CN103623080A - High-content jujube cyclic adenosine monophosphate extract and preparation method thereof - Google Patents
High-content jujube cyclic adenosine monophosphate extract and preparation method thereof Download PDFInfo
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Abstract
The invention provides a high-content jujube cyclic adenosine monophosphate extract and a preparation method thereof, wherein the concentration of cyclic adenosine monophosphate in the extract is more than 15mg per 100g, a solid or semisolid raw material of jujube is adopted, the solid or semisolid raw material is extracted by a high-pressure-difference continuous low-temperature extractor, and a crude extract of the jujube is obtained by vacuum drying and crushing after an extracting solution is concentrated; extracting the crude extract by adopting a supercritical extraction technology to obtain a jujube cyclic adenosine monophosphate extract; the jujube cyclic adenosine monophosphate extract has remarkable effects of resisting anoxia, resisting fatigue and improving the quality of life, and the preparation method has the following obvious advantages: the extraction transfer rate is high; (2) the production efficiency is high; (3) the quality controllability is high; (4) the operation controllable degree is high; (5) the comprehensive utilization rate of resources is high; (6) the comprehensive operation cost is low; (7) the automation degree is high; (8) the environmental pollution is low.
Description
Technical field
The present invention relates to extraction and the enrichment production field of effective ingredients in plant, especially a kind of preparation method of high-load Fructus Jujubae cyclic adenosine monophosphate extract.
Background technology
Cyclic adenosine monophosphate (cyclic ademodsine monophosphate is called for short cAMP) is the agent alive of a kind of protein kinase system, is extensively present in the tissue and cell of organism.It is subject to the control of neuroendocrine system, as the second message,second messenger of the hormones such as peptide hormone, catecholamine and prostaglandin, brings into play biological effect.Preclinical medicine and clinic study prove, cAMP can, by promoting brain cell metabolism, repairing old and feeble and tired brain cell, stop brain cell old and feeble, thereby improve sleep and memory; The physiological functions such as the formation of body lymphocyte transformation, antibody and release, cellular immunization are had to important regulating action, thereby enhancing immunity, selectivity suppress organism immune response, improve the immunologic functions such as allergic dermatitis, measles, asthma; Suppress cell proliferation, promote cell differentiation, play antineoplastic action; By approach such as cardiac nutrition, positive inotropic, vasodilators, improve cardiovascular function; Adjusting neurotransmitter is synthetic, promotes hormone secretion, maintains normal human physiological activity.
1991, Liu Mengjun etc. measure the cAMP content of 14 kinds of gardening plants by protein binding method, the content of finding cAMP in Fructus Jujubae is the highest, in its mature sarcocarp, the content of cAMP is the thousands of to tens thousand of times of general animals and plants material, scope is at 60-800 μ g/g, wherein, the content that is described as cAMP in the Golden jujube that the Wudi County in " Chinese Golden jujube the first county " abounds with is higher; People's reports such as Han Liwen, in the grand snow jujube of Yi Mengshan Mountain, Shandong, cAMP is suitable with Golden jujube content.
At present, the preparation method of cyclic adenosine monophosphate preparation mainly comprises that chemical synthesis, microbe fermentation method and traditional extraction technique merge column chromatography purification.Wherein, chemical synthesis be take adenosine as raw material such as (2003) such as Shen bright red, and phosphorus oxychloride is phosphorus esterification reagent, with triethyl phosphate, makes solvent, under low temperature, generate 5 ' dichloro phosphate ester of adenosine, this intermediate is separated with reaction system, incorporate suitable solvent, under stirring, slowly join in the water and acetonitrile solution of KOH, highly basic cyclisation obtains 3 ', 5 '-cyclic adenosine monophosphate, purity to 98.5% after recrystallization from second alcohol and water, total recovery 58%; Microbe fermentation method is Japanology person (Kokai Tokyyo Koho for example, 1997) adopt the means of gene recombinaton to obtain strain Escherichiacoli K-11, can fermenting and producing cAMP, adopt shaking table to cultivate 14h at 28 ℃, culture medium is glucose 0.5%, KH
2pO
41.4%, (NH
4)
2sO
40.2%, MgSO
47H
2o 0.02%, peptone 0.4%, and yeast powder 0.02%, in culture fluid, the concentration of cAMP is 3.9%mg/150mL; CN 100425620C discloses a kind of technique of extracting cyclic adenosine monophosphate from Fructus Jujubae, adopts immersion-supersound extraction Fructus Jujubae, obtains clarifying Fructus Jujubae juice, Fructus Jujubae juice passes through anion-exchange column, aqueous formic acid eluting, ammonia spirit regulates pH value, after anion-exchange column, the eluent of collecting is by chromatographic column (silica gel type, or macroporous resin type, or polyamide type), then water or ethanol water eluting, after eluent is concentrated, add dehydrated alcohol crystallization, obtain high-purity cyclic adenosine monophosphate powder.
