CN103623080B - 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-content jujube cyclic adenosine monophosphate extract.
Background technology
Cyclic adenosine monophosphate (cyclic ademodsine monophosphate, be called for short cAMP) is that a kind of protein kinase system is lived agent, in the tissue being extensively present in organism and cell.It is by the control of neuroendocrine system, and the second message,second messenger as hormones such as peptide hormone, catecholamine and prostaglandins plays 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, thus improving water flood and memory; Important regulating action is had to the formation of body lymphocyte transformation, antibody and the physiological function such as release, cellular immunization, thus enhancing immunity, Selective depression organism immune response, improve the immunologic functions such as allergic dermatitis, measles, asthma; Antiproliferative effect, promotion cell differentiation, play antineoplastic action; Cardiovascular function is improved by approach such as cardiac nutrition, positive inotropic, vasodilators; Adjustment neurotransmitter synthesizes, and promotes hormone secretion, maintains normal human physiological activity.
1991, Liu Mengjun etc. measure by the cAMP content of protein binding method to 14 kinds of gardening plants, find that the content of 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, in the Golden jujube that the Wudi County being described as " Chinese Golden jujube first county " abounds with, the content of cAMP 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 chemical synthesis, microbe fermentation method and traditional extraction technique and merges column chromatography purification.Wherein, chemical synthesis such as Shen bright red etc. (2003) take adenosine as raw material, and phosphorus oxychloride is phosphorus esterification reagent, makes solvent with triethyl phosphate, 5 ' position either dichlorophosphate of adenosine is generated under low temperature, this intermediate is separated with reaction system, incorporates suitable solvent, in stir under slowly join KOH water and acetonitrile solution in, highly basic cyclisation obtains 3 ', 5 '-cyclic adenosine monophosphate, from second alcohol and water, after recrystallization, purity can reach 98.5%, total recovery 58%; Microbe fermentation method such as Japanese researchers (Kokai Tokyyo Koho, 1997) adopts the means of gene recombinaton to obtain strain Escherichiacoli K-11, can fermenting and producing cAMP, and adopt shaking table to cultivate 14h at 28 DEG C, culture medium is glucose 0.5%, KH
2pO
41.4%, (NH
4)
2sO
40.2%, MgSO
47H
2o0.02%, peptone 0.4%, yeast powder 0.02%, in culture fluid, the concentration of cAMP is 3.9%mg/150mL; CN100425620C discloses a kind of technique 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 adjust ph, after anion-exchange column, the eluent collected is by chromatographic column (silica gel type, or macroporous resin type, or polyamide), then with water or ethanol water eluting, add dehydrated alcohol crystallization after eluent is concentrated, obtain high-purity cyclic adenosine monophosphate powder.
But 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 employs 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 be separated, uses and also has certain limitation.The equipment major part that conventional extracting method adopts is unit batch, is difficult to the scale forming continuous prodution, affects leaching process standardized process.
Visible, the technical problem such as large for the solvent-oil ratio existed in prior art, the cycle is long, automatization level is low, and 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-content jujube cyclic adenosine monophosphate extract.
Another technical problem to be solved by this invention is the preparation method providing above-mentioned high-content jujube cyclic adenosine monophosphate extract.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A kind of high-content jujube cyclic adenosine monophosphate extract, in described extract, the concentration of cyclic adenosine monophosphate is every more than 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: adopt the solid of Fructus Jujubae or semi-solid raw material, extract through High Pressure Difference continuous low-temperature extractor, 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-content jujube cyclic adenosine monophosphate extract, adopts the solid of Fructus Jujubae or semi-solid raw material, extracts through High Pressure Difference continuous low-temperature extractor, 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-content jujube cyclic adenosine monophosphate extract.
