CN103242314B - Method for comprehensively extracting effective ingredients in tea - Google Patents
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Abstract
The invention relates to a method for comprehensively extracting effective ingredients in tea. The method comprises the following steps of: with a faintly acidic water solution as a main extraction solvent and a certain amount of organic solvent as an auxiliary extraction solvent, carrying out step-by-step extraction on water extracts to obtain four effective ingredients, namely tea polyphenol, caffeine, tea polysaccharide and theanine; and meanwhile, extracting tea protein from tea residues by using an alkali dissolution and acid deposition method. According to the method, as water is used as the main solvent, the cost is low, the reactions are mild and active ingredients are favorably preserved; as a certain amount of organic solvent is used as the auxiliary extraction solvent, the problems of overhigh cost and product pollution caused by use of a large amount of organic solvents are solved; meanwhile, five effective ingredients, namely the tea polyphenol, the tea polysaccharide, the caffeine, the theanine and the tea protein are extracted, and therefore high extraction rate, high purity and high utilization rate of tea are achieved; the solvents are recycled in the extraction process, so that the preparation cost is reduced; and no alkali and acid waste liquor is discharged in the overall process, and therefore the method is environment-friendly. The overall preparation flow is high in efficiency and low in cost, and therefore the method has a favorable application value.
Description
Technical field
The invention belongs to field of deep tea processing technology, relate to the method for effective constituent in a kind of comprehensive extraction tealeaves, particularly a kind of method efficiently preparing effective constituent in tealeaves of applicable suitability for industrialized production.
Background technology
As the Traditional health care beverage of the Chinese nation, tealeaves is just subject to liking and paying attention to of people since ancient times.Moreover, in the world today, tealeaves has become first of three large beverages (tealeaves, coffee, cocoa).China is the country that a tea resources quite enriches, however along with Tea Consumption increasingly superior, a large amount of low and middle-grade tealeaves deadstocks, simultaneously can produce a large amount of byproducts in the Tea Production course of processing, utilization ratio is extremely low.Therefore, utilize the tankage of low and middle-grade tealeaves and Tea Processing to extract its effective constituent, greatly develop deep tea processing technology, open up tealeaves novelty teabag, not only can open up low and middle-grade tea market, make full use of tea resources, also will become the new direction of China's tealeaves industry development.
Scientific research and clinical medicine experiment show, tealeaves has many health-care effects, and this is inseparable with the effective efficiency composition in tealeaves.Effective constituent in tealeaves comprises tea-polyphenol, tea polysaccharide, trimethyl-xanthine, theanine, tea albumen etc.Tea-polyphenol is not only a kind of natural antioxidant, and there is reducing blood-fat, hypotensive and reduction cholesterol, arteriosclerosis, anti-mutation, anticancer change, anti-ageing, radioprotective, the physiological function such as antiviral, have purposes widely in the industries such as medicine, beverage, food, health care; Tea polysaccharide has excellent pharmacological function, experiment shows, after tea polysaccharide enters human body, can antithrombotic, anticoagulation, radioprotective, reducing blood-fat, hypoglycemic, delay senility, and the non-specific immunity of human body can be strengthened at short notice, control Tiroidina hypertrophy and diabetes, improve hemopoietic function etc.; Trimethyl-xanthine, as important medical material, has cardiac stimulus, excited cerebral nerve and diuretic properties, is also the additive of various beverages simultaneously; Theanine has step-down, improves memory, strengthens human body and resists the effects such as the ability of virus infection, is a kind of novel antiviral, bacterium, the medicine of fungi and healthcare products composition; Tea albumen can remove superoxide anion, has reducing blood-fat, the effects such as anti-mutation, atherosclerosis and coronary heart disease, is a kind of not only nutritious but also has the protein of plurality of health care functions.Therefore, high efficiency extraction tea-polyphenol from tealeaves, tea polysaccharide, trimethyl-xanthine, the effective constituents such as theanine and tea albumen, can produce great economic benefit and social benefit.