Yet above-mentioned chemical synthesis reagent used has certain toxicity, contaminated environment; And technical sophistication, expensive, be difficult to realize large-scale production; Due to the by-product reason in building-up process, the scope of application is very little, is mainly used in the treatment of the cardiovascular disease such as angina pectoris, myocardial infarction, myocarditis and cardiogenic shock, uses excessive meeting toxic side effect.Column chromatography has been used some irritating reagent in separation process, also very high to the security requirement of chromatographic column filler.Microbe fermentation method, owing to being subject to strain restriction and being difficult to separation, uses and also has certain limitation.The equipment major part that conventional extracting method adopts is unit batch, is difficult to form the scale that serialization is produced, and affects leaching process standardized process.
Visible, large for the solvent-oil ratio existing in prior art, the cycle is long, automatization level is low, the technical problem such as chemosynthesis byproduct in process thing is many, the production technology of seeking a kind of new cyclic adenosine monophosphate has very important production practices meaning.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of high-load Fructus Jujubae cyclic adenosine monophosphate extract.
Another technical problem to be solved by this invention is to provide the preparation method of above-mentioned high-load Fructus Jujubae cyclic adenosine monophosphate extract.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A kind of high-load Fructus Jujubae cyclic adenosine monophosphate extract, in described extract, the concentration of cyclic adenosine monophosphate is more than every 15mg/100g, cyclic adenosine monophosphate reaches more than 90% from the interest rate that turns of raw material, this extract is obtained by following method: the solid or the semi-solid raw material that adopt Fructus Jujubae, through High Pressure Difference continuous low-temperature extractor, extract, after extracting solution is concentrated, vacuum drying, pulverizes to obtain the crude extract of Fructus Jujubae; Adopt supercritical extraction technique extraction crude extract, obtain Fructus Jujubae cyclic adenosine monophosphate extract.
A preparation method for high-load Fructus Jujubae cyclic adenosine monophosphate extract, adopts solid or the semi-solid raw material of Fructus Jujubae, through High Pressure Difference continuous low-temperature extractor, extracts, and after extracting solution is concentrated, vacuum drying, pulverizes to obtain the crude extract of Fructus Jujubae; Adopt supercritical extraction technique extraction crude extract, obtain high-load Fructus Jujubae cyclic adenosine monophosphate extract.
Preferably, the preparation method of above-mentioned high-load Fructus Jujubae cyclic adenosine monophosphate extract, concrete steps are as follows:
(1) place material: choosing water content is raw material at the Fructus Jujubae of 5-30%, pulverize raw material, making particle diameter is 180-850 μ m(80-24 order);
(2) evacuation: under response system temperature-10-0 ℃ condition, in High Pressure Difference continuous low-temperature extractor, form vacuum, vacuum keep is at-100--20pa, add water or 5-70%(v/v) ethanol water, keep 5-30min, wherein, described raw material and water or 5-70%(v/v) weight ratio of ethanol water is 1:6-20;
(3) subtract vacuum: pass into purification of compressed air, make the pressure in High Pressure Difference continuous low-temperature extractor rise to 0Mpa, keep 1-10min;
(4) pressurization: continue to pass into compressed air, make the pressure in High Pressure Difference continuous low-temperature extractor reach 8-12Mpa, keep 1-20min;
(5) decompression: stop pressurization, evacuation, makes Pressure Drop in High Pressure Difference continuous low-temperature extractor to 0Mpa;
(6) circulation is extracted: circulated in step (2)-(5), circulate 10 times;
(7) separation: by filtration, centrifugal, make solid-liquid separation, collect extracting solution;
(8) dry: step (7) gained extracting solution is concentrated, and vacuum drying, pulverized 20-80 mesh sieve, obtained crude extract powder;
(9) supercritical extraction: with 5-99%(v/v) ethanol is made entrainer and is evenly mixed with crude extract powder, carry secretly than for 8-15%(herein, carry secretly than referring to the volume mass ratio of entrainer with crude extract powder, ml/g), after balance 10-30min, carry out dynamic extraction, at extraction kettle pressure 15-60Mpa, extraction temperature 35-60 ℃, extraction time 0.5-5 hour, separating still pressure 5-30Mpa, separating still temperature 10-50 ℃, disengaging time 0.5-5 hour, in same flow process, separating still pressure is less than extraction kettle pressure all the time, under the condition of carbon dioxide flow 10-100L/h, decompression separation, obtain Fructus Jujubae cyclic adenosine monophosphate extract.
Preferably, the preparation method of above-mentioned high-load Fructus Jujubae cyclic adenosine monophosphate extract, pulverizes after raw material in described step (1), and the content of cyclic adenosine monophosphate is 0.01-0.08%.
Preferably, the preparation method of above-mentioned high-load Fructus Jujubae cyclic adenosine monophosphate extract, in described step (1), choosing water content is raw material at the Fructus Jujubae of 5-15%.
