CN116239559A - A kind of extraction technology rich in EGCG nanoscale Pu'er tea pigment - Google Patents

Abstract

The application discloses an extraction technology of a Pu' er tea pigment rich in EGCG nanometer grade, which comprises the following steps: selecting tea, cleaning, drying and crushing; adding green tea powder into ultrasonic countercurrent extraction equipment to extract solution; filtering the extraction solution and then carrying out crude extraction; leaching for multiple times to obtain crystals. The ultrasonic countercurrent extraction equipment is adopted for extraction, the problem of high operation difficulty during extraction is avoided, the low-temperature water bath is matched, oxidation and deterioration of tea polyphenol during extraction are avoided, EGCG extracting solution during multiple times of extraction is collected and mixed, the problem that the operation of the existing EGCG nanoscale puer tea pigment is time-consuming and troublesome during extraction, the solvent consumption is high, the cost is high and the extraction rate is low is solved, the operation difficulty is reduced, the solvent consumption is high, the cost is high, the extraction rate is ensured, and meanwhile, the extraction variable is conveniently controlled according to the tea variable during extraction, and the variable during extraction is conveniently controlled.

Description

A kind of extraction technology of EGCG-rich nanoscale Pu'er tea pigment

technical field

This application relates to extraction technology, especially an extraction technology rich in EGCG nano-scale Pu'er tea pigment.

Background technique

EGCG is epigallocatechin gallate, which is the most effective active ingredient in tea polyphenols. It has antibacterial, antiviral, antioxidative, antiarteriosclerotic, antithrombotic, antiangioproliferative, antiinflammatory and antitumor effects. Green tea It contains EGCG, which has the functions of preventing and treating cancer and other diseases and enhancing immunity in medicine and health care. It can be used as anti-oxidant, antibacterial, fresh-keeping, and deodorant in the food industry, and it can be used as a special function of quality assurance in daily chemical products. agent, skin care agent.

EGCG is the main component of green tea polyphenols, and also the main component of green tea catechins. Using Puer green tea to extract EGCG is a relatively common EGCG extraction method. The common method of separating EGCG is generally to clean the tea leaves, extract, and then separate Purification. When extracting fresh tea leaves, methods such as high temperature, grinding, and enzymatic hydrolysis are usually used to destroy the cell walls of the tea leaves, so as to realize the full outflow of the substances in the tea leaves. The traditional extraction process uses water or ethanol as a solvent, and is heated in a water bath to Extract at 80°C for several times, combine the extracts and extract with an equal volume of chloroform, separate the chloroform phase and use ethyl acetate for multiple extractions, recover most of the ethyl acetate and concentrate it to dryness, freeze-dry and use deionized Repeated recrystallization of water can obtain high-quality goods, but the operation is time-consuming and troublesome during extraction, the solvent consumption is large, the cost is high, and the extraction rate is low. Extraction at high temperature, tea polyphenols are easy to oxidize and deteriorate, or use microwave radiation to extract tea polyphenols. The main factors affecting the microwave extraction process during radiation extraction of tea polyphenols include: microwave heating power, type of extraction solvent, extraction time, amount of solvent and amount of wetting water, etc. During extraction, the maturity of tea leaves is different, the size of tea leaves is different, etc. , During extraction, the power required for microwave heating is also different, and it is also difficult to control the extraction conditions during extraction. Therefore, in view of the above problems, an extraction technology of EGCG-rich nanoscale Pu-erh tea pigment is proposed.

Contents of the invention

In this embodiment, an extraction technology rich in EGCG nano-scale Pu-erh tea pigment is provided to solve the problem of time-consuming and troublesome extraction of EGCG nano-scale Pu-erh tea pigment in the prior art, large solvent consumption, high cost, and high extraction cost. low rate problem.