In tealeaves, the method for extracts active ingredients mainly contains water extract method, organic solvent extraction, the precipitator method, supercritical CO
2extraction process, ultrasonic extraction and microwave extraction method etc.Although organic solvent extraction extraction yield is higher, easily cause organic solvent pollution; Precipitator method three-waste pollution is serious, there is food safety hidden danger; Supercritical CO
2extraction process is high to equipment requirements, and device is complicated, involves great expense; Greatly, cost is high, how as supplementary means for ultrasonic extraction and microwave extraction method energy consumption.Therefore, water extract method is both economical efficient method for extracting effective content of tea.
At present, about the patent report of extraction plurality of active ingredients comprehensive from tealeaves is less, as: Chinese patent (96113134.9) reports a kind of method extracting tea-polyphenol and byproduct thereof from tealeaves, technique relative complex, and energy consumption is higher; Chinese patent (02132857.9) reports a kind of cold extraction method of effective content of tea, obtain effective constituent extracting solution and not by each component separating; Chinese patent application (200410015905.2) reports a kind of method of microwave radiation exaraction tea-polyphenol, tea polysaccharide, trimethyl-xanthine, and in this production technique, the purity of tea-polyphenol is 80%, but yield is only 5%; Chinese patent application (200410089179.9) reports the method for effective constituent in a kind of ultrasonic vibration extract at low temperature tealeaves, although extraction time is short, energy consumption is high, and the yield of effective constituent is also undesirable.Chinese patent application (200510042629.3) reports a kind of complex enzyme hydrolysis and extracts and water extraction tea-polyphenol the production technique of the effective constituent such as by-product trimethyl-xanthine and tea polysaccharide; Chinese patent application (200910040927.7) reports effective constituent in a kind of high efficiency extraction Camellia nitidissima Chi leaf and concentrated solution is applied to the technique in cigarette preparation; Chinese patent application (201210170786.2) reports a kind of method adopting light wave to extract plurality of active ingredients from tealeaves.The extraction of same valuable tea albumen in tea grounds is not all considered in above-mentioned patent.
Summary of the invention
The object of this invention is to provide one efficiently from tealeaves comprehensive extraction comprise tea-polyphenol, tea polysaccharide, trimethyl-xanthine, theanine, the method for the effective constituents such as tea albumen.Present method with commercially available low and middle-grade green tea for raw material, be main extraction solvent with weakly acidic water solution, organic solvent is as auxiliary extraction solvent, step by step arithmetic Tea Polyphenols in Tea, trimethyl-xanthine, tea polysaccharide, theanine, the effective constituents such as tea albumen, the method effectively can improve utilization ratio and the productivity effect of tealeaves, reduces preparation cost.Process flow sheet as shown in Figure 1.
The method of effective constituent in a kind of comprehensive extraction tealeaves of the present invention, its step is as follows:
(1) the weakly acidic water solution lixiviate of effective content of tea
Tealeaves is crossed 60 ~ 80 mesh sieves, obtain tea powder, by tea powder: phosphate buffered saline buffer=1:15 ~ 1:30(g/mL) tea powder is placed in phosphate buffered saline buffer by solid-to-liquid ratio, this system is placed in water bath with thermostatic control and shakes extraction 30 ~ 60min, repeat to extract, collecting by filtration tea grounds, namely merging filtrate obtains effective content of tea Aqueous extracts;
(2) extraction of tea albumen
Gained tea grounds in step (1) is dried, by tea grounds: tea grounds is placed in the alkaline NaOH aqueous solution by the solid-to-liquid ratio (g/mL) of alkali lye=1:20 ~ 1:40, this system is placed in water bath with thermostatic control and shakes extraction 60 ~ 120min, filter cleaner obtains the alkaline water extract of tea albumen; In the alkaline water extract of gained tea albumen, add hydrochloric acid, regulate pH 4.5 to precipitate, precipitation freeze-drying obtains the tea albumen crude product that purity is more than 50%;
(3) extracting and separating of trimethyl-xanthine
By gained effective content of tea Aqueous extracts in step (1), concentrated by rotary evaporation, to 1/3 of original volume, makes solid content reach 1% ~ 5%, adds isopyknic chloroform or methylene dichloride with concentrated solution; Concussion extraction trimethyl-xanthine under room temperature, fully after extraction, upper strata aqueous phase is separated with lower floor's organic phase, takes off a layer organic phase, and reduction vaporization reclaims organic solvent, and gained solid substance is multiple water-soluble, and freeze-drying obtains purity more than 85% trimethyl-xanthine;
(4) extracting and separating of tea-polyphenol
Isopyknic ethyl acetate is with it used to shake extraction under room temperature gained aqueous phase after extraction in step (3), after abundant extraction, upper organic phase is separated with lower layer of water, get upper organic phase, reduction vaporization reclaims ethyl acetate, gained solid substance is multiple water-soluble, and freeze-drying obtains the tea-polyphenol of purity more than 80%;
(5) precipitate and separate of tea polysaccharide and theanine
By gained aqueous phase after extraction in step (4), use isopyknic 95% alcohol settling with it, centrifugal collection supernatant liquor and precipitation respectively, precipitation freeze-drying obtains total sugar content more than 60% tea polysaccharide; By the freeze-drying of gained supernatant liquor, a small amount of water dissolution of solid substance, then uses dehydrated alcohol recrystallization repeatedly under low temperature, obtains the theanine of purity more than 65%.