Preferably, the preparation method of above-mentioned high-load Fructus Jujubae cyclic adenosine monophosphate extract, in described step (1), choosing water content is raw material at 10% Fructus Jujubae, pulverizes raw material, making particle diameter is 250 μ m(65 orders).
Preferably, the preparation method of above-mentioned high-load Fructus Jujubae cyclic adenosine monophosphate extract, in described step (1), Fructus Jujubae is Golden jujube (Cangzhou, Hebei) or grand snow jujube (Yimeng Mountain Area, Shandong Province).
Preferably, the preparation method of above-mentioned high-load Fructus Jujubae cyclic adenosine monophosphate extract, the vacuum keep of described step (2) evacuation is at-70pa, add 50%(v/v) ethanol water, keeping 20min, wherein, described raw material and 50%(v/v) weight ratio of ethanol water is 1:10.
Preferably, the preparation method of above-mentioned high-load Fructus Jujubae cyclic adenosine monophosphate extract, response system temperature-10-0 ℃ in described step (2), is to realize by the cooling water in High Pressure Difference continuous low-temperature extractor periphery condensation cycle system.
Preferably, the preparation method of above-mentioned high-load Fructus Jujubae cyclic adenosine monophosphate extract, described cooling water is 95%(v/v) ethanol.
Preferably, the preparation method of above-mentioned high-load Fructus Jujubae cyclic adenosine monophosphate extract, the pressure of described step (4) pressurization reaches 11Mpa, keeps 15min.
Preferably, the preparation method of above-mentioned high-load Fructus Jujubae cyclic adenosine monophosphate extract, in described step (7), extracting solution is the centrifugal liquid that solid-liquid separation is extremely clarified by 400 object membrane filtrations.
Preferably, the preparation method of above-mentioned high-load Fructus Jujubae cyclic adenosine monophosphate extract, in described step (9) with 90%(v/v) ethanol makes entrainer and evenly mixes with crude extract powder, carry secretly than being 15%, after balance 30min, carry out dynamic extraction, at extraction kettle pressure 40Mpa, 37 ℃ of extraction temperature, extraction time 5 hours, separating still pressure 6Mpa, 30 ℃ of separating still temperature, disengaging time 2.5 hours, in same flow process, separating still pressure is less than extraction kettle pressure all the time, under the condition of carbon dioxide flow 20L/h, decompression separation, obtains Fructus Jujubae cyclic adenosine monophosphate extract.
Preferably, the preparation method of above-mentioned high-load Fructus Jujubae cyclic adenosine monophosphate extract, resulting cyclic adenosine monophosphate can further produce through conventional formulation processes the product that obtains the relevant dosage forms such as capsule, oral liquid, distillate medicinal water, granule, electuary, tablet.
The invention has the beneficial effects as follows:
High-load Fructus Jujubae cyclic adenosine monophosphate extract of the present invention, anti-hypoxia, resisting fatigue, the quality of making the life better aspect is remarkably productive, the preparation method of this high-load Fructus Jujubae cyclic adenosine monophosphate extract, raw material Fructus Jujubae is carried out to cold drying processing, total ash is no more than 2.0%, utilize with batch medicinal material extract liquid enrichment cyclic adenosine monophosphate, adopt High Pressure Difference low temperature sequential extraction method, by instantaneous vacuum pressed, histiocyte in Fructus Jujubae is broken, Related Component in born of the same parents is fully contacted with solvent, directly dissolve, thereby reach the effect of high efficiency extraction, by supercritical carbon dioxide extraction method separation, obtain high yield again, highly purified cyclic adenosine monophosphate (cAMP), adopt the ethanol of certain concentration to make entrainer, alternative condition obtains the cyclic adenosine monophosphate active component with high-load, its concentration is more than 15mg/g, the quality raw materials of food or medicine.
Compare with existing extractive technique, the preparation method of high-load Fructus Jujubae cyclic adenosine monophosphate extract of the present invention has following obvious advantage:
(1) the extraction rate of transform is high;
(2) production efficiency is high;
(3) quality controllability is high;
(4) operation controllable degree is high;
(5) comprehensive utilization of resources rate is high: solvent consumption significantly reduces, and in extracting solution, Camp Content is high, and later stage concentrated cost reduces;
(6) integrated operation cost is low;
(7) automaticity is high;
(8) environmental pollution is low.
Accompanying drawing explanation
Fig. 1 is cyclic adenosine monophosphate standard substance high-efficient liquid phase chromatograms;
Fig. 2 is the high-efficient liquid phase chromatogram of embodiment 1 gained high-load Fructus Jujubae cyclic adenosine monophosphate extract.
The specific embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is further described.