According to one aspect of the present application, there is provided an extraction technique rich in EGCG nano-scale Pu'er tea pigment, the extraction technique of said Pu'er tea pigment comprises the following steps:

(1) select the tea leaves to be cleaned and dried and pulverized;

(2) adding green tea powder to the ultrasonic countercurrent extraction equipment to extract the solution;

(3) Carry out rough extraction after filtering the extraction solution;

(4) add deionized water to carry out rough extraction in the filtrate that separates;

(5) Crystals are obtained after multiple leaching.

Further, in the step (1), fresh Pu-erh green tea is selected, and the Pu-erh green tea is put into warm water to be cleaned several times. After cleaning, it is put into a drying box for drying, and the temperature during drying is 20° C. -30°C, dry until the surface of the Puer green tea is completely dry, put the dried Puer green tea into a pulverizer for crushing, crush the tea leaves of the Puer green tea to support the tea powder, and fully ensure the dryness of the Puer green tea when crushing. Avoid tea powder sticking when crushing.

Further, in the step (2), first filter the crushed Pu’er green tea leaves, filter out the Pu’er green tea leaves that do not meet the crushing scale, and add the filtered Pu’er green tea leaves to the ultrasonic Extraction is carried out in countercurrent extraction equipment, and the solution is extracted.

Further, in the step (2), the extract is microfiltered through a microporous precision filter, and then the microfiltered tea juice is ultrafiltered through an ultrafilter to remove impurities such as proteins collected in the tea juice, and Extract the ultra-filtered tea juice.

Further, in the step (2), when the extract is microfiltered through a microporous precision filter, it is first rinsed with clean water at 45°C-55°C. When rinsing, the water flow is slow and gentle, and the water flow rate is low. Keep the extracting solution stable while shaking to avoid turbidity of the washing solution caused by shaking. Rinse until the surface turbidity disappears, and then filter after rinsing.

Further, in the step (3), add citrate aqueous solution to the filtered tea juice in portions, heat to 55°C-65°C, keep for 1-2h, then filter the mixed solution, and obtain the extract after filtering , the extract is concentrated to obtain a concentrated solution, and then citric acid is added to the concentrated solution to adjust the pH to 5.5-6.5. After cooling and standing still, microfiltration is carried out through a microporous precision filter to obtain a precipitate containing tea polyphenols and a tea, coffee, and theophylline-containing tea pigment. of the filtrate.

Further, in the step (4), add deionized water to the precipitate containing tea polyphenols and mix evenly. When mixing, after adding deionized water, stir and mix along the same direction. After mixing, mix the mixture After standing still for 2-3 hours, keep the temperature of the mixed solution at 50° C.-60° C., and then filter the mixed solution to obtain EGCG extract and green tea filter residue respectively.

Further, in the step (5), the green tea filter residue is repeatedly added to deionized water for leaching, and the number of leaching is 2-3 times, and the EGCG extract during each leaching is collected, and the EGCG after each leaching is The extracts are all mixed together. When mixing, stir each EGCG extract evenly.

Further, the pH value of the deionized water during extraction in the steps (5) and (4) is 5-7, the temperature during extraction is 60°C-70°C, the extraction time is 25-30min, and the green tea filter residue and The volume ratio of deionized water is 3:1. As the number of extractions increases, the volume ratio of green tea residue to deionized water gradually decreases, and the lowest drops to a volume ratio of green tea residue to deionized water of 1:1. , and the extraction time gradually decreased with the increase of times.

Further, in the step (5), cool down the collected EGCG extract during each leaching to 1-4°C, let it stand for crystallization, vacuum filter to obtain solid crystals, and recrystallize the solid crystals with 7% acetic acid solution , vacuum filtration, freeze-drying the filter block after suction filtration to obtain the tea extract of white crystals.

Through the above-mentioned embodiments of the present application, ultrasonic countercurrent extraction equipment is used for extraction, which avoids the problem of difficult operation during extraction, and cooperates with a low-temperature water bath to avoid oxidation and deterioration of tea polyphenols during extraction. EGCG extracts collected during multiple extractions are mixed , to avoid excessive solvent consumption during extraction, and solve the problems of time-consuming operation, large solvent consumption, high cost and low extraction rate of the existing EGCG nano-scale Pu-erh tea pigment during extraction, while reducing the difficulty of operation, It also reduces the large consumption of solvent and high cost, and also ensures the extraction rate. At the same time, it is convenient to control the extraction variable according to the tea variable during extraction, and it is convenient to control the variable during extraction.