In described step (1), phosphate buffered saline buffer pH is 5 ~ 6, and water bath with thermostatic control temperature is 50 ° of C ~ 80 ° C.
Repeating extraction time in described step (1) is 1 ~ 3 time, filters and collects tea grounds, merging filtrate, obtaining effective content of tea Aqueous extracts.
Described step (2) neutral and alkali NaOH concentration of aqueous solution is 0.06 ~ 0.10mol/L, and bath temperature is 70 ° of C ~ 90 ° C, HCl concentration is 0.05mol/L ~ 0.10mol/L.
After extraction time 0.5h ~ 1h that in described step (3) or (4), the condition of fully extraction is, leave standstill abundant extraction time.
In described step (5), alcohol settling number of times is 2 times, and low temperature is-10 ° of C ~-20 ° C.
The present invention has the following advantages:
(1) distilled water is adopted to extract as primary solvent, with low cost, environmental protection; Extract as secondary solvent using a certain amount of organic solvent, avoid the high cost that with an organic solvent brings in a large number and product contamination problem;
(2) step-by-step extracting method is adopted, first extract with weakly acidic water solution, tea polyphenol extract rate improves nearly 30% compared with the extraction with aqueous solution speed under the same terms, avoids the shortcoming of too much tea albumen immersed proposition when weak alkaline aqueous solution extracts, is conducive to obtaining the higher tea-polyphenol of purity; Adopt alkali to put forward the heavy method of acid afterwards and extract tea albumen, method is simple and direct, and cost is low, and can obtain the higher tea albumen of purity;
(3) extract tea-polyphenol in tradition, trimethyl-xanthine, on the basis of tea polysaccharide and theanine, adds the extraction of tea albumen in tea grounds, improves utilization ratio and the productivity effect of tealeaves.
(4) adopt repeatedly solvent extraction and deionized water to wash the method combined in leaching process and obtain effective constituent, the extraction solvent that each step uses and the equal recoverable of deionized water, significantly reduce production cost, whole Production Flow Chart high-efficiency environment friendly, cost are lower, have good using value.
The present invention is main extraction solvent with weakly acidic water solution, a certain amount of organic solvent as auxiliary extraction solvent, to Aqueous extracts step by step arithmetic tea-polyphenol, trimethyl-xanthine, tea polysaccharide, theanine 4 kinds of effective constituents; Employing alkali carries the tea albumen in the heavy method extraction tea grounds of acid simultaneously.Advantage of the present invention: (1) is primary solvent with water, and cost is low, and mild condition, is beneficial to preservation activeconstituents; Extract as secondary solvent using a certain amount of organic solvent, avoid the high cost that with an organic solvent brings in a large number and product contamination problem; (2) Simultaneous Extraction of Tea Polyphenols, tea polysaccharide, trimethyl-xanthine, theanine and tea albumen 5 kinds of effective constituents, extraction yield is high, and purity is high, and the utilization ratio of tealeaves is high; (3) the equal recoverable of the solvent in leaching process, reduces preparation cost; (4) discharge without alkalescence and acid waste liquid in whole set process, environmental friendliness.A complete set of preparation flow is efficient, low cost, has good using value.