Embodiment 1
A high-load Fructus Jujubae cyclic adenosine monophosphate extract, its concrete preparation process is as follows:
(1) place material: the Hebei Cangzhou Golden Chinese Date 10kg by water content 10%, pulverized 65 mesh sieves, make particle diameter 250 μ m, be placed in High Pressure Difference continuous low-temperature extractor;
(2) evacuation: by cooling water (95%(v/v) ethanol in High Pressure Difference continuous low-temperature extractor periphery condensation cycle system) make under ℃ condition of response system temperature-7, in High Pressure Difference continuous low-temperature extractor, form vacuum, vacuum keep is at-70pa, after constant voltage, add 50%(v/v) ethanol water, keeping 20min, wherein, described raw material and 50%(v/v) weight ratio of ethanol water is 1:10;
(3) subtract vacuum: slowly pass into the compressed air of purification, make High Pressure Difference continuous low-temperature extractor internal pressure rise to 0Mpa, the time is about 3min;
(4) pressurization: continue to pass into compressed air, make the pressure in High Pressure Difference continuous low-temperature extractor reach 11Mpa, keep 15min;
(5) decompression: stop pressurization, open vent valve, evacuation, makes Pressure Drop in High Pressure Difference continuous low-temperature extractor to 0Mpa;
(6) circulation is extracted: continue step (2)-(5), circulate 10 times;
(7) separation: after filtration, centrifugal, by solid-liquid separation, centrifugal liquid to clarification, is collected extracting solution through 400 object membrane filtrations;
(8) dry: step (7) gained extracting solution is concentrated, and vacuum drying, pulverized 65 mesh sieves, obtained the crude extract powder of Fructus Jujubae;
(9) supercritical extraction: with 90%(v/v) ethanol is made entrainer and is evenly mixed with crude extract powder, carry secretly than for 15%(herein, carry secretly than referring to the volume mass ratio of entrainer with crude extract powder, ml/g), after balance 30min, carry out dynamic extraction, at extraction kettle pressure 40Mpa, 37 ℃ of extraction temperature, extraction time 5 hours, separating still pressure 6Mpa, 30 ℃ of separating still temperature, disengaging time 2.5 hours, in same flow process, separating still pressure is less than extraction kettle pressure all the time, under the condition of carbon dioxide flow 20L/h, concentrating under reduced pressure, dry, obtain Fructus Jujubae cyclic adenosine monophosphate extract, Fructus Jujubae cyclic adenosine monophosphate extract is carried out to high performance liquid chromatography detection, wherein, chromatograph: by P200 II high pressure constant flow pump, UV200 II ultraviolet variable-wavelenght detector and Echrom98 chromatographic work station etc. partly form, sample treatment: accurately measure 10ml and use distilled water standardize solution in 50ml volumetric flask, shake up, centrifugal, 0.45 μ m membrane filtration, obtains, chromatographic column: Hydersir BDS C18, mobile phase: 20mol/LKH
2pO
4-methanol (90:10), column temperature: 25 ℃, detect wavelength: 254nm, 7 flow velocitys: 0.6mL/min, sample size: 10 μ L.As depicted in figs. 1 and 2, the extract that wherein Camp Content is 15mg/100g.
Embodiment 2
A high-load Fructus Jujubae cyclic adenosine monophosphate extract, its concrete preparation process is as follows:
(1) place material: choosing water content be raw material at 5% grand snow jujube (Yimeng Mountain Area, Shandong Province), pulverizing raw material, making particle diameter is 180 μ m(80 orders);
(2) evacuation: under 0 ℃ of condition of response system temperature, form vacuum in High Pressure Difference continuous low-temperature extractor, vacuum keep, at-100pa, adds aqueous solution, keeps 30min, and wherein, the weight ratio of described raw material and aqueous solution is 1:6;
(3) subtract vacuum: pass into purification of compressed air, make the pressure in High Pressure Difference continuous low-temperature extractor rise to 0Mpa, keep 10min;
(4) pressurization: continue to pass into compressed air, make the pressure in High Pressure Difference continuous low-temperature extractor reach 12Mpa, keep 1min;
(5) decompression: stop pressurization, evacuation, makes Pressure Drop in High Pressure Difference continuous low-temperature extractor to 0Mpa;
(6) circulation is extracted: circulated in step (2)-(5), circulate 10 times;
(7) separation: by filtration, centrifugal, make solid-liquid separation, collect extracting solution;
(8) dry: step (7) gained extracting solution is concentrated, and vacuum drying, pulverized 80 mesh sieves, obtained crude extract powder;
(9) supercritical extraction: with 99%(v/v) ethanol is made entrainer and is evenly mixed with crude extract powder, carry secretly than for 8%(herein, carry secretly than referring to the volume mass ratio of entrainer with crude extract powder, ml/g), after balance 30min, carry out dynamic extraction, at extraction kettle pressure 60Mpa, 35 ℃ of extraction temperature, extraction time 0.5 hour, separating still pressure 30Mpa, 10 ℃ of separating still temperature, disengaging time 0.5 hour, in same flow process, separating still pressure is less than extraction kettle pressure all the time, under the condition of carbon dioxide flow 10L/h, decompression separation, obtain the extract that Camp Content is 10mg/100g.
