CN102382161A - Method for extracting red date cyclic adenosine monophosphate through ultrasonic composite membrane technology - Google Patents
Method for extracting red date cyclic adenosine monophosphate through ultrasonic composite membrane technology Download PDFInfo
- Publication number
- CN102382161A CN102382161A CN2011102471104A CN201110247110A CN102382161A CN 102382161 A CN102382161 A CN 102382161A CN 2011102471104 A CN2011102471104 A CN 2011102471104A CN 201110247110 A CN201110247110 A CN 201110247110A CN 102382161 A CN102382161 A CN 102382161A
- Authority
- CN
- China
- Prior art keywords
- red date
- extraction
- membrane
- cyclic monophosphate
- ultrasonic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention relates to a method for extracting red date cyclic adenosine monophosphate through an ultrasonic composite membrane technology. The method solves the problem that the existing extraction technology has the defects of complex processes, low extraction rate, high industrialization difficulty and low product purity. The method comprises the following steps of removing date pits of cleaned red dates, crushing the red dates obtained by the previous step, adding an appropriate amount of an ethanol solvent into the crushed red dates, carrying out ultrasonic reinforcement extraction, repeatedly carrying out ultrasonic extraction of extracted filter residues, merging the extract obtained by the previous step, removing macromolecules of bacteria, proteins, pectin, polysaccharides and starch, and monosaccharides of glucose and fructose respectively through ultrafiltration and nanofiltration, intercepting cyclic adenosine monophosphate-rich concentrate, and carrying out pressure reduction condensation and spray drying to obtain 30% of a powdery cyclic adenosine monophosphate crude product. The method provided by the invention is easy for operation, is convenient for extraction, is fast, has short extraction time and a high cyclic adenosine monophosphate extraction rate, and is suitable for industrialized production. A product obtained by the method has high purity, is purely natural and does not produce chemical pollution. Therefore, the method provides an effective approach for comprehensive development of red date further processing.
Description
Technical field
The present invention relates to the method for extracts active ingredients and exploitation in a kind of natural product, be specially and use ULTRASONIC COMPLEX membrane technique art from red date, to extract the method for cyclic monophosphate.
Background technology
Red date is the fruit of Rhamnaceae (Rhamnaceae) jujube jujube tree (Ziziphus Jujuba Mill); Originate in China; In the artificial culture history in existing 5000 of China, high nutritive value and good medical care effect are arranged, in the date except that containing a large amount of fructose and glucose; Also contain a certain amount of oligose and polysaccharide; Abundant vitamins C, cyclic monophosphate (cAMP) and cyclic guanosine monophosphate (cGMP) also have nutritive elements such as a certain amount of amino acid, VITAMINs, mineral element, and wherein cyclic monophosphate is the highest in the content in the known plants.Cyclic monophosphate (cAMP) is intracellular second messenger; Depend on the protein kinase of cAMP through activation; Take various adjusting information to target site specific in the cell; The important physical effects such as activity, genetic expression, cell fission and differentiation of performance regulatory enzyme, can be anticancer with the treatment cardiovascular disorder etc.At present cyclic monophosphate mainly obtains through chemical synthesis, the cyclic monophosphate that chemical synthesis is produced exist cost high with problems such as security is low, the extraction cyclic monophosphate can this type of problem of fine solution from the natural phant date.In the existing extractive technique, the extraction of red date cyclic monophosphate is mainly traditional decocting method and water extraction, and separation method mainly adopts ion exchange column, series of strata method etc., and there is long, problem such as extraction yield is low, complex process, product yield are low of extraction time in this method.
Ultrasound assisted extraction technique and membrane separation technique are 21 century biologically active substance separation and Extraction field new techniques.Supersound extraction can shorten leaching time greatly, improves leaching rate, particularly for the low temperature leaching of heat-sensitive ingredients, shows the special technique advantage.Membrane separation technique has realized the separating substances of molecular level, separates to belong to physical process, does not have phase transformation, and materials quality is protected greatly, and the operation continuity is strong, and yield is high, and material concentration can control arbitrarily in broad model a side gate of an imperial palace.At present; Domestic do not have as yet ultrasonic technique is matched acting in conjunction in the extraction of red date cyclic monophosphate with membrane separation technique; In view of the various advantages of ultrasound assisted extraction technique and membrane separation technique and in the suitability of red date cyclic monophosphate, this preparation method will have development potentiality.