Accompanying drawing explanation
Fig. 1 integrated extraction technique schema;
The color atlas of tea-polyphenol after Fig. 2 embodiment 1 purifying.
Embodiment
Embodiment 1:
(1) the weakly acidic water solution lixiviate of effective content of tea
By the tealeaves dedusting of oven dry, pulverizing, cross 60 ~ 80 mesh sieves.Get 10g60 ~ 80 object tea powder, add the phosphate buffered saline buffer that 150mL pH is 5, then this system is placed in the water bath with thermostatic control concussion extraction that temperature is 50 ° of C, after extracting 30min, filters, collect tea grounds dry, get supernatant liquor for subsequent use.
(2) extraction of tea albumen
Get the tea grounds 5g collected in (1) step, adding 100mL concentration by the solid-to-liquid ratio of 1:20 is in the alkaline NaOH aqueous solution of 0.06mol/L, and this system being placed in temperature is that 60min is extracted in the water bath with thermostatic control concussion of 70 ° of C, filters to obtain the alkaline water extract of tea albumen; In the alkaline water extract of tea albumen, add 0.05mol/L hydrochloric acid, regulate pH 4.5 to precipitate, centrifugal removing supernatant liquor, collecting precipitation, freeze-drying obtains tea albumen crude product 816.28mg, and extraction yield is 8.16%, purity 50.59%.
(3) extracting and separating of trimethyl-xanthine
By gained supernatant liquor concentrated by rotary evaporation in (1) step to 1/3 of original volume, solid content is made to reach 1% ~ 5%, add isopyknic chloroform or methylene dichloride with concentrated solution, under room temperature, fully concussion extracts 0.5h, leaves standstill 0.5h, collects upper strata aqueous phase and lower floor's organic phase respectively, organic phase is again with isopyknic chloroform or methylene dichloride room temperature concussion extraction 0.5h, leave standstill 0.5h, again collect upper strata aqueous phase and lower floor's organic phase, merge aqueous phase and organic phase that twice extraction obtain respectively.Reclaim for subsequent use by the organic phase reduction vaporization removing chloroform after merging or methylene dichloride, the solid substance obtained adds 5mL distilled water washing twice, and lyophilize obtains 10.52mg trimethyl-xanthine, and extraction yield is 1.05%, and purity is 85.5%.
(4) extracting and separating of tea-polyphenol
Gained aqueous phase concentrated by rotary evaporation will be merged to 1/3 of original volume in (3) step, solid content is made to reach 1% ~ 5%, use isopyknic ethyl acetate, abundant concussion extraction 0.5h, leaves standstill 0.5h, collects upper organic phase and lower floor's aqueous phase respectively, organic phase is again with isopyknic ethyl acetate concussion extraction 0.5h, leave standstill 0.5h, again collect upper organic phase and lower floor's aqueous phase, merge aqueous phase and organic phase that twice extraction obtain respectively.Reclaim for subsequent use by the organic phase reduction vaporization removing ethyl acetate after merging, the solid substance obtained adds 5mL distilled water washing twice, and lyophilize obtains 855.06mg tea-polyphenol, extraction yield 41.1%, and purity is 81.5%.
After purifying, the color atlas of tea-polyphenol is shown in Fig. 2, wherein containing gallic acid (GA) 5.11%, epi-nutgall acid catechin (EGC) 5.05%, l-Epicatechol (EC) 6.27%, NVP-XAA 723 (EGCG) 50.12%, nutgall catechin gallic acid ester (GCG) 1.67%, L-Epicatechin gallate (ECG) 13.28%.