Embodiment 3
A high-load Fructus Jujubae cyclic adenosine monophosphate extract, its concrete preparation process is as follows:
(1) place material: choosing water content be raw material at 30% Golden jujube (Cangzhou, Hebei), pulverizing raw material, making particle diameter is 850 μ m(24 orders);
(2) evacuation: under ℃ condition of response system temperature-10, form vacuum in High Pressure Difference continuous low-temperature extractor, vacuum keep is at-20pa, add 5%(v/v) ethanol water, keeping 5min, wherein, described raw material and 5%(v/v) weight ratio of ethanol water is 1:20;
(3) subtract vacuum: pass into purification of compressed air, make the pressure in High Pressure Difference continuous low-temperature extractor rise to 0Mpa, keep 1min;
(4) pressurization: continue to pass into compressed air, make the pressure in High Pressure Difference continuous low-temperature extractor reach 8Mpa, keep 20min;
(5) decompression: stop pressurization, evacuation, makes Pressure Drop in High Pressure Difference continuous low-temperature extractor to 0Mpa;
(6) circulation is extracted: circulated in step (2)-(5), circulate 10 times;
(7) separation: after filtration, centrifugal, by solid-liquid separation, centrifugal liquid to clarification, is collected extracting solution through 400 object membrane filtrations;
(8) dry: step (7) gained extracting solution is concentrated, and vacuum drying, pulverized 20 mesh sieves, obtained crude extract powder;
(9) supercritical extraction: with 5%(v/v) ethanol is made entrainer and is evenly mixed with crude extract powder, carry secretly than for 15%(herein, carry secretly than referring to the volume mass ratio of entrainer with crude extract powder, ml/g), after balance 10min, carry out dynamic extraction, at extraction kettle pressure 15Mpa, 60 ℃ of extraction temperature, extraction time 5 hours, separating still pressure 5Mpa, separating still temperature 50 C, disengaging time 5 hours, in same flow process, separating still pressure is less than extraction kettle pressure all the time, under the condition of carbon dioxide flow 100L/h, decompression separation, obtain the extract that Camp Content is 9.5mg/100g.
Embodiment 4
A high-load Fructus Jujubae cyclic adenosine monophosphate extract, its concrete preparation process is as follows:
(1) place material: choosing water content is raw material at 15% Golden jujube, pulverizes raw material, crosses 65 mesh sieves;
(2) evacuation: under ℃ condition of response system temperature-5, form vacuum in High Pressure Difference continuous low-temperature extractor, vacuum keep is at-50pa, add 70%(v/v) ethanol water, keeping 20min, wherein, described raw material and 70%(v/v) weight ratio of ethanol water is 1:8;
(3) subtract vacuum: pass into purification of compressed air, make the pressure in High Pressure Difference continuous low-temperature extractor rise to 0Mpa, keep 5min;
(4) pressurization: continue to pass into compressed air, make the pressure in High Pressure Difference continuous low-temperature extractor reach 10Mpa, keep 10min;
(5) decompression: stop pressurization, evacuation, makes Pressure Drop in High Pressure Difference continuous low-temperature extractor to 0Mpa;
(6) circulation is extracted: circulated in step (2)-(5), circulate 10 times;
(7) separation: after filtration, centrifugal, by solid-liquid separation, centrifugal liquid to clarification, is collected extracting solution through 400 object membrane filtrations;
(8) dry: step (7) gained extracting solution is concentrated, and vacuum drying, pulverized 40 mesh sieves, obtained crude extract powder;
(9) supercritical extraction: with 70%(v/v) ethanol is made entrainer and is evenly mixed with crude extract powder, carry secretly than for 12%(herein, carry secretly than referring to the volume mass ratio of entrainer with crude extract powder, ml/g), after balance 25min, carry out dynamic extraction, at extraction kettle pressure 40Mpa, 45 ℃ of extraction temperature, extraction time 4 hours, separating still pressure 25Mpa, 40 ℃ of separating still temperature, disengaging time 4 hours, in same flow process, separating still pressure is less than extraction kettle pressure all the time, under the condition of carbon dioxide flow 90L/h, decompression separation, obtain the extract that Camp Content is 13mg/100g.
