CN109221530A - A kind of gamma-aminobutyric acid in tea leaves extraction and purification process - Google Patents

A kind of gamma-aminobutyric acid in tea leaves extraction and purification process Download PDF

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Publication number
CN109221530A
CN109221530A CN201811219488.1A CN201811219488A CN109221530A CN 109221530 A CN109221530 A CN 109221530A CN 201811219488 A CN201811219488 A CN 201811219488A CN 109221530 A CN109221530 A CN 109221530A
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aminobutyric acid
tea
water
gamma
extraction
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石影
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Guizhou Qianxin Maoyuan Agricultural Development Co Ltd
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Guizhou Qianxin Maoyuan Agricultural Development Co Ltd
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23FCOFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
    • A23F3/00Tea; Tea substitutes; Preparations thereof
    • A23F3/16Tea extraction; Tea extracts; Treating tea extract; Making instant tea
    • A23F3/18Extraction of water soluble tea constituents

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)

Abstract

The present invention provides a kind of gamma-aminobutyric acid in tea leaves extraction and purification process, specific method is the following steps are included: 1) pretreatment of raw material process;2) process of extraction with ultrasonic-NaOH γ-aminobutyric acid is utilized;3) γ-aminobutyric acid crude extract concentration process;4) γ-aminobutyric acid concentrate isolates and purifies process;5) process γ-aminobutyric acid drying and saved.Beneficial effect of the present invention: the present invention uses the low-grade tea such as Summer-autumn tea for raw material, using low frequency cycle ultrasonic technique assisted extraction γ-aminobutyric acid, the method γ-aminobutyric acid recovery rate is high, purity is high, method is at low cost, simple and easy, easy to spread, the color of gained tea protein product is green tea color, and product quality meets food hygienic standard.The present invention provides the new ways that summer and autumn low grade tea increment conversion recycles;A kind of novel plant source γ-aminobutyric acid new product is developed, tea resources comprehensive utilization and intensive processing are realized.