Summary of the invention
The invention solves problems such as existing technology extraction process is complicated, extraction yield is low, the industriallization difficulty is big, product purity is low, the method for the ULTRASONIC COMPLEX membrane technique extraction red date cyclic monophosphate that is suitable for suitability for industrialized production that a kind of product purity content is high, extraction yield is high, technology is simple, production cost is low is provided.
The technical scheme that the present invention adopts is: a kind of ULTRASONIC COMPLEX membrane technique extracts the method for red date cyclic monophosphate, it is characterized in that may further comprise the steps:
(1) red date of cleaning being added adequate amount of ethanol solution pulls an oar;
(2) the red date slurry of step (1) being handled well carries out ultrasound-enhanced extraction;
(3) extracting solution that step (2) is obtained carries out coarse filtration, obtains jujube juice and filter residue respectively;
(4) filter residue that step (2) is obtained is supersound extraction repeatedly;
(5) step (3) and step (4) gained jujube juice are merged, carry out uf processing;
(6) step (5) gained is seen through liquid and carry out the nanofiltration processing;
(7) step (6) is carried out the liquid concentrator that nanofiltration holds back and obtain containing the Powdered bullion of cyclic monophosphate through concentrating under reduced pressure and spraying drying.
In the said step (1), the red date particle size after cracking is 5～20 orders, and the concentration of ethanolic soln is 0%～95%, and add-on is 4～16 ml/g red dates; Ultrasonic frequency is 20kHZ～100kHz in the said step (2), and intensity is 0.1～0.5W/cm2, and temperature is 25 ℃～65 ℃, and extraction time is 10 min～100min; Ultransonic repeatedly number of times is 1～5 time in the said step (4), extraction conditions such as step (2); In the said step (5), carry out uf processing, the material of said film is polysulfones, polyethersulfone or aromatic polyamides, molecular weight cut-off 6000, and WP is 0.2～0.5MPa, temperature is 35～45 ℃; Feed nitrogen in the ultrafiltration system discontinuous, form the gas-liquid stream of pulses, the cycle be ventilation in 1 hour once, each 1 minute; In the said step (6), during nanofiltration was handled, the material of said film was polysulfones, polyethersulfone or aromatic polyamides, and molecular weight cut-off is 300～1000, and WP is 0.5～0.8MPa, and temperature is 35～45 ℃.
The present invention compared with prior art has the following advantages:
L, the present invention are raw material with the red date, adopt the ULTRASONIC COMPLEX membrane technique to extract, and have improved extraction yield and product purity content, and wherein, the cyclic monophosphate extraction yield can reach 95%, and cyclic monophosphate content is more than 30% in the bullion;
2, the present invention adopts ultrasonic technique, has shortened extraction time effectively, generally at 10 min～100min;
3, technical process is simple, and is easy to control.
Description of drawings
Fig. 1 is the liquid chromatogram of standard substance cAMP;
Fig. 2 is the liquid chromatogram of the cAMP bullion of employing technology extraction according to the invention.
Embodiment
Embodiment 1:
Extracting red date stone is cleaned pulverizing, and globule size is 5 orders, gets the 1000g red date, adds 15% ethanol 5000ml, and bath temperature is 25 ℃, and the supersound extraction time is 30 minutes, and ultrasonic frequency is 50kHz, and ultrasound intensity is 0.4W/cm
2, with the ultrasonic extracting solution coarse filtration that obtains, the extraction solvent that filter residue adds identical weight again repeats supersound extraction, carries out altogether 2 times, filters and merges all and extract jujube juice, amounts to 1350ml.
Jujube juice adopts the ultra-filtration membrane of molecular weight cut-off 6000 polysulfones materials to carry out ultrafiltration, and WP is 0.4MPa, and temperature is 35 ℃; Feed nitrogen in the ultrafiltration system discontinuous, form the gas-liquid stream of pulses, the cycle be ventilation in 1 hour once, each 1 minute; Adopting molecular weight cut-off is the nf membrane of 300～1000 polyethersulfones; Jujube juice to through ultra-filtration membrane is handled; WP is 0.8MPa, and temperature is 35 ℃, must contain the liquid concentrator solution 500ml of cyclic monophosphate; Get cyclic monophosphate bullion 200mg, content 31% through concentrating under reduced pressure and spraying drying again.