Preferably, the preparation method of above-mentioned high-content jujube cyclic adenosine monophosphate extract, concrete steps are as follows:
(1) place material: choosing water content at the Fructus Jujubae of 5-30% is raw material, pulverize raw material, make particle diameter be 180-850 μm (80-24 order);
(2) evacuation: under response system temperature-10-0 DEG C of condition, vacuum is formed in High Pressure Difference continuous low-temperature extractor, vacuum remains on-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) pressurize: continue to pass into compressed air, make the pressure in High Pressure Difference continuous low-temperature extractor reach 8-12Mpa, keep 1-20min;
(5) reduce pressure: stop pressurization, evacuation, make Pressure Drop in High Pressure Difference continuous low-temperature extractor to 0Mpa;
(6) circulation is extracted: circulated step (2)-(5), circulate 10 times;
(7) be separated: by filter, centrifugal, make solid-liquid separation, collect extracting solution;
(8) dry: concentrated by step (7) gained extracting solution, vacuum drying, pulverized 20-80 mesh sieve, obtained crude extract powder;
(9) supercritical extraction: with 5-99%(v/v) ethanol makes entrainer and crude extract powder Homogeneous phase mixing, 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 DEG C, extraction time 0.5-5 hour, separating still pressure 5-30Mpa, separating still temperature 10-50 DEG C, 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-content jujube cyclic adenosine monophosphate extract, after pulverizing raw material in described step (1), the content of cyclic adenosine monophosphate is 0.01-0.08%.
Preferably, the preparation method of above-mentioned high-content jujube cyclic adenosine monophosphate extract, choosing water content in described step (1) at the Fructus Jujubae of 5-15% is raw material.
Preferably, the preparation method of above-mentioned high-content jujube cyclic adenosine monophosphate extract, choose in described step (1) water content 10% Fructus Jujubae be raw material, pulverize raw material, make particle diameter be 250 μm (65 orders).
Preferably, the preparation method of above-mentioned high-content jujube 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-content jujube cyclic adenosine monophosphate extract, the vacuum of described step (2) evacuation remains on-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-content jujube cyclic adenosine monophosphate extract, response system temperature-10-0 DEG C in described step (2) is realized by the cooling water in the condensation cycle system of High Pressure Difference continuous low-temperature extractor periphery.
Preferably, the preparation method of above-mentioned high-content jujube cyclic adenosine monophosphate extract, described cooling water is 95%(v/v) ethanol.
Preferably, the preparation method of above-mentioned high-content jujube cyclic adenosine monophosphate extract, the pressure that described step (4) is pressurizeed reaches 11Mpa, keeps 15min.
Preferably, the preparation method of above-mentioned high-content jujube cyclic adenosine monophosphate extract, in described step (7) extracting solution be after solid-liquid separation through 400 object membrane filtrations to the centrifugal liquid of clarification.
Preferably, the preparation method of above-mentioned high-content jujube cyclic adenosine monophosphate extract, with 90%(v/v in described step (9)) ethanol makes entrainer and crude extract powder Homogeneous phase mixing, carry secretly than being 15%, after balance 30min, carry out dynamic extraction, at extraction kettle pressure 40Mpa, extraction temperature 37 DEG C, extraction time 5 hours, separating still pressure 6Mpa, separating still temperature 30 DEG C, 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-content jujube cyclic adenosine monophosphate extract, the cyclic adenosine monophosphate obtained can produce through conventional formulation processes the product obtaining the relevant dosage forms such as capsule, oral liquid, distillate medicinal water, granule, electuary, tablet further.
The invention has the beneficial effects as follows:
High-content jujube cyclic adenosine monophosphate extract of the present invention, anti-hypoxia, resisting fatigue, quality of making the life better aspect is remarkably productive, the preparation method of this high-content jujube cyclic adenosine monophosphate extract, raw material Fructus Jujubae is carried out cold drying process, 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, direct dissolving, thus reach the effect of high efficiency extraction, be separated by supercritical carbon dioxide extraction method again and obtain high yield, highly purified cyclic adenosine monophosphate (cAMP), the ethanol of certain concentration is adopted to make entrainer, alternative condition obtains with the cyclic adenosine monophosphate active component of high-load, its concentration is at more than 15mg/g, the quality raw materials of food or medicine.