Description

A kind of gamma-aminobutyric acid in tea leaves extraction and purification process
Technical field
The present invention relates to the development and utilization field of plant product, mainly a kind of gamma-aminobutyric acid in tea leaves and extraction are pure Chemical industry skill.
Background technique
Tealeaves originates from China, is one of beverage most popular in the world, while tea industry is also the traditional excellent of China Gesture industry.Tealeaves is just to be become until the Western Jin Dynasty by as sacrificial offerings and popularized civil common beverages, have so far earliest More than 6000 years history.Contain the multiple functions such as tea polyphenols, tea albumen, tea polysaccharide, caffeine and γ-aminobutyric acid in tealeaves Property ingredient, they all have good medical value and health-care effect.So far, both at home and abroad to the several functions in tealeaves The existing many researchs of ingredient.China's tea yield is abundant, and tealeaves total output reaches 233.5 ten thousand tons or so within 2016, wherein in Low-grade tea accounts for very big specific gravity, serious unsalable on the market, while a large amount of Summer-autumn tea is unutilized, or even is discarded, these are existing As all to China's tea industry development and tea resources utilization cause very big influence, therefore, to tealeaves carry out deep processing The research and application of novel technique are to improve tea resources utilization rate and China's tea industry is kept quickly to send out in international market The urgent need of exhibition is the only way that traditional tea industry extends to industries such as food, medicine, is the weight for extending Tea Industry chain Want means.
China's tea resources are abundant, and tea industry is quickly grown, but spring tea is usually only picked in tea place, and a large amount of Summer-autumn tea is not It is utilized, or even is discarded, this causes great waste to tea resources.Contain γ-aminobutyric acid and tea albumen in tealeaves Etc. several functions compositions, have good health-care effect, the use to these ingredients in tealeaves can be such that tea resources are had Effect utilizes.
γ-aminobutyric acid is a kind of crystalline powder white or yellowish, and hygroscopicity is strong, is highly soluble in water, is slightly soluble in heat Ethyl alcohol, insoluble in organic solvents such as benzene, cold ethyl alcohol, ether, micro- smelly, no optical activity is polar substances, fusing point 203-205 DEG C, relative molecular mass 103.12, molecular formula C4H9NO2, the dissociation constant of γ-aminobutyric acid: pKCOOH=4.03, pKNH3= 10.56.γ-aminobutyric acid usually exists as zwitterions in aqueous solution, and dissociation situation depends primarily on The size of pH value, isoelectric point 7.295.γ-aminobutyric acid is a kind of nonprotein amino acid, certain spies with amino acid Hydrocarbyl reaction, acylation reaction, ninhydrin chromogenic reaction etc. can occur for different chemical property.
In recent years, concern of the γ-aminobutyric acid as a kind of novel foodstuff function factor, by more and more people.It is existing The study found that γ-aminobutyric acid can enhance neuron membrane to Na+Permeability, make cell membrane hyperpolarization, can increase movement electricity The starting threshold value of position, so, γ-aminobutyric acid is a kind of important inhibiting nerve in people and mammalian nervous cental system Mediator can participate in a variety of metabolic activities in organism, have a very strong physiological activity, its production and application just becoming food, The hot research direction of the fields such as Medical Animal feed and agricultural concern.The physiological function of γ-aminobutyric acid mainly has following several Point.
A adjusts cardiovascular function