Embodiment 2:
Extracting red date stone is cleaned pulverizing, and globule size is 10 orders, gets the 1000g red date, adds 25% ethanol 4000ml, and bath temperature is 25 ℃, and the supersound extraction time is 25 minutes, and ultrasonic frequency is 25kHz, and ultrasound intensity is 0.3W/cm
2, with the ultrasonic extracting solution coarse filtration that obtains, the extraction solvent that filter residue adds identical weight again repeats supersound extraction, carries out altogether 3 times, filters and merges all and extract jujube juice, amounts to 1150ml.
Jujube juice adopts the ultra-filtration membrane of molecular weight cut-off 6000 polysulfones materials to carry out ultrafiltration, and WP is 0.3MPa, and temperature is 35 ℃; Feed nitrogen in the ultrafiltration system discontinuous, form the gas-liquid stream of pulses, the cycle be ventilation in 1 hour once, each 1 minute; Adopting molecular weight cut-off is the nf membrane of 300～1000 polyethersulfones; Jujube juice to through ultra-filtration membrane is handled; WP is 0.7MPa, and temperature is 30 ℃, must contain the liquid concentrator solution 500ml of cyclic monophosphate; Get cyclic monophosphate bullion 220mg, content 32% through concentrating under reduced pressure and spraying drying again.
Claims (8)
1. a ULTRASONIC COMPLEX membrane technique extracts the method for red date cyclic monophosphate, it is characterized in that may further comprise the steps:
(1), adds adequate amount of ethanol solution with extracting red date stone, the pulverizing cleaned;
(2) the red date slurry of step (1) being handled well carries out ultrasound-enhanced extraction;
(3) extracting solution that step (2) is obtained carries out coarse filtration, obtains jujube juice and filter residue respectively;
(4) filter residue that step (2) is obtained is supersound extraction repeatedly;
(5) step (3) and step (4) gained jujube juice are merged, carry out uf processing;
(6) step (5) gained is seen through liquid and carry out the nanofiltration processing;
(7) step (6) is carried out the liquid concentrator that nanofiltration holds back and obtain containing the Powdered bullion of cyclic monophosphate through concentrating under reduced pressure and spraying drying.
2. ULTRASONIC COMPLEX membrane technique according to claim 1 extracts the method for red date cyclic monophosphate, it is characterized in that in the step (1), the red date grinding particle size is 5～20 orders, and the concentration of ethanolic soln is 0%～95%, and add-on is 4～16 ml/g red dates.
3. ULTRASONIC COMPLEX membrane technique according to claim 1 and 2 extracts the method for red date cyclic monophosphate; It is characterized in that: ultrasonic frequency is 20kHZ～100kHz in the said step (2); Intensity is 0.1～0.5W/cm2, and temperature is 25 ℃～65 ℃, and extraction time is 10 min～100min.
4. ULTRASONIC COMPLEX membrane technique according to claim 1 extracts the method for red date cyclic monophosphate, and it is characterized in that: ultransonic repeatedly number of times is 1～5 time in the said step (4), extraction conditions such as claim 3.
5. ULTRASONIC COMPLEX membrane technique according to claim 1 extracts the method for red date cyclic monophosphate; It is characterized in that: in the said step (5); Carry out uf processing, the material of said film is polysulfones, polyethersulfone or aromatic polyamides, molecular weight cut-off 6000; WP is 0.2～0.5MPa, and temperature is 35～45 ℃; Feed nitrogen in the ultrafiltration system discontinuous, form the gas-liquid stream of pulses, the cycle be ventilation in 1 hour once, each 1 minute.
6. ULTRASONIC COMPLEX membrane technique according to claim 1 extracts the method for red date cyclic monophosphate; It is characterized in that: in the said step (6); During nanofiltration was handled, the material of said film was polysulfones, polyethersulfone or aromatic polyamides, and molecular weight cut-off is 300～1000; WP is 0.5～0.8MPa, and temperature is 35～45 ℃.
7. extract the method for red date cyclic monophosphate according to claim 5,6 said ULTRASONIC COMPLEX membrane techniquies, it is characterized in that said ultra-filtration membrane and nf membrane are rolled film, hollow-fibre membrane or tubular membrane.