Embodiment 5
A high-load Fructus Jujubae cyclic adenosine monophosphate extract, its concrete preparation process is as follows:
(1) place material: choosing water content is raw material at 20% Golden jujube, pulverizes raw material, crosses 40 mesh sieves;
(2) evacuation: under ℃ condition of response system temperature-8, form vacuum in High Pressure Difference continuous low-temperature extractor, vacuum keep is at-60pa, add 70%(v/v) ethanol water, keeping 15min, wherein, described raw material and 70%(v/v) weight ratio of ethanol water is 1:15;
(3) subtract vacuum: pass into purification of compressed air, make the pressure in High Pressure Difference continuous low-temperature extractor rise to 0Mpa, keep 5min;
(4) pressurization: continue to pass into compressed air, make the pressure in High Pressure Difference continuous low-temperature extractor reach 12Mpa, keep 5min;
(5) decompression: stop pressurization, evacuation, makes Pressure Drop in High Pressure Difference continuous low-temperature extractor to 0Mpa;
(6) circulation is extracted: circulated in step (2)-(5), circulate 10 times;
(7) separation: after filtration, centrifugal, by solid-liquid separation, centrifugal liquid to clarification, is collected extracting solution through 400 object membrane filtrations;
(8) dry: step (7) gained extracting solution is concentrated, and vacuum drying, pulverized 65 mesh sieves, obtained crude extract powder;
(9) supercritical extraction: with 90%(v/v) ethanol is made entrainer and is evenly mixed with crude extract powder, carry secretly than for 13%(herein, carry secretly than referring to the volume mass ratio of entrainer with crude extract powder, ml/g), after balance 20min, carry out dynamic extraction, at extraction kettle pressure 50Mpa, 40 ℃ of extraction temperature, extraction time 2.5 hours, separating still pressure 15Mpa, 20 ℃ of separating still temperature, disengaging time 2.5 hours, in same flow process, separating still pressure is less than extraction kettle pressure all the time, under the condition of carbon dioxide flow 30L/h, decompression separation, obtain the extract that Camp Content is 11.5mg/100g.
In above-described embodiment, gained high-load Fructus Jujubae cyclic adenosine monophosphate extract can be used for preparing liquid beverage, for example, gets gained high-load Fructus Jujubae cyclic adenosine monophosphate extract in 2g embodiment 1, is dissolved in 4L pure water aseptic embedding, every bottle of 10mL.
With high-load Fructus Jujubae cyclic adenosine monophosphate extract described in embodiment 1, test as follows:
By the variation of blood oxygen saturation, content of hemoglobin, Serum lactic acid content, blood urea nitrogen content before and after contrast test, anti-hypoxia, the anti-fatigue effect of high-load Fructus Jujubae cyclic adenosine monophosphate extract of the present invention are evaluated.
Adopt randomized controlled EXPERIMENTAL DESIGN, the trial volunteer that 120 examples is met to inclusive criteria/exclusion standard distributes according to the ratio of 1:1:1, and 120 people are divided into three groups of high dose group, low dose group, blank group at random.
The observation cycle is 40 days, and time window is ± 7 days, and detailed process is referring to table 1 clinical trial flow table.
Table 1 clinical trial flow table
Object of study: age, 16-25 year; Male.Adopt method of randomization, 3 groups of armed policemans that choose from the same area are subjects.By group, be divided at random three groups, i.e. high dose test group, low dosage test group and blank group, wherein,
High dose test group is embodiment 1 gained Fructus Jujubae cyclic adenosine monophosphate extract,
Low dosage test group is embodiment solution after 2 times of distilled water dilutings for 1 gained Fructus Jujubae cyclic adenosine monophosphate extract,
Blank group, be commercial high fructose syrup (Shanghai emergence sugar industry company limited),
Every group of number is 40 people, and Time of Administration is 40 days, usage for everyone deal be 20ml, every day twice, adding distil water is diluted to 200ml and drinks.
Evaluation index comprises:
Leading indicator: HGB, BUN, blood oxygen saturation, blood lactic acid;
Less important index: Evaluation on quality of life; Three kilometers are run time run.
Result of the test, in Table index situation of change table, table 3 Evaluation on quality of life table before and after 2 tests, does not have the generation of untoward reaction and adverse events in process of the test.
Index situation of change table before and after table 2 test
Through t check, between test first three groups, age, height, body weight etc. compare no difference of science of statistics, have comparability; Three groups enter group and are male, and between three groups, sex compares no difference of science of statistics, has comparability.
Through t check, between three groups, the equal not statistically significant of drug allergy history difference, has comparability (p>0.05).
Through T, check, before and after test, high dose group blood lactic acid (LAC), blood urea nitrogen (BUN), hemoglobin (HGB), blood oxygen saturation, three kilometers of time run comparing differences have statistical significance, after treatment, LAC, HGB treat front obvious reduction, and after treatment, BUN, blood oxygen saturation obviously raise; Before and after test, low dose group LAC, BUN, three kilometers of time runs more all have significant difference, before and after three kilometers of time run tests of matched group, have significant difference.Result shows, before and after the test of high and low dose group, LAC, BUN, HGB, blood oxygen saturation, three kilometers of time runs are improved to successful.