Compared with existing extractive technique, the preparation method of high-content jujube cyclic adenosine monophosphate extract of the present invention has following obvious advantage:
(1) rate of transform is extracted high;
(2) production efficiency is high;
(3) quality controllability is high;
(4) controllable degree is operated high;
(5) comprehensive resource utilization 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-content jujube cyclic adenosine monophosphate extract.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme of the present invention is further described.
Embodiment 1
A kind of high-content jujube cyclic adenosine monophosphate extract, its concrete preparation process is as follows:
(1) material is placed: by the Hebei Cangzhou Golden Chinese Date 10kg of water content 10%, pulverized 65 mesh sieves, and made particle diameter 250 μm, and be placed in High Pressure Difference continuous low-temperature extractor;
(2) evacuation: cooling water (95%(v/v) ethanol by the condensation cycle system of High Pressure Difference continuous low-temperature extractor periphery) make response system temperature-7 DEG C of conditions under, vacuum is formed in High Pressure Difference continuous low-temperature extractor, vacuum remains on-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: the compressed air slowly passing into purification, make pressure in High Pressure Difference continuous low-temperature extractor rise to 0Mpa, the time is about 3min;
(4) pressurize: continue to pass into compressed air, make the pressure in High Pressure Difference continuous low-temperature extractor reach 11Mpa, keep 15min;
(5) reduce pressure: stop pressurization, open vent valve, evacuation, make Pressure Drop in High Pressure Difference continuous low-temperature extractor to 0Mpa;
(6) circulation is extracted: continue step (2)-(5), circulate 10 times;
(7) be separated: after filtration, centrifugal, by solid-liquid separation, centrifugal liquid to clarification, collects extracting solution through 400 object membrane filtrations;
(8) dry: concentrated by step (7) gained extracting solution, vacuum drying, pulverized 65 mesh sieves, obtained the crude extract powder of Fructus Jujubae;
(9) supercritical extraction: with 90%(v/v) ethanol makes entrainer and crude extract powder Homogeneous phase mixing, 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, extraction temperature 37 DEG C, extraction time 5 hours, separating still pressure 6Mpa, separating still temperature 30 DEG C, 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, high performance liquid chromatography detection is carried out to Fructus Jujubae cyclic adenosine monophosphate extract, wherein, chromatograph: by P200 II high pressure constant flow pump, the part such as UV200 II ultraviolet variable-wavelenght detector and Echrom98 chromatographic work station composition, sample treatment: accurately measure 10ml distilled water standardize solution in 50ml volumetric flask, shake up, centrifugal, 0.45 μm of membrane filtration, to obtain final product, chromatographic column: Hydersir BDS C18, mobile phase: 20mol/LKH
2pO
4-methanol (90:10), column temperature: 25 DEG C, determined wavelength: 254nm, 7 flow velocitys: 0.6mL/min, sample size: 10 μ L.As depicted in figs. 1 and 2, wherein Camp Content is the extract of 15mg/100g.