γ-aminobutyric acid has cardiovascular activity to adjust well and make as inhibitory transmitter important in central nervous system With being mainly shown as and adjust heart rate, blood pressure lowering and hypoglycemic etc..γ-aminobutyric acid has certain pharmacology in terms of blood pressure lowering Effect, reason may be in the cerebrovascular there are specific neuroceptor can with γ-aminobutyric acid ining conjunction with, when the neuroceptor and When γ-aminobutyric acid combines, it can achieve the purpose that reduce blood pressure.Mao Zhifang etc. has found spontaneous hypertension by test Green tea of the rat long-term drinking containing γ-aminobutyric acid can be such that blood pressure is decreased obviously.Kazami and Inoue K has been found that, if high blood Patient is pressed continuously to eat the food containing γ-aminobutyric acid, then blood pressure decreased significantly;But normotensive people continuously eats Afterwards, blood pressure will not change, and will not influence other indexs of body, without any side effects.γ-aminobutyric acid can also pass through resistance Disconnected sympathetic modulation vasomotor center, so that blood vessel dilatation, to achieve the purpose that blood pressure lowering.Gabanergic is logical The activity for inhibiting Angiotensin-Converting and antidiuretic hormone vasopressins is crossed, the effect of blood pressure lowering is played.Gamma-amino fourth Acid can also inhibit the activity of glutamate decarboxylase, effectively prevent the progress of glutamic acid decarboxylase, so that Blood Ammonia Concentration declines, protect Demonstrate,prove human health;Meanwhile γ-aminobutyric acid also can promote the glutamic acid in blood to generate urea in conjunction with ammonia, to effectively solve Except internal ammonia poison, promote liver kidney function.
B treats epilepsy
It is reported that the epileptic in China has reached 9,000,000 or so, epilepsy invasion reason multiplicity, mechanism is complicated, with maincenter mind There is substantial connection through mediator.Currently, epilepsy has become the second largest common disease in China, the work and life of people is drastically influenced. And γ-aminobutyric acid is as inhibitory neurotransmitter important in human body, to diseases such as treatment epilepsy, insomnia, parkinsonisms Disease has improvement result.There is two amino acid of excitatory amino acid and inhibitory aminoacid in central nervous system, if excitability Amino acid content is too high, then neural inhibiting effect will decline, and may cause the generation of epilepsy.It is many study found that work as γ-ammonia When base butyric acid lacks, it will lead to neuron and be overexcited, and have single-minded binding site in central nervous system, with the position The combination of point can increase neu to Cl-Permeability so that cell membrane potential be in resting potential level, so as to subtract Reaction of the weak cynapse to excitement input.So Gabanergic improves the anticonvulsion threshold value of human body, intractable can be effectively treated Epilepsy.The discoveries such as Okada pass through the oral rice plumule food containing γ-aminobutyric acid, γ-aminobutyric acid can promote sleep, Calm nerve, resistance anxiety etc., and facilitate the improvement of old initial stage phrenoblabia and women's climacteric syndrome symptom, together When research discovery cerebrospinal fluid in the negatively correlated property of the severity of alpha-aminobutyric acid content and epileptic, and γ-aminobutyric acid Content is relatively low.So epilepsy can be treated by directly increasing the content of γ-aminobutyric acid in cerebrospinal fluid.The study found that when big When brain severe ischemic, γ-aminobutyric acid can also reduce the nervous excitement as caused by glutamic acid, to subtract to nerve cell Few damage.In addition, γ-aminobutyric acid also has certain effect to stiff people's disease and Parkinson's disease is treated.
C promotes hormone secretion
γ-aminobutyric acid is to a variety of hormones such as growth hormone, somatomedin, thyroid hormone and sex hormone in endocrine system Secretion have adjustment effect, the metaboilic level of human body can be effectively improved.γ-aminobutyric acid can directly stimulate body secretes institute Hormone is needed, compared with directly taking exogenous hormone, there is higher safety.Studies have shown that γ-aminobutyric acid can pass through suppression The excitement of certain nerves in hypothalamus processed and the secretion for adjusting promoting sexual gland hormone.
D improves hepatic and renal function
γ-aminobutyric acid other than reducing blood ammonia, also has diuresis in addition to that can inhibit the decarboxylation of glutamic acid, so that extra in vivo Salinity discharge, is effectively relieved liver kidney pressure.Existing research shows that γ-aminobutyric acid can activate renal function.Meanwhile gamma-amino Butyric acid can also inhibit alkaline phosphatase activities, and an important indicator for evaluating liver function reactivity is exactly the work of alkaline phosphatase Property size.