Description of drawings

In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings that need to be used in the description of the embodiments or the prior art. Obviously, the accompanying drawings in the following description are only These are some embodiments of the present application. Those skilled in the art can also obtain other drawings based on these drawings without any creative effort.

FIG. 1 is a schematic diagram of an extraction process in an embodiment of the present application.

Detailed ways

In order to enable those skilled in the art to better understand the solution of the present application, the technical solution in the embodiment of the application will be clearly and completely described below in conjunction with the accompanying drawings in the embodiment of the application. Obviously, the described embodiment is only It is an embodiment of a part of the application, but not all of the embodiments. Based on the embodiments in this application, all other embodiments obtained by persons of ordinary skill in the art without creative efforts shall fall within the scope of protection of this application.

It should be noted that the terms "first" and "second" in the description and claims of the present application and the above drawings are used to distinguish similar objects, but not necessarily used to describe a specific sequence or sequence. It should be understood that the data so used may be interchanged under appropriate circumstances for the embodiments of the application described herein. Furthermore, the terms "comprising" and "having", as well as any variations thereof, are intended to cover a non-exclusive inclusion, for example, a process, method, system, product or device comprising a sequence of steps or elements is not necessarily limited to the expressly listed instead, may include other steps or elements not explicitly listed or inherent to the process, method, product or apparatus.

In this application, the terms "upper", "lower", "left", "right", "front", "rear", "top", "bottom", "inner", "outer", "middle", The orientations or positional relationships indicated by "vertical", "horizontal", "horizontal", and "longitudinal" are based on the orientations or positional relationships shown in the drawings. These terms are mainly used to better describe the present application and its embodiments, and are not used to limit that the indicated device, element or component must have a specific orientation, or be constructed and operated in a specific orientation.

Moreover, some of the above terms may be used to indicate other meanings besides orientation or positional relationship, for example, the term "upper" may also be used to indicate a certain attachment relationship or connection relationship in some cases. Those skilled in the art can understand the specific meanings of these terms in this application according to specific situations.

Furthermore, the terms "mounted", "disposed", "provided", "connected", "connected", "socketed" should be interpreted broadly. For example, it may be a fixed connection, a detachable connection, or an integral structure; it may be a mechanical connection or an electrical connection; it may be a direct connection or an indirect connection through an intermediary; internal connectivity. Those of ordinary skill in the art can understand the specific meanings of the above terms in this application according to specific situations.

It should be noted that, in the case of no conflict, the embodiments in the present application and the features in the embodiments can be combined with each other. The present application will be described in detail below with reference to the accompanying drawings and embodiments.

Please refer to shown in Figure 1, a kind of extraction technology that is rich in EGCG nano-scale Pu'er tea pigment, the extraction technology of described Pu'er tea pigment comprises the following steps:

(1) select the tea leaves to be cleaned and dried and pulverized;

(2) adding green tea powder to the ultrasonic countercurrent extraction equipment to extract the solution;

(3) Carry out rough extraction after filtering the extraction solution;

(4) add deionized water to carry out rough extraction in the filtrate that separates;

(5) Crystals are obtained after multiple leaching.

In the step (1), fresh Pu’er green tea is selected, and the Pu’er green tea is put into warm water to be cleaned several times. After cleaning, it is put into a drying box for drying, and the temperature during drying is 20° C.-30° C. , dry until the surface of the Pu’er green tea is completely dry, put the dried Pu’er green tea into a pulverizer for crushing, crush the tea leaves of the Pu’er green tea to support the tea powder, fully ensure the dryness of the Pu’er green tea when crushing, and avoid crushing The tea powder is sticky.

