CN108640848A - The extracting method of γ-aminobutyric acid in a kind of seawater rice plumule - Google Patents
The extracting method of γ-aminobutyric acid in a kind of seawater rice plumule Download PDFInfo
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- CN108640848A CN108640848A CN201810493571.1A CN201810493571A CN108640848A CN 108640848 A CN108640848 A CN 108640848A CN 201810493571 A CN201810493571 A CN 201810493571A CN 108640848 A CN108640848 A CN 108640848A
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- aminobutyric acid
- extracting method
- seawater rice
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
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Abstract
The present invention relates to gamma aminobutyric acid extractive technique fields, specially a kind of method that external condition stimulation strengthening extraction method extracts gamma aminobutyric acid from seawater rice plumule, including pretreatment, extraction, purifying, ultrafiltration, concentration, decoloration and drying, in extraction process, strengthened using the methods of vacuum nitrogen, infrared radiation, ultrasonic wave and microwave radiation technology;In the extraction process of gamma aminobutyric acid, gamma aminobutyric acid activity is improved using environmental stimuli, and then improve extraction efficiency, by vacuum nitrogen, infrared radiation, ultrasonic wave and microwave reinforced, gamma aminobutyric acid purity can be improved in finished product to 60% or more;This preparation method simplifies technological process, reduces production cost, and gamma aminobutyric acid purity obtained is high.
Description
Technical field
The present invention relates to γ-aminobutyric acid extractive technique field, γ-aminobutyric acid in specially a kind of seawater rice plumule
Extracting method.
Background technology
γ-aminobutyric acid, English name:γ-aminobutyric acid (GABA) γ-aminobutyric acid, chemical name:4-
Aminobutyric acid, alias:γ-aminobutyric acid, amino acid injection-800, nipecotic acid.Molecular formula:C4H9NO2.Molecular weight:103.1.It is widely distributed
In in animal and plant body.All contain GABA in plant such as Macroptilium, ginseng category, the seed of Chinese herbal medicine, rhizome and tissue fluid.In animal body
Interior, GABA is almost existed only in nerve fiber, and the content in mesencephalic tissue is about 0.1-0.6mg/ grams of tissue, immunology
Studies have shown that the highest region of its concentration is black substance in brain.GABA is a kind of more deep important inhibition of current research
Nerve mediator, it participates in a variety of metabolic activities, has very high physiological activity.
Chinese patent library discloses a kind of method of glutamic acid biology solid phase Enzyme catalyzed synthesis γ-aminobutyric acid
(CN201210171987.4), include the following steps:(1) substrate glutamic acid solution and solid phase Enzyme catalyzed synthesis are generated into γ-ammonia
Base butyric acid solution, then by filtering or centrifuging biological immobilized enzyme and reaction solution;(2) γ-aminobutyric acid aqueous solution activated carbon
After decoloration, vacuum film is concentrated to give γ-aminobutyric acid concentrated solution;(3) 95% alcohol is added in γ-aminobutyric acid concentrated solution, is precipitated
γ-aminobutyric acid white precipitate crystallizes, and centrifuges, is dried in vacuo to obtain white γ-aminobutyric acid powder.The technological reaction is special
One, yield is high, purity is good, the period is short, low energy consumption, is suitble to industrialized production.
Chinese patent library discloses a kind of method (CN201210304596.5) of bioanalysis preparation γ-aminobutyric acid, packet
Thalline is included to prepare, production γ-aminobutyric acid, decoloration, electrodialysis, γ-aminobutyric acid powder product or γ-aminobutyric acid crystalline substance is made
Body product and etc..The present invention synthesizes γ-aminobutyric acid using free lactic acid bacterium cell catalysis, and improves production technology, makes γ-
Aminobutyric acid output increased, cost reduction, but also establish the method for preparing high-purity γ-aminobutyric acid.It is anti-in this technique
It answers and cultivates ingredient without containing carbon source, nitrogen source etc. in system, reaction solution ingredient is simple for zymotic fluid, can increase substantially
Product purity, while having many advantages, such as that simple, the with short production cycle and environmental pollution of post-processing is small, at low cost.