Embodiment 2
A kind of high-content jujube cyclic adenosine monophosphate extract, its concrete preparation process is as follows:
(1) place material: choose water content 5% grand snow jujube (Yimeng Mountain Area, Shandong Province) be raw material, pulverize raw material, make particle diameter be 180 μm (80 orders);
(2) evacuation: under response system temperature 0 DEG C of condition, form vacuum in High Pressure Difference continuous low-temperature extractor, vacuum remains on-100pa, adds aqueous solution, keep 30min, 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) pressurize: continue to pass into compressed air, make the pressure in High Pressure Difference continuous low-temperature extractor reach 12Mpa, keep 1min;
(5) reduce pressure: stop pressurization, evacuation, make Pressure Drop in High Pressure Difference continuous low-temperature extractor to 0Mpa;
(6) circulation is extracted: circulated step (2)-(5), circulate 10 times;
(7) be separated: by filter, centrifugal, make solid-liquid separation, collect extracting solution;
(8) dry: concentrated by step (7) gained extracting solution, vacuum drying, pulverized 80 mesh sieves, obtained crude extract powder;
(9) supercritical extraction: with 99%(v/v) ethanol makes entrainer and crude extract powder Homogeneous phase mixing, 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, extraction temperature 35 DEG C, extraction time 0.5 hour, separating still pressure 30Mpa, separating still temperature 10 DEG C, 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 kind of high-content jujube cyclic adenosine monophosphate extract, its concrete preparation process is as follows:
(1) place material: choose water content 30% Golden jujube (Cangzhou, Hebei) be raw material, pulverize raw material, make particle diameter be 850 μm (24 orders);
(2) evacuation: under response system temperature-10 DEG C of conditions, form vacuum in High Pressure Difference continuous low-temperature extractor, vacuum remains on-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) pressurize: continue to pass into compressed air, make the pressure in High Pressure Difference continuous low-temperature extractor reach 8Mpa, keep 20min;
(5) reduce pressure: stop pressurization, evacuation, make Pressure Drop in High Pressure Difference continuous low-temperature extractor to 0Mpa;
(6) circulation is extracted: circulated step (2)-(5), circulate 10 times;
(7) be separated: after filtration, centrifugal, by solid-liquid separation, centrifugal liquid to clarification, collects extracting solution through 400 object membrane filtrations;
(8) dry: concentrated by step (7) gained extracting solution, vacuum drying, pulverized 20 mesh sieves, obtained crude extract powder;
(9) supercritical extraction: with 5%(v/v) ethanol makes entrainer and crude extract powder Homogeneous phase mixing, 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, extraction temperature 60 DEG C, 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 kind of high-content jujube cyclic adenosine monophosphate extract, its concrete preparation process is as follows:
(1) place material: choose water content 15% Golden jujube be raw material, pulverize raw material, cross 65 mesh sieves;
(2) evacuation: under response system temperature-5 DEG C of conditions, form vacuum in High Pressure Difference continuous low-temperature extractor, vacuum remains on-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) pressurize: continue to pass into compressed air, make the pressure in High Pressure Difference continuous low-temperature extractor reach 10Mpa, keep 10min;
(5) reduce pressure: stop pressurization, evacuation, make Pressure Drop in High Pressure Difference continuous low-temperature extractor to 0Mpa;
(6) circulation is extracted: circulated step (2)-(5), circulate 10 times;
(7) be separated: after filtration, centrifugal, by solid-liquid separation, centrifugal liquid to clarification, collects extracting solution through 400 object membrane filtrations;
(8) dry: concentrated by step (7) gained extracting solution, vacuum drying, pulverized 40 mesh sieves, obtained crude extract powder;
(9) supercritical extraction: with 70%(v/v) ethanol makes entrainer and crude extract powder Homogeneous phase mixing, 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, extraction temperature 45 DEG C, extraction time 4 hours, separating still pressure 25Mpa, separating still temperature 40 DEG C, 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 kind of high-content jujube cyclic adenosine monophosphate extract, its concrete preparation process is as follows:
(1) place material: choose water content 20% Golden jujube be raw material, pulverize raw material, cross 40 mesh sieves;
(2) evacuation: under response system temperature-8 DEG C of conditions, form vacuum in High Pressure Difference continuous low-temperature extractor, vacuum remains on-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) pressurize: continue to pass into compressed air, make the pressure in High Pressure Difference continuous low-temperature extractor reach 12Mpa, keep 5min;
(5) reduce pressure: stop pressurization, evacuation, make Pressure Drop in High Pressure Difference continuous low-temperature extractor to 0Mpa;
(6) circulation is extracted: circulated step (2)-(5), circulate 10 times;
(7) be separated: after filtration, centrifugal, by solid-liquid separation, centrifugal liquid to clarification, collects extracting solution through 400 object membrane filtrations;
(8) dry: concentrated by step (7) gained extracting solution, vacuum drying, pulverized 65 mesh sieves, obtained crude extract powder;
(9) supercritical extraction: with 90%(v/v) ethanol makes entrainer and crude extract powder Homogeneous phase mixing, 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, extraction temperature 40 DEG C, extraction time 2.5 hours, separating still pressure 15Mpa, separating still temperature 20 DEG C, 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-content jujube cyclic adenosine monophosphate extract can be used for preparing liquid beverage, such as, gets gained high-content jujube cyclic adenosine monophosphate extract in 2g embodiment 1, is dissolved in 4L pure water, aseptic embedding, every bottle of 10mL.