In the step (2), first filter the crushed Puer green tea leaves, filter out the Puer green tea leaves that do not meet the crushing scale, and add the filtered Puer green tea leaves to the ultrasonic countercurrent extraction equipment continuously in equal amounts Extraction is carried out and the solution is extracted.

In the step (2), the extract is microfiltered through a microporous precision filter, and then the microfiltered tea juice is ultrafiltered through an ultrafilter to remove impurities such as proteins collected in the tea juice, and extract the ultrafiltered After the tea juice.

In the step (2), when the extract is microfiltered through a microporous precision filter, it is first rinsed with 45°C-55°C clean water. When rinsing, ensure that the water flow is slow and gentle, and the water flow rate is low. Keep the extraction during rinsing. The solution should be stable, avoid turbidity caused by shaking, rinse until the surface turbidity disappears, and then filter after rinsing.

In the step (3), add citrate aqueous solution to the filtered tea juice in stages, heat to 55°C-65°C, keep for 1-2h, then filter the mixed solution, and obtain the extract after filtering, the extract Concentrate to obtain a concentrated solution, then add citric acid to the concentrated solution to adjust the pH to 5.5-6.5, after cooling and standing still, perform microfiltration through a microporous precision filter to obtain a precipitate containing tea polyphenols and a filtrate containing theophylline and theophylline.

In the step (4), add deionized water to the precipitate containing tea polyphenols and mix evenly. When mixing, after adding deionized water, stir and mix along the same direction. After mixing, leave the mixed solution for 2 After -3 hours, when standing still, keep the temperature of the mixed solution at 50°C-60°C, and then filter the mixed solution to obtain EGCG extract and green tea filter residue respectively.

In described step (5), the green tea filter residue is repeatedly added to deionized water for leaching, and the number of times of leaching is 2-3 times, and the EGCG extracting solution during each leaching is collected, and the EGCG extracting solution after each leaching is all Mix together, while mixing, stir each EGCG extract to mix well.

The pH value of the deionized water during extraction in the steps (5) and (4) is 5-7, the temperature during extraction is 60°C-70°C, and the extraction time is 25-30min. Green tea filter residue and deionized water The volume ratio of green tea filter residue to deionized water is 3:1. With the increase of extraction times, the volume ratio of green tea residue to deionized water gradually decreases, and the lowest drops to a volume ratio of green tea residue to deionized water of 1:1. The time also decreases gradually as the number of times increases.

In the step (5), the collected EGCG extract during each leaching is cooled to 1-4° C., left to crystallize, vacuum filtered to obtain solid crystals, and the solid crystals are recrystallized with 7% acetic acid solution, vacuum pumped Filter, and freeze-dry the filter block after suction filtration to obtain the tea extract of white crystals.

The circuits, electronic components and modules involved are all existing technologies, and those skilled in the art can fully realize them. Needless to say, the protection content of this application does not involve the improvement of software and methods.

The above descriptions are only preferred embodiments of the present application, and are not intended to limit the present application. For those skilled in the art, there may be various modifications and changes in the present application. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of this application shall be included within the protection scope of this application.

Claims (10)

1. An extraction technology of a nano-scale puer tea pigment rich in EGCG is characterized in that: the extraction technology of the puer tea pigment comprises the following steps:

(1) Selecting tea, cleaning, drying and crushing;

(2) Adding green tea powder into ultrasonic countercurrent extraction equipment to extract solution;

(3) Filtering the extraction solution and then carrying out crude extraction;

(4) Adding deionized water into the filtrate obtained by separation for crude extraction;

(5) Leaching for multiple times to obtain crystals.

2. The technology for extracting the EGCG-rich nanoscale puer tea pigment according to claim 1, which is characterized in that: and (2) selecting fresh puer green tea in the step (1), putting puer green tea into warm water for cleaning for a plurality of times, putting into a drying box for drying after cleaning, wherein the temperature during drying is 20-30 ℃, drying until the surface of puer green tea is thoroughly dried, putting the dried puer green tea into a pulverizer for pulverizing, pulverizing puer green tea into tea powder, fully ensuring the dryness of puer green tea during pulverizing, and avoiding the sticking of the tea powder during pulverizing.