Seawater rice achieves huge success in China, the extra large rice not only ordinary nutritional ingredient containing cereal crops, and
And as a kind of crop grown under special marine environment, also contain the special bioactive substance different from common rice,
Including:Lipase inhibitor (pancreatic lipase inhibitor, PLI), phospho phytate (IP6), gamma-amino fourth
How sour (GABA), glutathione (GSH) etc., efficiently extract the active ingredient in going to sea rice, and further investigation is made.
Invention content
Technical problem to be solved by the invention is to provide a kind of external conditions to stimulate strengthening extraction method from seawater rice plumule
The method of middle extraction γ-aminobutyric acid, simplifies preparation process, and γ-aminobutyric acid purity obtained is high.
To achieve the goals above, the present invention uses following technical scheme
The extracting method of γ-aminobutyric acid, includes the following steps in a kind of seawater rice plumule:
A extra large aid from rice germ powder) is prepared:
(1) plumule is tamed, selected seawater rice, and is soaked in domestication liquid;
(2) vernalization is placed in vernalization in germinator, is used in pregermination procedure and use electric field-enhanced vernalization, floated with water after germination
Wash clean;
(3) it crushes, seawater rice plumule is dried, ultramicro grinding is carried out to dry plumule;
B γ-aminobutyric acid) is extracted:
(1) it pre-processes, germ flour is placed in retort, vacuum produces nitrogen 3-6h;
(2) it extracts, water is added, germ flour and water solid-liquid ratio 1: 2-1: 4 in terms of bulking value add citric acid, plumule
Powder and citric acid solid-liquid ratio 1: 2-1: 3 in terms of bulking value, are eventually adding the glutamic acid of the 0.1%-0.5% of germ flour weight,
35-45 DEG C of temperature, pH5-6, reaction time 4-6h in reaction process, are assisted using ultrasonic wave;
(3) it purifies, supernatant is extracted after the completion of reaction, the ethanol solution of 70-85% concentration is added, supernatant is molten with ethyl alcohol
The weight ratio of liquid is 2:2-3, refluxing extraction 1-1.5h at a temperature of 60-75 DEG C;Extraction 15-30min is centrifuged again, is extracted later
Supernatant;
(4) ultrafiltration carries out ultrafiltration using 50 nanometers of ultrafiltration membranes under 0.3MPa pressure;
(5) it concentrates, concentration is evaporated to ultrafiltration permeate, is concentrated into the 1/10-1/20 of permeate volume;
(6) it decolourizes, decolourizes as needed in concentration process;
(7) dry, it is dried using spray drying process and γ-aminobutyric acid pulvis is made.
Preferably, step A) in, electric field-enhanced condition:Electric field strength 30-50kV/cm, burst length 500-600 μ s, arteries and veins
Rush frequency 100-300Hz.
Preferably, step A) in, it is dried using micro-wave drying method, microwave drying condition is:Frequency 3000-
4000MHz, power 3000W, 50-60 DEG C of temperature.
Preferably, step A) in, ultra micro grain size of micropowder obtained is less than 10 μm.
Preferably, step B) in, when pretreatment, 3h is handled using infrared radiation, was irradiated 1 minute every 1 minute.
Preferably, step B) in, intensified by ultrasonic wave, power 400-800W, frequency 50-100KHz work half a minute, interval
Half a minute.
Preferably, step B) in, using microwave reinforced when purifying.
Preferably, microwave frequency 105HZ-107HZ。
Preferably, step B) in, it is decolourized using absorption resin.
Preferably, step B) in, γ-aminobutyric acid pulvis water content obtained is less than 8%, and γ-aminobutyric acid purity is big
In 60%.
Beneficial effects of the present invention:In the extraction process of γ-aminobutyric acid, gamma-amino fourth is improved using environmental stimuli
Acid activity, and then extraction efficiency is improved, by vacuum nitrogen, infrared radiation, ultrasonic wave and microwave reinforced, can be improved in finished product
γ-aminobutyric acid purity is to 60% or more;This preparation method simplifies technological process, reduces production cost, γ-ammonia obtained
Base butyric acid purity is high.
Specific implementation mode
Below in conjunction with the embodiment of the present invention, technical solution in the embodiment of the present invention is clearly and completely retouched
It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention
In embodiment, all other implementation that those of ordinary skill in the art are obtained without creative efforts
Example, shall fall within the protection scope of the present invention.