Through t check, high-load Fructus Jujubae cyclic adenosine monophosphate extract high and low dose group and matched group comparison after treatment, BUN, HGB, blood oxygen saturation comparing difference, not statistically significant, relatively improves index degree difference not obvious between group; After treatment, three groups of LAC, three kilometers of race timing comparing differences have statistical significance.Be that high and low dose group has statistical significance compared with matched group comparing difference, LAC, three kilometers of race timing reduce obviously compared with matched group.But comparing difference not statistically significant between high and low dose group.Statistical result shows, compares Fructus Jujubae cyclic adenosine monophosphate extract high and low dose group remarkable to LAC and three kilometers of time run effects with matched group, is obviously better than matched group, and there is no notable difference between high and low dose group.
Table 3 Evaluation on quality of life table
High dose group is remarkable with matched group comparing difference aspect improving in sleep, physical ability, appetite, and low dose group also has certain effect improving aspect sleep.
Wherein, abbreviation that above-mentioned test is used is in Table 4 abbreviation abridged tables
Table 4 abbreviation abridged table
By above-mentioned test, can be found out, treat sex between first two groups, age, height, body weight, the equal not statistically significant of drug allergy history comparing difference, have comparability, curative effect comparative result shows:
Before and after treatment, compare: before and after test, high dose group LAC, BUN, HGB, blood oxygen saturation, three kilometers of time run comparing differences have significant difference, after treatment, LAC, HGB treat front obvious reduction, and after treating, BUN, blood oxygen saturation obviously raise; Before and after test, low dose group LAC, BUN, three kilometers of time runs more all have significant difference, before and after three kilometers of time run tests of matched group, have significant difference.
Between group relatively: three groups of BUN, HGB, blood oxygen saturation comparing difference after test, not statistically significant, three groups to improve index degree difference not obvious; After treatment, three groups of LAC, three kilometers of race timing comparing differences have statistical significance: after test, high and low dose group LAC is with respect to matched group, and low dose group has statistical significance; High dose group has significant difference; Between high and low dose group, contrast does not have statistical significance; LAC, three kilometers of race timing reduce obviously compared with matched group, but comparing difference not statistically significant between high and low dose group.
To sum up, can find out:
1) pass through clinical experimental study, high-load Fructus Jujubae cyclic adenosine monophosphate extract high dose group is to blood lactic acid, blood urea nitrogen, hemoglobin, blood oxygen saturation, three kilometers of time runs, before and after test, change variant, there is significant difference, and especially outstanding on the impact of blood lactic acid, there is remarkable statistical significance; High dose group is also improved effect to sleep, physical ability, appetite, and effective percentage is respectively 97.5%, 80%, 80%, illustrates that high dose group is comparatively obvious to the impact effect of animal economy.
2) high-load Fructus Jujubae cyclic adenosine monophosphate extract low dose group, to influential before and after HGB, blood oxygen saturation test, does not still have statistical significance, and blood lactic acid, blood urea nitrogen, three kilometers of race timing are changed significantly, and has statistical significance; Low dose group has certain help to the improvement of sleep quality, and the improvement of physical ability and appetite and matched group ratio are not had to significant difference.
3) with matched group comparison, high and low dose group changes and has statistical significance blood lactic acid, and wherein high dose group has remarkable statistical significance; High and low dose group has significant difference to the impact of three kilometers of time runs, and compares not statistically significant between high and low dose group.To other index blood urea nitrogen, hemoglobin, three indexs of blood oxygen saturation, before and after test, self relatively there is statistical significance, relatively there is no statistical significance with matched group.
Result of the test shows, the lactic acid producing in body in high-load Fructus Jujubae cyclic adenosine monophosphate extract high and low dose grouping machine body anoxia and motion, blood urea nitrogen etc. have good removing effect, especially the elimination of lactic acid are had to more outstanding effect.By reducing the generation of lactic acid or accelerating the elimination of lactic acid, reduce the fatigue factor in body, thereby reach the effect of anti-hypoxia, fatigue alleviating.And by the comprehensive regulating action to the hemoglobin of body, blood oxygen saturation, sleep etc., reach a comprehensive effect of improving body body constitution.
Above-mentioned detailed description of this kind of high-load Fructus Jujubae cyclic adenosine monophosphate extract and preparation method thereof being carried out with reference to embodiment; illustrative rather than determinate; can list several embodiment according to institute's limited range; therefore in the variation and the modification that do not depart under general plotting of the present invention, within should belonging to protection scope of the present invention.
Claims (10)
1. a high-load Fructus Jujubae cyclic adenosine monophosphate extract, it is characterized in that: in described extract, the concentration of cyclic adenosine monophosphate is that every 100g is greater than 15mg, this extract is obtained by following method: the solid or the semi-solid raw material that adopt Fructus Jujubae, through High Pressure Difference continuous low-temperature extractor, extract, after extracting solution is concentrated, vacuum drying, pulverizes to obtain the crude extract of Fructus Jujubae; Adopt supercritical extraction technique extraction crude extract, obtain Fructus Jujubae cyclic adenosine monophosphate extract.