E other function
In addition, γ-aminobutyric acid also has pre- preventing obesity, promotes lipid-metabolism, prevent vascular sclerosis, repair skin, delay to decline It waits for a long time physiological function.Clinically, γ-aminobutyric acid can also treat uremia, the illnesss such as anthracemia.In addition, γ-ammonia Base butyric acid also has desinsection, smelly eliminating and other effects.
Therefore, γ-aminobutyric acid is powerful, has to have and is mass produced by succinct easy mode, promotes the well-being of mankind.
Summary of the invention
The purpose of the present invention is provide for shortcoming present in the comprehensive utilization techniques such as low-grade tea, tea grounds now A kind of gamma-aminobutyric acid in tea leaves extraction and purification process, this extracts wherein γ-aminobutyric acid using ultrasound assisted extraction technology Method and process is simple, and production cost is low, and γ-aminobutyric acid recovery rate is high.
It is another object of the present invention to provide a kind of γ-aminobutyric acid extracts prepared using the above method, should Product alpha-aminobutyric acid content is 70-80%, and amino acid content is abundant, and composition compares balance.
The technical scheme adopted by the invention to solve the technical problem: this gamma-aminobutyric acid in tea leaves and extraction purification work Skill, this method including the following steps:
(1) pretreatment of raw material process: cleaning removal of impurities dephenolize is carried out using tealeaves as raw material, is crushed after water-removing drying spare;
(2) γ-aminobutyric acid leaching process: low frequency ultrasound assists alkali carries, and γ-aminobutyric acid extracting solution, detailed process is made are as follows: It weighs a certain amount of tea powder to be placed in conical flask, be shaken up after a certain amount of ultrapure water is added according to liquid-to-solid ratio 20:1 mL/g, in temperature It is 50 DEG C, is centrifuged after 30 min of ultrasound extraction are cooling under the conditions of power is 220 W, filters, it is thick to obtain γ-aminobutyric acid Extract;
(3) γ-aminobutyric acid concentration process: γ-aminobutyric acid crude extract being concentrated with Rotary Evaporators, needed for adding water to be configured to Sample liquid concentration.;
(4) γ-aminobutyric acid concentrate isolates and purifies process: can be used Static Adsorption or dynamic desorption separate it is pure Change;
(5) process γ-aminobutyric acid drying and saved;
Preferably: fresh leaf is cleaned and is dried to water content about 80% by step (1) pretreatment of raw material process, respectively by fresh leaf- 16 h are handled under the conditions of 18 DEG C, then with micro-wave oven water-removing 2-3 min(using medium and high quality, every 30 s turns over even primary), then It is put into air dry oven and is dried to over dry at 80 DEG C, crushed 80 meshes.
Preferably: step (1) pretreatment of raw material process is also possible to clean fresh leaf and dry to water content about 80%, sets 2 h of Anaerobic Treatment is carried out to it at 0.085 MPa of vacuum degree and 30 DEG C of temperature in vacuum oven, then in air In spread 1 h, so recycle 4 times respectively, later with micro-wave oven water-removing 2-3 min(using medium-to-high grade, every 30 s turns over even Once), it is then put in air dry oven and is dried to over dry under the conditions of 80 DEG C, crushed 80 meshes.
Preferably: step (2) is to tea gamma-aminobutyric acid leaching process are as follows: and it weighs a certain amount of tea powder and is placed in conical flask, It is shaken up after a certain amount of ultrapure water is added according to liquid-to-solid ratio 20:1 mL/g, is 50 DEG C in temperature, under the conditions of power is 220 W It is centrifuged after 30 min of ultrasound extraction are cooling, filters, obtain γ-aminobutyric acid crude extract.
Preferably: the process that γ-aminobutyric acid extracting solution is concentrated in step (3) are as follows: using vacuum concentration or rotation Turn to be concentrated by evaporation, temperature concentrated in vacuo is controlled at 40-60 DEG C, is concentrated into the 20-50% of original volume.Rotary evaporation concentration time is 2h。