8. extract the method for red date cyclic monophosphate according to claim 5,6,7 described ULTRASONIC COMPLEX membrane techniquies; The step that it is characterized in that said cleaning ultra-filtration membrane and nf membrane does; Earlier use the hot water injection, clean respectively with acidic solution and basic soln again, make film recover membrane flux fully.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102471104A CN102382161A (en) | 2011-08-26 | 2011-08-26 | Method for extracting red date cyclic adenosine monophosphate through ultrasonic composite membrane technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102471104A CN102382161A (en) | 2011-08-26 | 2011-08-26 | Method for extracting red date cyclic adenosine monophosphate through ultrasonic composite membrane technology |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102382161A true CN102382161A (en) | 2012-03-21 |
Family
ID=45822048
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011102471104A Pending CN102382161A (en) | 2011-08-26 | 2011-08-26 | Method for extracting red date cyclic adenosine monophosphate through ultrasonic composite membrane technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102382161A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103374053A (en) * | 2012-04-12 | 2013-10-30 | 新疆农业大学 | Method for extracting cyclic adenosine monophosphate from red dates by ultrasonic waves |
| CN103585782A (en) * | 2013-11-26 | 2014-02-19 | 浙江安赛生物科技有限公司 | Method for preparing red date extract by utilizing ultrasonic cavitation technology |
| CN106074763A (en) * | 2016-07-29 | 2016-11-09 | 孙震 | A kind of Fructus Jujubae electromagnetic dissociation liquid Fructus Jujubae electromagnetic dissociation powder and preparation method and application |
| CN106188198A (en) * | 2016-07-14 | 2016-12-07 | 塔里木大学 | A kind of method of cAMP in high efficiency extraction Fructus Jujubae |
| CN107541440A (en) * | 2017-10-18 | 2018-01-05 | 湖州新驰医药科技有限公司 | A kind of preparation method of edible mushroom wine |
| CN109651471A (en) * | 2018-12-29 | 2019-04-19 | 河北科技大学 | The extracting method of cyclic adenosine monophosphate and cyclic guanosine monophosphate in jujube fruit |
| CN114656576A (en) * | 2022-03-09 | 2022-06-24 | 中国农业大学 | Cyclic adenosine monophosphate-Chinese date acidic polysaccharide compound and preparation method and application thereof |
| CN116262772A (en) * | 2021-12-14 | 2023-06-16 | 无棣县华龙食品有限公司 | Method for extracting cAMP in red jujube residues by water-alcohol double phase |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1948329A (en) * | 2006-11-09 | 2007-04-18 | 常月梅 | Technology of extracting adenosin phosphoric acid from date |
| CN101108871A (en) * | 2007-07-24 | 2008-01-23 | 天津欧瑞生物科技有限公司 | Technique for extracting cycli phosphate adenosine from chinese date |
| CN101525363A (en) * | 2009-04-24 | 2009-09-09 | 天津科技大学 | Method for extracting cyclic adenosine monophosphate (cAMP) from red jujubes |
| CN101643491A (en) * | 2009-09-07 | 2010-02-10 | 河南农业大学 | Method for extracting cyclic adenosine monophosphate from dates |
| CN102060900A (en) * | 2009-11-13 | 2011-05-18 | 天津市食品研究所有限公司 | Technological process for extracting cyclic adenosine monophosphate (CAMP) from red dates |
-
2011
- 2011-08-26 CN CN2011102471104A patent/CN102382161A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1948329A (en) * | 2006-11-09 | 2007-04-18 | 常月梅 | Technology of extracting adenosin phosphoric acid from date |
| CN101108871A (en) * | 2007-07-24 | 2008-01-23 | 天津欧瑞生物科技有限公司 | Technique for extracting cycli phosphate adenosine from chinese date |
| CN101525363A (en) * | 2009-04-24 | 2009-09-09 | 天津科技大学 | Method for extracting cyclic adenosine monophosphate (cAMP) from red jujubes |
| CN101643491A (en) * | 2009-09-07 | 2010-02-10 | 河南农业大学 | Method for extracting cyclic adenosine monophosphate from dates |
| CN102060900A (en) * | 2009-11-13 | 2011-05-18 | 天津市食品研究所有限公司 | Technological process for extracting cyclic adenosine monophosphate (CAMP) from red dates |
Non-Patent Citations (2)
| Title |
|---|
| 严静等: "超声波辅助提取赞皇枣环磷酸腺苷工艺研究", 《农产品加工·学刊》, no. 9, 30 September 2010 (2010-09-30), pages 48 - 51 * |
| 张岩等: "高效液相色谱法同时测定浓缩枣汁中环磷酸腺苷和环磷酸鸟苷的含量", 《食品科学》, vol. 30, no. 18, 31 December 2009 (2009-12-31), pages 321 - 322 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103374053A (en) * | 2012-04-12 | 2013-10-30 | 新疆农业大学 | Method for extracting cyclic adenosine monophosphate from red dates by ultrasonic waves |