Test as follows with high-content jujube cyclic adenosine monophosphate extract described in embodiment 1:
By the change of blood oxygen saturation, content of hemoglobin, Serum lactic acid content, blood urea nitrogen content before and after contrast test, the anti-hypoxia of high-content jujube cyclic adenosine monophosphate extract of the present invention, anti-fatigue effect are evaluated.
Employing Double-blind randomized clinical trial designs, and the trial volunteer 120 examples being met inclusive criteria/exclusion standard distributes according to the ratio of 1:1:1,120 people is divided at random high dose group, low dose group, blank group three groups.
The observation cycle is 40 days, and time window is ± 7 days, and detailed process is see table 1 clinical trial flow table.
Table 1 clinical trial flow table
Object of study: age, 16-25 year; Male.Adopt method of randomization, the 3 groups of armed policemans chosen from the same area are subjects.Three groups are divided at random, i.e. high dose test group, low dosage test group and blank group by group, wherein,
High dose test group is embodiment 1 gained Fructus Jujubae cyclic adenosine monophosphate extract,
Low dosage test group is solution after embodiment 1 gained Fructus Jujubae cyclic adenosine monophosphate extract distilled water diluting 2 times,
Blank group, is commercial high fructose syrup (Shanghai emergence sugar industry company limited),
Often organize number be 40 people, 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 lactase acid;
Secondary index: Evaluation on quality of life; Three kilometers are run time run.
Result of the test tests front and back index situation of change table, table 3 Evaluation on quality of life table in table 2, does not have the generation of untoward reaction and adverse events in process of the test.
Front and back index situation of change table tested by table 2
Through t inspection, 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, gender comparison no difference of science of statistics, has comparability.
Through t inspection, between three groups, the equal not statistically significant of drug allergy history difference, has comparability (p>0.05).
Check through T, before and after test, high dose group blood lactase 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 obviously reduce before comparatively treating, 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, have significant difference before and after matched group three kilometers of time run tests.Result shows to improve successful to LAC, BUN, HGB, blood oxygen saturation, three kilometers of time runs before and after the test of high and low dose group.
Through t inspection, after treatment, high-content jujube cyclic adenosine monophosphate extract high and low dose group compares with matched group, BUN, HGB, blood oxygen saturation comparing difference, not statistically significant, namely compares between group that to improve index degree difference not obvious; After treatment, three groups of LAC, three kilometers of race timing comparing differences have statistical significance.Namely high and low dose group comparatively matched group comparing difference have statistical significance, LAC, three kilometers run timing comparatively matched group reduce obviously.But comparing difference not statistically significant between high and low dose group.Statistical result shows, Fructus Jujubae cyclic adenosine monophosphate extract high and low dose group is to LAC and three kilometer of time run Be very effective compared with matched group, is obviously better than matched group, and does not have 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 in sleep, physical ability, appetite improvement, and low dose group also has certain effect in improving water flood.
Wherein, abbreviation that above-mentioned test uses is in table 4 abbreviation abridged table
Table 4 abbreviation abridged table
As can be seen from above-mentioned test, treat sex between first two groups, age, height, body weight, the equal not statistically significant of drug allergy history comparing difference, have comparability, comparitive study result shows:
Compare before and after treatment: 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 obviously reduce before comparatively treating, 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, have significant difference before and after matched group three kilometers of time run tests.