Preferably: Static Adsorption in step (4) specifically: the resin of certain volume is added 95% ethyl alcohol and impregnates 24 h, It is washed with water to no floccule and without ethanol flavor;Then 5 h are impregnated with 4% NaOH, be washed with water to neutrality, then with 5% HCl 8 h are impregnated, are washed with water to neutrality;Dynamic Adsorption elution process are as follows: loading flow velocity 3mL/min, 0.2 mg/mL of sample concentration, Eluent pH=9,2 mL/min of elution flow rate.With this condition, the retention rate of γ-aminobutyric acid is 80.06%, γ-ammonia The purity of base butyric acid reaches 78.51%.
Preferably: kept dry process of the step (5) to γ-aminobutyric acid are as follows: heavy to above-mentioned resulting γ-aminobutyric acid The pure water of 20~60 times of Sediment weights is added in shallow lake, washs 6~8 times at room temperature, 5000-11000r/min centrifuge separation 30min obtains γ-aminobutyric acid, and the pure water of 5~15 times of weight, agitated adjusting pH to neutrality, after colloid mill and is added Matter machine is spray-dried or is freeze-dried and to obtain γ-aminobutyric acid product.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, below with reference to citing, to the present invention into Row is further described.It should be appreciated that citing described herein is only used to explain the present invention, it is not used to limit this hair It is bright.
(1) pretreatment of raw material process: cleaning removal of impurities dephenolize is carried out using tealeaves as raw material, is crushed after water-removing drying spare; Fresh leaf is cleaned and is dried to water content about 80%, respectively fresh leaf 16 h is handled under the conditions of -18 DEG C, is then killed with micro-wave oven Using medium and high quality, every 30 s turns over even primary green 2-3 min(), it is then placed in air dry oven and is dried at 80 DEG C absolutely It is dry, it crushed 80 meshes.Or fresh leaf is cleaned and is dried to water content about 80%, respectively by fresh leaf under the conditions of -18 DEG C 16 h are handled, then with micro-wave oven water-removing 2-3 min(using medium and high quality, every 30 s turns over even primary), it is dry to be then placed in air blast It is dried to over dry at 80 DEG C in dry case, crushed 80 meshes.
(2) γ-aminobutyric acid leaching process: low frequency ultrasound assists alkali carries, and γ-aminobutyric acid extracting solution, specific mistake is made Journey are as follows: it weighs a certain amount of tea powder and is placed in conical flask, shaken up after a certain amount of ultrapure water is added according to liquid-to-solid ratio 20:1 mL/g, Temperature is 50 DEG C, is centrifuged after 30 min of ultrasound extraction are cooling under the conditions of power is 220 W, filters, obtain gamma-amino fourth Sour crude extract;
(3) γ-aminobutyric acid concentration process: γ-aminobutyric acid crude extract being concentrated with Rotary Evaporators, needed for adding water to be configured to Sample liquid concentration.It is controlled using vacuum concentration or rotary evaporation concentration, temperature concentrated in vacuo at 40-60 DEG C, is concentrated into substance Long-pending 20-50%.Rotary evaporation concentration time is 2h
(4) γ-aminobutyric acid concentrate isolates and purifies process: can be used Static Adsorption or dynamic desorption separate it is pure Change;Middle Static Adsorption specifically: the resin of certain volume is added 95% ethyl alcohol and impregnates 24 h, is washed with water to no floccule and nothing Ethanol flavor;Then 5 h are impregnated with 4% NaOH, be washed with water to neutrality, then impregnate 8 h with 5% HCl, be washed with water into Property;Dynamic Adsorption elution process are as follows: loading flow velocity 3mL/min, 0.2 mg/mL of sample concentration, eluent pH=9, elution stream 2 mL/min of speed.With this condition, the retention rate of γ-aminobutyric acid is 80.06%, and the purity of γ-aminobutyric acid reaches 78.51%。
(5) process γ-aminobutyric acid drying and saved;It is added 20 into above-mentioned resulting γ-aminobutyric acid precipitating~ The pure water of 60 times of Sediment weights washs 6~8 times at room temperature, and 5000-11000r/min is centrifugated 30min, obtains gamma-amino Butyric acid, is added the pure water of 5~15 times of weight, agitated adjustings pH to neutrality, after colloid mill and homogenizer, be spray-dried or It is freeze-dried to obtain γ-aminobutyric acid product.
The γ-aminobutyric acid obtained by this method is not only with high purity, and prototroph substance also saves more completely, is suitble to big Area is promoted.