Embodiment 1
The extracting method of γ-aminobutyric acid, includes the following steps in a kind of seawater rice plumule:
A extra large aid from rice germ powder) is prepared:
(1) plumule is tamed, selected seawater rice, and is soaked in domestication liquid;
(2) vernalization is placed in vernalization in germinator, is used in pregermination procedure and use electric field-enhanced vernalization, floated with water after germination
Wash clean;Electric field-enhanced condition:Electric field strength 30kV/cm, 500 μ s of burst length, pulse frequency 100Hz;
(3) it crushes, seawater rice plumule is dried using micro-wave drying method, ultramicro grinding is carried out to dry plumule;
Microwave drying condition is:Frequency 3000MHz, power 3000W, temperature 50 C;
B γ-aminobutyric acid) is extracted:
(1) it pre-processes, germ flour is placed in retort, vacuum produces nitrogen 3h;3h is handled using infrared radiation simultaneously,
It was irradiated 1 minute every 1 minute;
(2) extract, water be added, germ flour and water solid-liquid ratio 1: 2 in terms of bulking value add citric acid, germ flour and
Citric acid solid-liquid ratio 1: 2 in terms of bulking value, is eventually adding 0.2% glutamic acid of germ flour weight, 35 DEG C of temperature, pH5, anti-
4h between seasonable in reaction process, is assisted using ultrasonic wave;Intensified by ultrasonic wave condition, power 400W, frequency 50KHz, work half point
Clock is spaced half a minute;
(3) it purifies, supernatant is extracted after the completion of reaction, the ethanol solution of 75% concentration, supernatant and ethanol solution is added
Weight ratio be 1:1, refluxing extraction 1h at a temperature of 65 DEG C;Extraction 15min is centrifuged again, extracts supernatant later;It purified
Microwave reinforced, microwave frequency 10 is used in journey5HZHZ;
(4) ultrafiltration carries out ultrafiltration using 50 nanometers of ultrafiltration membranes under 0.3MPa pressure;
(5) it concentrates, concentration is evaporated to ultrafiltration permeate, is concentrated into the 1/10 of permeate volume;
(6) it decolourizes, is decolourized using absorption resin in concentration process;
(7) dry, it is dried using spray drying process and γ-aminobutyric acid pulvis is made.
Embodiment 2
The extracting method of γ-aminobutyric acid, includes the following steps in a kind of seawater rice plumule:
A extra large aid from rice germ powder) is prepared:
(1) plumule is tamed, selected seawater rice, and is soaked in domestication liquid;
(2) vernalization is placed in vernalization in germinator, is used in pregermination procedure and use electric field-enhanced vernalization, floated with water after germination
Wash clean;Electric field-enhanced condition:Electric field strength 40kV/cm, 550 μ s of burst length, pulse frequency 200Hz;
(3) it crushes, seawater rice plumule is dried using micro-wave drying method, ultramicro grinding is carried out to dry plumule;
Microwave drying condition is:Frequency 3500MHz, power 3000W, 55 DEG C of temperature;
B γ-aminobutyric acid) is extracted:
(1) it pre-processes, germ flour is placed in retort, vacuum produces nitrogen 4h;3h is handled using infrared radiation simultaneously,
It was irradiated 1 minute every 1 minute;
(2) extract, water be added, germ flour and water solid-liquid ratio 1: 3 in terms of bulking value add citric acid, germ flour and
Citric acid solid-liquid ratio 1: 3 in terms of bulking value, is eventually adding 0.3% glutamic acid of germ flour weight, 40 DEG C of temperature, pH5.5,
Reaction time 5h in reaction process, is assisted using ultrasonic wave;Intensified by ultrasonic wave condition, power 600W, frequency 80KHz, work half
Minute, it is spaced half a minute;
(3) it purifies, supernatant is extracted after the completion of reaction, the ethanol solution of 70-85% concentration is added, supernatant is molten with ethyl alcohol
The weight ratio of liquid is 2:3, refluxing extraction 1h at a temperature of 70 DEG C;Extraction 20min is centrifuged again, extracts supernatant later;Purifying
Microwave reinforced, microwave frequency 10 is used in the process6HZ;
(4) ultrafiltration carries out ultrafiltration using 50 nanometers of ultrafiltration membranes under 0.3MPa pressure;
(5) it concentrates, concentration is evaporated to ultrafiltration permeate, is concentrated into the 1/15 of permeate volume;
(6) it decolourizes, is decolourized using bamboo charcoal in concentration process;
(7) dry, it is dried using spray drying process and γ-aminobutyric acid pulvis is made.