Compare between group: three groups of BUN, HGB, blood oxygen saturation comparing difference after test, not statistically significant, namely 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 relative 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 run timing comparatively matched group reduce obviously, but comparing difference not statistically significant between high and low dose group.
To sum up, can find out:
1) clinical experimental study is passed through, high-content jujube cyclic adenosine monophosphate extract high dose group is to blood lactase acid, blood urea nitrogen, hemoglobin, blood oxygen saturation, three kilometers of time runs, before and after test, change is variant, there is significant difference, and especially outstanding on the impact of blood lactase 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-content jujube cyclic adenosine monophosphate extract low dose group has impact to before and after HGB, blood oxygen saturation test, but does not have statistical significance, is changed significantly, has statistical significance to blood lactase acid, blood urea nitrogen, three kilometers of race timing; The improvement of low dose group to sleep quality has certain help, does not have significant difference to the improvement of physical ability and appetite with matched group ratio.
3) compare with matched group, high and low dose group has statistical significance to blood lactase acid change, and wherein high dose group has remarkable statistical significance; The impact of high and low dose group on three kilometers of time runs has significant difference, and compares not statistically significant between high and low dose group.To other index blood urea nitrogen, hemoglobin, blood oxygen saturation three indexs, self compare before and after test and have statistical significance, comparing with matched group does not have statistical significance.
Result of the test shows, high-content jujube cyclic adenosine monophosphate extract high and low dose grouping machine body anoxia and the lactic acid, blood urea nitrogen etc. that produce in body in moving have good elimination effect, especially have more outstanding effect to the elimination of lactic acid.By reducing the generation of lactic acid or accelerating the elimination of lactic acid, reduce the fatigue factor in body, thus reach the effect of anti-hypoxia, fatigue alleviating.And by comprehensive regulating action to the hemoglobin, blood oxygen saturation, sleep etc. of body, reach the effect of a comprehensive improvement body body constitution.
Above-mentioned detailed description of this kind of high-content jujube cyclic adenosine monophosphate extract and preparation method thereof being carried out with reference to embodiment; illustrative instead of determinate; several embodiments can be listed according to institute's limited range; therefore in the change do not departed under general plotting of the present invention and amendment, should belong within protection scope of the present invention.
Claims (9)
1. a high-content jujube 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: adopt the solid of Fructus Jujubae or semi-solid raw material, extract through High Pressure Difference continuous low-temperature extractor, 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, concrete steps are as follows:
(1) place material: choosing water content at the Fructus Jujubae of 5-30% is raw material, pulverize raw material, make particle diameter be 180-850 μm;
(2) evacuation: under response system temperature-10-0 DEG C of condition, make to form vacuum in High Pressure Difference continuous low-temperature extractor, vacuum remains on-100--20Pa, add water or 5-70% (v/v) ethanol water, keep 5-30min, wherein, the weight ratio of described raw material and water or 5-70% (v/v) 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) pressurize: continue to pass into compressed air, make the pressure in High Pressure Difference continuous low-temperature extractor reach 8-12MPa, keep 1-20min;
(5) reduce pressure: stop pressurization, evacuation, make Pressure Drop in High Pressure Difference continuous low-temperature extractor to 0MPa;
(6) circulation is extracted: circulated step (2)-(5), circulate 10 times;
(7) be separated: by filter, centrifugal, make solid-liquid separation, collect extracting solution;
(8) dry: concentrated by step (7) gained extracting solution, vacuum drying, pulverized 20-80 mesh sieve, obtained crude extract powder;
(9) supercritical extraction: make entrainer and crude extract powder Homogeneous phase mixing with 5-99% (v/v) ethanol, carry secretly than being 8-15%, after balance 10-30min, carry out dynamic extraction, at extraction kettle pressure 15-60MPa, extraction temperature 35-60 DEG C, extraction time 0.5-5 hour, separating still pressure 5-30MPa, separating still temperature 10-50 DEG C, 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.