| CN103585782A (en) * | 2013-11-26 | 2014-02-19 | 浙江安赛生物科技有限公司 | Method for preparing red date extract by utilizing ultrasonic cavitation technology |
| CN103585782B (en) * | 2013-11-26 | 2015-12-30 | 浙江安赛生物科技有限公司 | A kind of method utilizing ultrasonic cavitation technology to prepare red date extract |
| CN106188198A (en) * | 2016-07-14 | 2016-12-07 | 塔里木大学 | A kind of method of cAMP in high efficiency extraction Fructus Jujubae |
| CN106188198B (en) * | 2016-07-14 | 2018-09-11 | 塔里木大学 | A kind of method of cAMP in high efficiency extraction jujube |
| CN106074763A (en) * | 2016-07-29 | 2016-11-09 | 孙震 | A kind of Fructus Jujubae electromagnetic dissociation liquid Fructus Jujubae electromagnetic dissociation powder and preparation method and application |
| CN107541440A (en) * | 2017-10-18 | 2018-01-05 | 湖州新驰医药科技有限公司 | A kind of preparation method of edible mushroom wine |
| CN109651471A (en) * | 2018-12-29 | 2019-04-19 | 河北科技大学 | The extracting method of cyclic adenosine monophosphate and cyclic guanosine monophosphate in jujube fruit |
| CN116262772A (en) * | 2021-12-14 | 2023-06-16 | 无棣县华龙食品有限公司 | Method for extracting cAMP in red jujube residues by water-alcohol double phase |
| CN114656576A (en) * | 2022-03-09 | 2022-06-24 | 中国农业大学 | Cyclic adenosine monophosphate-Chinese date acidic polysaccharide compound and preparation method and application thereof |
| CN114656576B (en) * | 2022-03-09 | 2022-11-25 | 中国农业大学 | Cyclic adenosine monophosphate-Chinese date acidic polysaccharide compound and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102382161A (en) | Method for extracting red date cyclic adenosine monophosphate through ultrasonic composite membrane technology | |
| CN100503626C (en) | Producing raw material containing benzyl carbinol glycosides from Cistanche deserticola by using membrane separation technique and preparation method thereof | |
| CN103087128B (en) | A kind of method extracting peoniflorin from the peony seeds dregs of rice | |
| CN108752231B (en) | Method for extracting theanine from sweet tea and simultaneously extracting rubusoside and tea polyphenol | |
| CN102351956B (en) | Extraction method of morindea officinalis polysaccharide | |
| CN101133811B (en) | Shaddock genus olive, secondary fruit pericarp comprehensive utilization and process technique | |
| CN101731749B (en) | Ultrasonic zymohydrolysis extracting method for extracting tobacco perfumes from chrysanthemum natural plant flowers | |
| CN202124582U (en) | Membrane treatment system capable of extracting levodopa from velvet beans | |
| CN101781351B (en) | Method for extracting ginsenoside Rb1 from American ginseng and powder-injection thereof | |
| CN104069151B (en) | A kind of high method for preparing extractive of content of mogroside IV | |
| CN104961839A (en) | Preparation method of specific pachyman formula granule | |
| CN106810618A (en) | A kind of extraction from Chinese caterpillar fungus culture medium and the method for continuous polysaccharide enrichment | |
| CN101371856A (en) | Method and device for continuously extracting Chinese medicine effective ingredient at normal temperature | |
| CN102827299A (en) | Efficient extraction and purification method for kumquat polysaccharide | |
| CN102060856B (en) | Method for extracting tabersonine from voacanga seeds | |
| CN107721909B (en) | Method and system for continuously extracting DNJ, flavone and polysaccharide from Moraceae plant | |
| CN103274992A (en) | Method for preparing high-purity 1-deoxynojirimycin with combined membrane separation and column chromatography technology | |
| CN102382203A (en) | High-efficiency extraction process for polysaccharide of lotus seeds | |
| CN102180991B (en) | Comprehensive utilization method of pumpkin | |
| CN107056741A (en) | A kind of preparation technology of Application of Mulberry Anthocyanins powder | |
| CN104292281A (en) | Method for preparing high-purity rutin by using integrated technique | |
| CN101792394B (en) | Extraction separation method of L-synephrine | |
| CN103289969A (en) | Method for extracting superoxide dismutase from plant stem leaves | |
| CN110256597A (en) | A kind of method that embrane method reduces heavy-metal residual in ganoderma lucidum polysaccharide | |
| CN102391117A (en) | Method for preparing chlorogenic acid from eucommia leaves |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120321 |