(5) precipitate and separate of tea polysaccharide and theanine
By merging gained aqueous phase concentrated by rotary evaporation in (4) step to 1/3 of original volume, making solid content reach 1% ~ 5%, with isopyknic 95% alcohol settling 2 times, centrifugally collecting supernatant liquor and precipitation respectively.Supernatant liquor freeze-drying, a small amount of water dissolution of solid substance, then uses dehydrated alcohol in-10 ° of C recrystallizations 2 times, obtains 10.9mg theanine, extraction yield 1.09%, purity 65.2%; Precipitation distilled water washing twice, lyophilize obtains 786mg tea polysaccharide, total sugar content 65.5%, and extraction yield is 7.86%.
Embodiment 2:
(1) the weakly acidic water solution lixiviate of effective content of tea
By the tealeaves dedusting of oven dry, pulverizing, cross 60 ~ 80 mesh sieves.Get 10g60 ~ 80 object tea powder, add the phosphate buffered saline buffer that 250mL pH is 5 ~ 6, then this system is placed in the water bath with thermostatic control concussion extraction that temperature is 70 ° of C, after extracting 40min, filter tea grounds by above-mentioned steps add 250mL pH be 5.5 phosphate buffered saline buffer extract 1 time again, collecting by filtration tea grounds is dry, and the supernatant liquor merging extracted twice is for subsequent use.
(2) extraction of tea albumen
Get the tea grounds 5g collected in (1) step, adding 150mL concentration by the solid-to-liquid ratio of 1:30 is in the alkaline NaOH aqueous solution of 0.08mol/L, and this system being placed in temperature is that 90min is extracted in the water bath with thermostatic control concussion of 80 ° of C, filters to obtain the alkaline water extract of tea albumen; In the alkaline water extract of tea albumen, add 0.075mol/L hydrochloric acid, regulate pH 4.5 to precipitate, centrifugal removing supernatant liquor, collecting precipitation, freeze-drying obtains tea albumen crude product 942.5mg, and extraction yield is 9.43%, and purity is 52.32%.
(3) extracting and separating of trimethyl-xanthine
By gained supernatant liquor concentrated by rotary evaporation in (1) step to 1/3 of original volume, solid content is made to reach 1% ~ 5%, with isopyknic chloroform or methylene dichloride, abundant concussion extraction 45min, leaves standstill 45min, collects upper strata aqueous phase and lower floor's organic phase respectively, organic phase is again with isopyknic chloroform or methylene dichloride concussion extraction 45min, leave standstill 45min, again collect upper strata aqueous phase and lower floor's organic phase, merge aqueous phase and organic phase that twice extraction obtain respectively.Reclaim for subsequent use by the organic phase reduction vaporization removing chloroform/methylene dichloride after merging, the solid substance obtained adds 5mL distilled water washing twice, and lyophilize obtains 11.8mg trimethyl-xanthine, and extraction yield is 1.18%, and purity is 87%.
(4) extracting and separating of tea-polyphenol
Gained aqueous phase concentrated by rotary evaporation will be merged to 1/3 of original volume in (3) step, solid content is made to reach 1% ~ 5%, use isopyknic ethyl acetate, abundant concussion extraction 45min, leaves standstill 45min, collects upper organic phase and lower floor's aqueous phase respectively, organic phase is again with isopyknic ethyl acetate concussion extraction 45min, leave standstill 45min, again collect upper organic phase and lower floor's aqueous phase, merge aqueous phase and organic phase that twice extraction obtain respectively.Reclaim for subsequent use by the organic phase reduction vaporization removing ethyl acetate after merging, the solid substance obtained adds 5mL distilled water washing twice, and lyophilize obtains 1530.2mg tea-polyphenol, extraction yield 78.16%, and purity is 82.7%.
(5) precipitate and separate of tea polysaccharide and theanine
Gained aqueous phase is concentrated into original volume 1/3 will be merged in (4) step, and make solid content reach 1% ~ 5%, with isopyknic 95% alcohol settling 2 times, centrifugally collect supernatant liquor and precipitation respectively.Supernatant liquor freeze-drying, a small amount of water dissolution of solid substance, then use dehydrated alcohol in-15 ° of C recrystallizations 2 times, obtain 13.9mg theanine, extraction yield is 1.39%, and purity is 66.4%.Precipitation distilled water washing twice, lyophilize obtains 1346.5mg tea polysaccharide, total sugar content 66.8%, and extraction yield is 13.47%.