2. the preparation method of Fructus Jujubae cyclic adenosine monophosphate extract according to claim 1, is characterized in that: adopt the solid of Fructus Jujubae or semi-solid raw material, extracts through High Pressure Difference continuous low-temperature extractor, 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 Fructus Jujubae cyclic adenosine monophosphate extract, concrete steps are as follows:
(1) place material: choosing water content at the Fructus Jujubae of 5-30% is raw material, pulverize raw material, make particle diameter be 180-850 μm;
(2) evacuation: under response system temperature-10-0 DEG C of condition, make to form vacuum in High Pressure Difference continuous low-temperature extractor, vacuum remains on-100--20Pa, add water or 5-70% (v/v) ethanol water, keep 5-30min, wherein, the weight ratio of described raw material and water or 5-70% (v/v) 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) pressurize: continue to pass into compressed air, make the pressure in High Pressure Difference continuous low-temperature extractor reach 8-12MPa, keep 1-20min;
(5) reduce pressure: stop pressurization, evacuation, make Pressure Drop in High Pressure Difference continuous low-temperature extractor to 0MPa;
(6) circulation is extracted: circulated step (2)-(5), circulate 10 times;
(7) be separated: by filter, centrifugal, make solid-liquid separation, collect extracting solution;
(8) dry: concentrated by step (7) gained extracting solution, vacuum drying, pulverized 20-80 mesh sieve, obtained crude extract powder;
(9) supercritical extraction: make entrainer and crude extract powder Homogeneous phase mixing with 5-99% (v/v) ethanol, carry secretly than being 8-15%, after balance 10-30min, carry out dynamic extraction, at extraction kettle pressure 15-60MPa, extraction temperature 35-60 DEG C, extraction time 0.5-5 hour, separating still pressure 5-30MPa, separating still temperature 10-50 DEG C, 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.
3. the preparation method of Fructus Jujubae cyclic adenosine monophosphate extract according to claim 2, is characterized in that: choosing water content in described step (1) at the Fructus Jujubae of 5-15% is raw material.
4. the preparation method of the Fructus Jujubae cyclic adenosine monophosphate extract according to Claims 2 or 3, is characterized in that: choose in described step (1) water content 10% Fructus Jujubae be raw material, pulverize raw material, make particle diameter be 250 μm.
5. the preparation method of Fructus Jujubae cyclic adenosine monophosphate extract according to claim 2, it is characterized in that: the vacuum of described step (2) evacuation remains on-70Pa, add 50% (v/v) ethanol water, keep 20min, wherein, the weight ratio of described raw material and 50% (v/v) ethanol water is 1:10; Response system temperature-10-0 DEG C in described step (2) is realized by the cooling water in the condensation cycle system of High Pressure Difference continuous low-temperature extractor periphery.
6. the preparation method of Fructus Jujubae cyclic adenosine monophosphate extract according to claim 5, is characterized in that: described cooling water is 95% (v/v) ethanol.
7. the preparation method of Fructus Jujubae cyclic adenosine monophosphate extract according to claim 2, is characterized in that: the pressure that described step (4) is pressurizeed reaches 11MPa, keeps 15min.
8. the preparation method of Fructus Jujubae cyclic adenosine monophosphate extract according to claim 2, is characterized in that: in described step (7) extracting solution be after solid-liquid separation through 400 object membrane filtrations to the centrifugal liquid of clarification.
9. the preparation method of Fructus Jujubae cyclic adenosine monophosphate extract according to claim 2, it is characterized in that: in described step (9), make entrainer and crude extract powder Homogeneous phase mixing with 90% (v/v) ethanol, carry secretly than being 15%, after balance 30min, carry out dynamic extraction, at extraction kettle pressure 40MPa, extraction temperature 37 DEG C, extraction time 5 hours, separating still pressure 6MPa, separating still temperature 30 DEG C, 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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