Embodiment 3
The extracting method of γ-aminobutyric acid, includes the following steps in a kind of seawater rice plumule:
A extra large aid from rice germ powder) is prepared:
(1) plumule is tamed, selected seawater rice, and is soaked in domestication liquid;
(2) vernalization is placed in vernalization in germinator, is used in pregermination procedure and use electric field-enhanced vernalization, floated with water after germination
Wash clean;Electric field-enhanced condition:Electric field strength 50kV/cm, 600 μ s of burst length, pulse frequency 300Hz;
(3) it crushes, seawater rice plumule is dried using micro-wave drying method, ultramicro grinding is carried out to dry plumule;
Microwave drying condition is:Frequency 4000MHz, power 3000W, temperature 60 C;
B γ-aminobutyric acid) is extracted:
(1) it pre-processes, germ flour is placed in retort, vacuum produces nitrogen 6h;3h is handled using infrared radiation simultaneously,
It was irradiated 1 minute every 1 minute;
(2) extract, water be added, germ flour and water solid-liquid ratio 1: 4 in terms of bulking value add citric acid, germ flour and
Citric acid solid-liquid ratio 1: 3 in terms of bulking value, is eventually adding 0.5% glutamic acid of germ flour weight, temperature 45 C, pH6, anti-
6h between seasonable in reaction process, is assisted using ultrasonic wave;Intensified by ultrasonic wave condition, power 800W, frequency 100KHz, work half
Minute, it is spaced half a minute;
(3) it purifies, supernatant is extracted after the completion of reaction, the ethanol solution of 85% concentration, supernatant and ethanol solution is added
Weight ratio be 2:3, refluxing extraction 1.5h at a temperature of 75 DEG C;Extraction 25min is centrifuged again, extracts supernatant later;Purifying
Microwave reinforced, microwave frequency 10 is used in the process7HZ;
(4) ultrafiltration carries out ultrafiltration using 50 nanometers of ultrafiltration membranes under 0.3MPa pressure;
(5) it concentrates, concentration is evaporated to ultrafiltration permeate, is concentrated into the 1/10-1/20 of permeate volume;
(6) it decolourizes, without decoloration;
(7) dry, it is dried using spray drying process and γ-aminobutyric acid pulvis is made.
In the description of this specification, the description of reference term " one embodiment ", " example ", " specific example " etc. means
Particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one implementation of the present invention
In example or example.In the present specification, schematic expression of the above terms may not refer to the same embodiment or example.
Moreover, particular features, structures, materials, or characteristics described can be in any one or more of the embodiments or examples to close
Suitable mode combines.
Finally, it should be noted that present invention disclosed above preferred embodiment is only intended to help to illustrate the present invention.It is excellent
It selects embodiment there is no all details of detailed descriptionthe, does not limit the invention to the specific embodiments described.Obviously, root
According to the content of this specification, can make many modifications and variations.These embodiments are chosen and specifically described to this specification, be in order to
The principle of the present invention and practical application are preferably explained, to enable skilled artisan to be best understood by and utilize
The present invention.The invention is limited only by the claims and the full scope thereof and equivalents thereof.
Claims (10)
1. the extracting method of γ-aminobutyric acid in a kind of seawater rice plumule, it is characterised in that:Include the following steps:
A extra large aid from rice germ powder) is prepared:
(1) plumule is tamed, selected seawater rice, and is soaked in domestication liquid;
(2) vernalization is placed in vernalization in germinator, is used in pregermination procedure and use electric field-enhanced vernalization, rinsed and done with water after germination
Only;
(3) it crushes, seawater rice plumule is dried, ultramicro grinding is carried out to dry plumule;
B γ-aminobutyric acid) is extracted:
(1) it pre-processes, germ flour is placed in retort, vacuum produces nitrogen 3-6h;
(2) extract, water be added, germ flour and water solid-liquid ratio 1: 2-1: 4 in terms of bulking value add citric acid, germ flour and
Citric acid solid-liquid ratio 1: 2-1: 3 in terms of bulking value are eventually adding the glutamic acid of the 0.1%-0.5% of germ flour weight, temperature
35-45 DEG C, pH5-6, reaction time 4-6h, in reaction process, assisted using ultrasonic wave;
(3) purifying, extraction supernatant after the completion of reaction, the ethanol solution of addition 70-85% concentration, supernatant and ethanol solution
Weight ratio is 2:2-3, refluxing extraction 1-1.5h at a temperature of 60-75 DEG C;Extraction 15-30min is centrifuged again, extracts supernatant later
Liquid;
(4) ultrafiltration carries out ultrafiltration using 50 nanometers of ultrafiltration membranes under 0.3MPa pressure;
(5) it concentrates, concentration is evaporated to ultrafiltration permeate, is concentrated into the 1/10-1/20 of permeate volume;
(6) it decolourizes, decolourizes as needed in concentration process;
(7) dry, it is dried using spray drying process and γ-aminobutyric acid pulvis is made.