Embodiment 3:
(1) the weakly acidic water solution lixiviate of effective content of tea
By the tealeaves dedusting of oven dry, pulverizing, cross 60 ~ 80 mesh sieves.Get 10g60 ~ 80 object tea powder, add the phosphate buffered saline buffer that 300mL pH is 5 ~ 6, then this system is placed in the water bath with thermostatic control concussion extraction that temperature is 80 ° of C, after extracting 60min, collecting by filtration tea grounds add 300mL pH be 6 phosphate buffered saline buffer more repeatedly extract 2 times, filter, collect tea grounds dry, merge the supernatant liquor extracted for 3 times for subsequent use.
(2) extraction of tea albumen
Get the tea grounds 5g collected in (1) step, adding 200mL concentration by the solid-to-liquid ratio of 1:40 is in the alkaline NaOH aqueous solution of 0.10mol/L, and this system being placed in temperature is that 120min is extracted in the water bath with thermostatic control concussion of 90 ° of C, filters to obtain the alkaline water extract of tea albumen; To in the alkaline water extract of tea albumen, adding 0.10mol/L salt acid for adjusting pH is 4.5 to precipitate, and centrifugal removing supernatant liquor, collecting precipitation, freeze-drying obtains tea albumen crude product 1025.8mg, and extraction yield is 10.26%, and purity is 53.56%.
(3) extracting and separating of trimethyl-xanthine
By gained supernatant liquor concentrated by rotary evaporation in (1) step to 1/3 of original volume, solid content is made to reach 1% ~ 5%, with isopyknic chloroform or methylene dichloride, abundant concussion extraction 1h, leaves standstill 1h, collects upper strata aqueous phase and lower floor's organic phase respectively, organic phase is again with isopyknic chloroform/methylene dichloride concussion extraction 1h, leave standstill 1h, again collect upper strata aqueous phase and lower floor's organic phase, merge aqueous phase and organic phase that twice extraction obtain respectively.Reclaim for subsequent use by the organic phase reduction vaporization removing chloroform after merging or methylene dichloride, the solid substance obtained adds 5mL distilled water washing twice, and lyophilize obtains 13.6mg trimethyl-xanthine, and extraction yield is 1.36%, and purity is 90%.
(4) extracting and separating of tea-polyphenol
Gained aqueous phase is concentrated into original volume 1/3 will be merged in (3) step, solid content is made to reach 1% ~ 5%, use isopyknic ethyl acetate, abundant concussion extraction 1h, leaves standstill 1h, collects upper organic phase and lower floor's aqueous phase respectively, organic phase is again with isopyknic extraction into ethyl acetate concussion extraction 1h, leave standstill 1h, again collect upper organic phase and lower floor's aqueous phase, merge aqueous phase and organic phase that twice extraction obtain respectively.Reclaim for subsequent use by the organic phase reduction vaporization removing ethyl acetate after merging, the solid substance obtained adds 5mL distilled water washing twice, and lyophilize obtains 1838.9mg tea-polyphenol, extraction yield 90.1%, and purity is 83.5%.
(5) precipitate and separate of tea polysaccharide and theanine
By merging gained aqueous phase concentrated by rotary evaporation in (4) step to 1/3 of original volume, making solid content reach 1% ~ 5%, with isopyknic 95% alcohol settling 2 times, centrifugally collecting supernatant liquor and precipitation respectively.Supernatant liquor freeze-drying, a small amount of water dissolution of solid substance, then use dehydrated alcohol in-20 ° of C recrystallizations 2 times, obtain 14.2mg theanine, extraction yield is 1.42%, purity 67.1%.Precipitation distilled water washing twice, lyophilize obtains 1446.2mg tea polysaccharide, total sugar content 68.5%, and extraction yield is 14.46%.