Claims (7)

1. a kind of gamma-aminobutyric acid in tea leaves extraction and purification process, it is characterized in that: this method including the following steps:
(1) pretreatment of raw material process: cleaning removal of impurities dephenolize is carried out using tealeaves as raw material, is crushed after water-removing drying spare;
(2) γ-aminobutyric acid leaching process: low frequency ultrasound assists alkali carries, and γ-aminobutyric acid extracting solution, detailed process is made are as follows: It weighs a certain amount of tea powder to be placed in conical flask, be shaken up after a certain amount of ultrapure water is added according to liquid-to-solid ratio 20:1 mL/g, in temperature It is 50 DEG C, is centrifuged after 30 min of ultrasound extraction are cooling under the conditions of power is 220 W, filters, it is thick to obtain γ-aminobutyric acid Extract;
(3) γ-aminobutyric acid concentration process: γ-aminobutyric acid crude extract being concentrated with Rotary Evaporators, needed for adding water to be configured to Sample liquid concentration;
(4) γ-aminobutyric acid concentrate isolates and purifies process: can be used Static Adsorption or dynamic desorption separate it is pure Change;
(5) process γ-aminobutyric acid drying and saved.
2. gamma-aminobutyric acid in tea leaves extraction and purification process according to claim 1, it is characterised in that: step (1) raw material Fresh leaf is cleaned and is dried to water content about 80%, fresh leaf handled 16 h under the conditions of -18 DEG C respectively, so by preprocessing process Afterwards with micro-wave oven water-removing 2-3 min(using medium and high quality, every 30 s turns over even primary), it is then placed in air dry oven 80 It is dried to over dry at DEG C, crushed 80 meshes.
3. gamma-aminobutyric acid in tea leaves extraction and purification process according to claim 1, it is characterised in that: step (1) raw material Preprocessing process is also possible to clean fresh leaf and dry to water content about 80%, is placed in vacuum oven in vacuum degree 0.085 2 h of Anaerobic Treatment is carried out to it at MPa and 30 DEG C of temperature, then spreads 1 h in air, is so recycled 4 times respectively, Later with micro-wave oven water-removing 2-3 min(using medium and high quality, every 30 s turns over even primary), it is then put in 80 in air dry oven It is dried to over dry under the conditions of DEG C, crushed 80 meshes.
4. gamma-aminobutyric acid in tea leaves extraction and purification process according to claim 1, it is characterised in that: step (2) is to tea Leaf γ-aminobutyric acid leaching process are as follows: weigh a certain amount of tea powder and be placed in conical flask, be added one according to liquid-to-solid ratio 20:1 mL/g Shaken up after quantitative ultrapure water, be 50 DEG C in temperature, after 30 min of ultrasound extraction are cooling under the conditions of power is 220 W from The heart filters, obtains γ-aminobutyric acid crude extract.
5. gamma-aminobutyric acid in tea leaves extraction and purification process according to claim 1, it is characterised in that: step (3) is right The process that γ-aminobutyric acid extracting solution is concentrated are as follows: using vacuum concentration or rotary evaporation concentration, temperature concentrated in vacuo control System is concentrated into the 20-50% of original volume at 40-60 DEG C,
Rotary evaporation concentration time is 2h.
6. gamma-aminobutyric acid in tea leaves extraction and purification process according to claim 1, it is characterised in that: quiet in step (4) State absorption specifically: the resin of certain volume is added 95% ethyl alcohol and impregnates 24 h, is washed with water to no floccule and without ethanol flavor; Then 5 h are impregnated with 4% NaOH, be washed with water to neutrality, then impregnate 8 h with 5% HCl, be washed with water to neutrality;Dynamic is inhaled Attached elution process are as follows: loading flow velocity 3mL/min, 0.2 mg/mL of sample concentration, eluent pH=9,2 mL/ of elution flow rate Min,
With this condition, the retention rate of γ-aminobutyric acid is 80.06%, and the purity of γ-aminobutyric acid reaches 78.51%.
7. gamma-aminobutyric acid in tea leaves extraction and purification process according to claim 1, it is characterised in that: step (5) is right The kept dry process of γ-aminobutyric acid are as follows: 20~60 times of Sediment weights are added into above-mentioned resulting γ-aminobutyric acid precipitating Pure water, wash 6~8 times at room temperature, 5000-11000r/min is centrifugated 30min, obtains γ-aminobutyric acid, be added 5~ The pure water of 15 times of weight, agitated adjusting pH to neutrality are spray-dried or are freeze-dried after colloid mill and homogenizer γ-aminobutyric acid product.
CN201811219488.1A 2018-10-19 2018-10-19 A kind of gamma-aminobutyric acid in tea leaves extraction and purification process Pending CN109221530A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113350557A (en) * 2020-03-06 2021-09-07 李彤 Multipurpose aromatherapy liquid
CN114343064A (en) * 2021-12-10 2022-04-15 上海吉吉白泽宠物有限公司 SL-RSR pet snack formula capable of relieving stress response and production process
CN115477592A (en) * 2022-09-30 2022-12-16 西安萃源生物科技有限公司 Crystallization method of gamma-aminobutyric acid

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113350557A (en) * 2020-03-06 2021-09-07 李彤 Multipurpose aromatherapy liquid
CN114343064A (en) * 2021-12-10 2022-04-15 上海吉吉白泽宠物有限公司 SL-RSR pet snack formula capable of relieving stress response and production process
CN115477592A (en) * 2022-09-30 2022-12-16 西安萃源生物科技有限公司 Crystallization method of gamma-aminobutyric acid

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