3. The technology for extracting the EGCG-rich nanoscale puer tea pigment according to claim 1, which is characterized in that: in the step (2), the crushed puer green tea dust is filtered, puer green tea dust which does not accord with the crushing scale is filtered, and the filtered puer green tea dust is continuously added into ultrasonic countercurrent extraction equipment for extraction in equal quantity and in batches, and the solution is extracted.

4. The technology for extracting the EGCG-rich nanoscale puer tea pigment according to claim 1, which is characterized in that: in the step (2), the extracting solution is subjected to microfiltration through a microporous precise filter, and the tea juice after microfiltration is subjected to ultrafiltration through an ultrafilter, so that impurities such as protein summarized by the tea juice are removed, and the tea juice after ultrafiltration is extracted.

5. The technology for extracting the EGCG-rich nanoscale puer tea pigment according to claim 1, which is characterized in that: in the step (2), when the extracting solution is subjected to microfiltration through a microporous precise filter, the extracting solution is firstly washed by purified water at 45-55 ℃, the water flow is ensured to be slow and mild during washing, the water flow is low, the extracting solution is kept stable during washing, the turbidity of the washing solution caused by shaking is avoided, the washing solution is washed until the surface turbidity disappears, and the filtering is performed after the washing.

6. The technology for extracting the EGCG-rich nanoscale puer tea pigment according to claim 1, which is characterized in that: and (3) adding citrate aqueous solution into the filtered tea juice in a plurality of times, heating to 55-65 ℃, keeping for 1-2h, filtering the mixed solution, obtaining an extracting solution after filtering, concentrating the extracting solution to obtain a concentrated solution, adding citric acid into the concentrated solution to adjust the pH value to 5.5-6.5, cooling and standing, and carrying out microfiltration through a microporous precise filter to obtain a precipitate containing tea polyphenol and a filtrate containing tea pigment of caffeine.

7. The technology for extracting the EGCG-rich nanoscale puer tea pigment according to claim 1, which is characterized in that: adding deionized water into the precipitate containing tea polyphenol in the step (4) and uniformly mixing, adding deionized water when mixing, stirring and mixing along the same direction, standing the mixed solution for 2-3h after mixing, keeping the temperature of the mixed solution at 50-60 ℃ when standing, and filtering the mixed solution to obtain EGCG extract and green tea filter residues respectively.

8. The technology for extracting the EGCG-rich nanoscale puer tea pigment according to claim 1, which is characterized in that: and (3) repeatedly adding deionized water into green tea filter residues for leaching for 2-3 times, collecting EGCG extract liquid obtained in each leaching, mixing the EGCG extract liquid obtained in each leaching, and uniformly stirring and mixing the EGCG extract liquid in each mixing.

9. The technology for extracting the EGCG-rich nanoscale puer tea pigment according to claim 1, which is characterized in that: the PH value of deionized water in the leaching in the steps (5) and (4) is 5-7, the temperature in the extracting is 60-70 ℃, the extracting time is 25-30min, and the volume ratio of green tea filter residues to deionized water is 3:1, along with the increase of the extraction times, the volume ratio of the green tea filter residue to the deionized water is gradually reduced, and the minimum volume ratio of the green tea filter residue to the deionized water is 1:1, the leaching time also gradually decreases with increasing times.

10. The technology for extracting the EGCG-rich nanoscale puer tea pigment according to claim 1, which is characterized in that: and (3) cooling the collected EGCG extract liquid during each leaching in the step (5) to 1-4 ℃, standing for crystallization, vacuum-filtering to obtain solid crystals, recrystallizing the solid crystals by using 7% acetic acid solution, vacuum-filtering, and freeze-drying the filter blocks after the vacuum filtration to obtain the tea extract of white crystals.

Images