2. the extracting method of γ-aminobutyric acid in a kind of seawater rice plumule according to claim 1, it is characterised in that:Step
Rapid A) in, electric field-enhanced condition:Electric field strength 30-50kV/cm, burst length 500-600 μ s, pulse frequency 100-300Hz.
3. the extracting method of γ-aminobutyric acid in a kind of seawater rice plumule according to claim 1, it is characterised in that:Step
Rapid A) in, it is dried using micro-wave drying method, microwave drying condition is:Frequency 3000-4000MHz, power 3000W, temperature
50-60℃。
4. the extracting method of γ-aminobutyric acid in a kind of seawater rice plumule according to claim 1, it is characterised in that:Step
Rapid A) in, ultra micro grain size of micropowder obtained is less than 10 μm.
5. the extracting method of γ-aminobutyric acid in a kind of seawater rice plumule according to claim 1, it is characterised in that:Step
Rapid B) in, when pretreatment, 3h is handled using infrared radiation, was irradiated 1 minute every 1 minute.
6. the extracting method of γ-aminobutyric acid in a kind of seawater rice plumule according to claim 1, it is characterised in that:Step
Rapid B) in, intensified by ultrasonic wave, power 400-800W, frequency 50-100KHz work half a minute, are spaced half a minute.
7. the extracting method of γ-aminobutyric acid in a kind of seawater rice plumule according to claim 1, it is characterised in that:Step
Rapid B) in, using microwave reinforced when purifying.
8. the extracting method of γ-aminobutyric acid in a kind of seawater rice plumule according to claim 7, it is characterised in that:It is micro-
Wave frequency rate is 105HZ-107HZ。
9. the extracting method of γ-aminobutyric acid in a kind of seawater rice plumule according to claim 1, it is characterised in that:Step
Rapid B) in, it is decolourized using absorption resin.
10. the extracting method of γ-aminobutyric acid in a kind of seawater rice plumule according to claim 1, it is characterised in that:Step
Rapid B) in, γ-aminobutyric acid pulvis water content obtained is less than 8%, and γ-aminobutyric acid purity is more than 60%.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110916098A (en) * | 2019-12-14 | 2020-03-27 | 黑龙江省科学院高技术研究院 | Vegetable soybean sprouting preparation process and preparation process of edible raw materials thereof |
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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CN104498548A (en) * | 2014-11-27 | 2015-04-08 | 苏州嘉禧萝生物科技有限公司 | Production method for enriching gamma-aminobutyric acid from germinated brown rice |
CN105815665A (en) * | 2016-03-18 | 2016-08-03 | 武汉海稻国际生物科技有限公司 | Preparation method of seawater rice brown rice enzyme powder |
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CN1995365A (en) * | 2006-12-15 | 2007-07-11 | 江南大学 | Method for preparing high concentration gamma-aminobutyric acid powder using rice bran as material |
CN104498548A (en) * | 2014-11-27 | 2015-04-08 | 苏州嘉禧萝生物科技有限公司 | Production method for enriching gamma-aminobutyric acid from germinated brown rice |
CN105815665A (en) * | 2016-03-18 | 2016-08-03 | 武汉海稻国际生物科技有限公司 | Preparation method of seawater rice brown rice enzyme powder |
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CN110916098A (en) * | 2019-12-14 | 2020-03-27 | 黑龙江省科学院高技术研究院 | Vegetable soybean sprouting preparation process and preparation process of edible raw materials thereof |
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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Application publication date: 20181012 |