2. the preparation method of Fructus Jujubae cyclic adenosine monophosphate extract claimed in claim 1, is characterized in that: adopt solid or the semi-solid raw material of Fructus Jujubae, through High Pressure Difference continuous low-temperature extractor, extract, after extracting solution is concentrated, vacuum drying, pulverizes to obtain the crude extract of Fructus Jujubae; Adopt supercritical extraction technique extraction crude extract, obtain Fructus Jujubae cyclic adenosine monophosphate extract.
3. the preparation method of Fructus Jujubae cyclic adenosine monophosphate extract according to claim 2, is characterized in that: concrete steps are as follows:
(1) place material: choosing water content is raw material at the Fructus Jujubae of 5-30%, pulverize raw material, making particle diameter is 180-850 μ m;
(2) evacuation: under response system temperature-10-0 ℃ condition, make formation vacuum in High Pressure Difference continuous low-temperature extractor, vacuum keep is at-100--20pa, add water or 5-70%(v/v) ethanol water, keep 5-30min, wherein, described raw material and water or 5-70%(v/v) weight ratio of ethanol water is 1:6-20;
(3) subtract vacuum: pass into purification of compressed air, make the pressure in High Pressure Difference continuous low-temperature extractor rise to 0Mpa, keep 1-10min;
(4) pressurization: continue to pass into compressed air, make the pressure in High Pressure Difference continuous low-temperature extractor reach 8-12Mpa, keep 1-20min;
(5) decompression: stop pressurization, evacuation, makes Pressure Drop in High Pressure Difference continuous low-temperature extractor to 0Mpa;
(6) circulation is extracted: circulated in step (2)-(5), circulate 10 times;
(7) separation: by filtration, centrifugal, make solid-liquid separation, collect extracting solution;
(8) dry: step (7) gained extracting solution is concentrated, and vacuum drying, pulverized 20-80 mesh sieve, obtained crude extract powder;
(9) supercritical extraction: with 5-99%(v/v) ethanol is made entrainer and is evenly mixed with crude extract powder, carry secretly than being 8-15%, after balance 10-30min, carry out dynamic extraction, at extraction kettle pressure 15-60Mpa, extraction temperature 35-60 ℃, extraction time 0.5-5 hour, separating still pressure 5-30Mpa, separating still temperature 10-50 ℃, disengaging time 0.5-5 hour, in same flow process, separating still pressure is less than extraction kettle pressure all the time, under the condition of carbon dioxide flow 10-100L/h, decompression separation, obtains Fructus Jujubae cyclic adenosine monophosphate extract.
4. the preparation method of Fructus Jujubae cyclic adenosine monophosphate extract according to claim 3, is characterized in that: in described step (1), choosing water content is raw material at the Fructus Jujubae of 5-15%.
5. according to the preparation method of the Fructus Jujubae cyclic adenosine monophosphate extract described in claim 3 or 4, it is characterized in that: in described step (1), choosing water content is raw material at 10% Fructus Jujubae, pulverizes raw material, and making particle diameter is 250 μ m.
6. the preparation method of Fructus Jujubae cyclic adenosine monophosphate extract according to claim 3, it is characterized in that: the vacuum keep of described step (2) evacuation is at-70pa, add 50%(v/v) ethanol water, keep 20min, wherein, described raw material and 50%(v/v) weight ratio of ethanol water is 10:1; Response system temperature-10-0 ℃ in described step (2) is to realize by the cooling water in High Pressure Difference continuous low-temperature extractor periphery condensation cycle system.
7. the preparation method of Fructus Jujubae cyclic adenosine monophosphate extract according to claim 6, is characterized in that: described cooling water is 95%(v/v) ethanol.
8. the preparation method of Fructus Jujubae cyclic adenosine monophosphate extract according to claim 3, is characterized in that: the pressure of described step (4) pressurization reaches 11Mpa, keeps 15min.
9. the preparation method of Fructus Jujubae cyclic adenosine monophosphate extract according to claim 3, is characterized in that: in described step (7), extracting solution is the centrifugal liquid that solid-liquid separation is extremely clarified by 400 object membrane filtrations.
10. the preparation method of Fructus Jujubae cyclic adenosine monophosphate extract according to claim 3, it is characterized in that: in described step (9) with 90%(v/v) ethanol makes entrainer and evenly mixes with crude extract powder, carry secretly than being 15%, after balance 30min, carry out dynamic extraction, at extraction kettle pressure 40Mpa, 37 ℃ of extraction temperature, extraction time 5 hours, separating still pressure 6Mpa, 30 ℃ of separating still temperature, disengaging time 2.5 hours, in same flow process, separating still pressure is less than extraction kettle pressure all the time, under the condition of carbon dioxide flow 20L/h, decompression separation, obtain Fructus Jujubae cyclic adenosine monophosphate extract.
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