaporate the aqueous solution layer under negative pressure;

[0093] (8) Maintain the temperature of 60~65℃ to stir and evaporate the aqueous layer under negative pressure. The maintenance time is based on the following formula: T=Hm/2S, where T: time (h), H: solution height (m), m: solution Mass (kg), S: solution surface area (m 2 );

[0094] (9) Standing: After the temperature of the solution obtained in step (8) naturally drops to room temperature, it is placed in an environment of 6 to 8°C and left to stand for more than 1 hour;

[0095] (10) Filtration: filter the solid-liquid mixture obtained in step (9), recycle the filter residue, and take the filtrate;

[0096] (11) The filtrate obtained in step (10) is adsorbed on activated carbon, and the activated carbon has a mesh number of 290-315 mesh;

[0097] (12) Concentration: vacuum the filtrate obtained in step (11), and evaporate the solvent in a water bath at 38-40°C;

[0098] (13) Place the resultant in step (12) in a vacuum drying oven and dry at 75-80°C for 2 to 4 hours.

PUM

Property	Measurement	Unit
Aperture	0.25 ~ 0.9	nm
Mesh	230.0 ~ 315.0	mesh
Mesh	230.0 ~ 250.0	mesh

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Classification and recommendation of technical efficacy words

efficient extraction

Resin adsorption synthesis technology for extracting tea polyphenols from discarded fresh tea leaves

AI-Extracted Technical Summary

Problems solved by technology

Abstract

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Examples

Example Embodiment

Example Embodiment

Example Embodiment

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Description & Claims & Application Information

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