Embodiment 4:
(1) the weakly acidic water solution lixiviate of effective content of tea
By the tealeaves dedusting of oven dry, pulverizing, cross 60 ~ 80 mesh sieves.Get 1kg60 ~ 80 object tea powder, add the phosphate buffered saline buffer that 25L pH is 5.5, then this system is placed in the water bath with thermostatic control concussion extraction that temperature is 70 ° of C, after extracting 40min, collecting by filtration tea grounds add 25L pH be 5.5 phosphate buffered saline buffer extract 1 time again, collecting by filtration tea grounds is dry, merges the supernatant liquor extracted for 2 times for subsequent use.
(2) extraction of tea albumen
Get the tea grounds 500g collected in (1) step, adding 20L concentration by solid-to-liquid ratio 1:40 is in the alkaline NaOH aqueous solution of 0.10mol/L, and this system being placed in temperature is that 120min is extracted in the water bath with thermostatic control concussion of 90 ° of C, filters to obtain the alkaline water extract of tea albumen; To in the alkaline water extract of tea albumen, adding 0.10mol/L salt acid for adjusting pH is 4.5 to precipitate, and centrifugally removes supernatant liquor, collecting precipitation, and freeze-drying obtains tea albumen crude product 9.26g, and extraction yield is 9.26%, purity 50.28%.
(3) extracting and separating of trimethyl-xanthine
By the supernatant liquor concentrated by rotary evaporation of gained in (1) step to 1/3 of original volume, solid content is made to reach 1% ~ 5%, with isopyknic chloroform or methylene dichloride, abundant concussion extraction 1h, leaves standstill 1h, collects upper strata aqueous phase and lower floor's organic phase respectively, organic phase is again with isopyknic chloroform or methylene dichloride concussion extraction 1h, leave standstill 1h, again collect upper strata aqueous phase and lower floor's organic phase, merge aqueous phase and organic phase that twice extraction obtain respectively.Reclaim for subsequent use by the organic phase reduction vaporization removing chloroform/methylene dichloride after merging, the solid substance obtained adds 500mL distilled water washing twice, and lyophilize obtains 1.32g trimethyl-xanthine, and extraction yield is 1.32%, and purity is 90%.
(4) extracting and separating of tea-polyphenol
Gained aqueous phase concentrated by rotary evaporation will be merged to 1/3 of original volume in (3) step, solid content is made to reach 1% ~ 5%, use isopyknic ethyl acetate, abundant concussion extraction 1h, leaves standstill 1h, collects upper organic phase and lower floor's aqueous phase respectively, organic phase is again with isopyknic ethyl acetate concussion extraction 1h, leave standstill 1h, again collect upper organic phase and lower floor's aqueous phase, merge aqueous phase and organic phase that twice extraction obtain respectively.Reclaim for subsequent use by the organic phase reduction vaporization removing ethyl acetate after merging, the solid substance obtained adds 500mL distilled water washing twice, and lyophilize obtains 12.39g tea-polyphenol, extraction yield 60.1%, and purity is 81.52%.
(5) precipitate and separate of tea polysaccharide and theanine
By merging gained aqueous phase concentrated by rotary evaporation in (4) step to 1/3 of original volume, making solid content reach 1% ~ 5%, with isopyknic 95% alcohol settling 2 times, centrifugally collecting supernatant liquor and precipitation respectively.Supernatant liquor freeze-drying, a small amount of water dissolution of solid substance, then use dehydrated alcohol in-20 ° of C recrystallizations 2 times, obtain 1.41g theanine, extraction yield is 1.41%, purity 65.8%.Precipitation distilled water washing twice, lyophilize obtains 14.46g tea polysaccharide, and extraction yield is 14.46%, total sugar content 66.3%.
The method of effective constituent in a kind of comprehensive extraction tealeaves that the present invention proposes, be described by preferred embodiment, person skilled obviously can not depart from content of the present invention, spirit and scope method as herein described is changed or suitably change with combination realize the technology of the present invention.Special needs to be pointed out is, all similar replacements and change apparent to those skilled in the art, they are deemed to be included in spirit of the present invention, scope and content.
Claims (4)
1. the comprehensive method extracting effective constituent in tealeaves, is characterized in that step is as follows:
(1) the weakly acidic water solution lixiviate of effective content of tea
Tealeaves is crossed 60 ~ 80 mesh sieves, obtain tea powder, by tea powder: tea powder is placed in phosphate buffered saline buffer by phosphate buffered saline buffer=1:15 ~ 1:30 (g/mL) solid-to-liquid ratio, this system is placed in constant temperature, bath temperature is 50 DEG C ~ 80 DEG C and shakes extraction 30 ~ 60min, repeat to extract, collecting by filtration tea grounds, namely merging filtrate obtains effective content of tea Aqueous extracts; Phosphate buffered saline buffer pH is 5 ~ 6;
(2) extraction of tea albumen
Gained tea grounds in step (1) is dried, by tea grounds: tea grounds is placed in the alkaline NaOH aqueous solution by the solid-to-liquid ratio (g/mL) of alkali lye=1:20 ~ 1:40, and alkaline NaOH concentration of aqueous solution is 0.06 ~ 0.10mol/L; This system is placed in constant temperature, bath temperature is 70 DEG C ~ 90 DEG C, middle concussion extraction 60 ~ 120min, filter cleaner obtains the alkaline water extract of tea albumen; In the alkaline water extract of gained tea albumen, add hydrochloric acid, HCl concentration is 0.05mol/L ~ 0.10mol/L, regulates pH 4.5 to precipitate, and precipitation freeze-drying obtains the tea albumen crude product that purity is more than 50%;
(3) extracting and separating of trimethyl-xanthine
By gained effective content of tea Aqueous extracts in step (1), concentrated by rotary evaporation, to 1/3 of original volume, makes solid content reach 1% ~ 5%, adds isopyknic chloroform or methylene dichloride with concentrated solution; Concussion extraction trimethyl-xanthine under room temperature, fully after extraction, upper strata aqueous phase is separated with lower floor's organic phase, takes off a layer organic phase, and reduction vaporization reclaims organic solvent, and gained solid substance is multiple water-soluble, and freeze-drying obtains purity more than 85% trimethyl-xanthine;
(4) extracting and separating of tea-polyphenol
Isopyknic ethyl acetate is with it used to shake extraction under room temperature gained aqueous phase after extraction in step (3), after abundant extraction, upper organic phase is separated with lower layer of water, get upper organic phase, reduction vaporization reclaims ethyl acetate, gained solid substance is multiple water-soluble, and freeze-drying obtains the tea-polyphenol of purity more than 80%;
(5) precipitate and separate of tea polysaccharide and theanine
By gained aqueous phase after extraction in step (4), use isopyknic 95% alcohol settling with it, centrifugal collection supernatant liquor and precipitation respectively, precipitation freeze-drying obtains total sugar content more than 60% tea polysaccharide; By the freeze-drying of gained supernatant liquor, a small amount of water dissolution of solid substance, then uses dehydrated alcohol recrystallization repeatedly at low temperature-10 DEG C ~-20 DEG C, obtains the theanine of purity more than 65%.
2. the method for claim 1, is characterized in that repeating extraction time according to step (1) is 1 ~ 3 time, filters and collects tea grounds, merging filtrate, obtaining effective content of tea Aqueous extracts.
3. the method for claim 1, is characterized in that the condition of fully extraction in described step (3) or (4) is after extraction time 0.5h ~ 1h, leaves standstill abundant extraction time.
4. the method for claim 1, is characterized in that in step (5), alcohol settling number of times is 2 times.
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| CN110272354A (en) * | 2019-03-08 | 2019-09-24 | 贺州学院 | The technique of theanine is extracted from tea polyphenols waste liquid using foam separating technology |
| CN111358045B (en) * | 2020-03-13 | 2022-03-18 | 颐中（青岛）实业有限公司 | Black tea extract compound and application thereof |
| CN112858604A (en) * | 2021-01-06 | 2021-05-28 | 华润怡宝饮料（中国）有限公司 | Evaluation method of tea extraction end point |
| CN113190066B (en) * | 2021-04-29 | 2022-04-01 | 广西河丰药业有限责任公司 | High-purity EGCG automatic extraction system based on Internet of things |
| CN116235894A (en) * | 2023-03-02 | 2023-06-09 | 大闽食品（漳州）有限公司 | Preparation method and application of tea dreg protein |
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