CN106543068A - A kind of melatonin separating technology - Google Patents
A kind of melatonin separating technology Download PDFInfo
- Publication number
- CN106543068A CN106543068A CN201610845424.7A CN201610845424A CN106543068A CN 106543068 A CN106543068 A CN 106543068A CN 201610845424 A CN201610845424 A CN 201610845424A CN 106543068 A CN106543068 A CN 106543068A
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- CN
- China
- Prior art keywords
- melatonin
- technology
- leaching
- semen juglandiss
- separating technology
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D209/00—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D209/02—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom condensed with one carbocyclic ring
- C07D209/04—Indoles; Hydrogenated indoles
- C07D209/10—Indoles; Hydrogenated indoles with substituted hydrocarbon radicals attached to carbon atoms of the hetero ring
- C07D209/14—Radicals substituted by nitrogen atoms, not forming part of a nitro radical
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a kind of melatonin separating technology, extraction process step includes：Step one, pretreatment；Step 2, crushing；Step 3, leaching；Step 4, film process；Step 5, desolventing technology；Step 6, revolving；Step 7, drying, filtering accuracy of the present invention are high, fundamentally ensure that the formedness of the degree of purity and quality of filtrate；Membrane process is pure physical process, and without phase transformation, energy consumption is low, and system is operated at normal temperatures, overcomes destruction of the heat to active substance in enzyme preparation product；Traditional filtering technique is compared, product quality is not only improved, and product yield and production efficiency have more significant raising.
Description
Technical field
The present invention relates to membrane technology field, particularly a kind of melatonin separating technology.
Background technology
Melatonin, is also called melatonin, peaceful U.S. drawing ketone, suppression melanocyte, melatonin, is the pine by mammal and the mankind
A kind of amine bormones that fruit body is produced, can make a kind of melanic cell of generation shinny, thus be named as melatonin.It is present
In numerous biologies such as from algae to the mankind, contents level is with daily time change.Research shows, human body melatonin after the middle age
Secretion start reduce, to old age, its secretory volume Yi Weibuzhong road.The enough melatonin of supplement are absorbed as early as possible, can improve interior
The function of excretory system, enhance immunity improve antitonic, antioxidative function, improve the health care of sleep, reducing human aging speed,
Slow down sexual organ's catagen speed for habitual insomnia etc. has substantially help especially.
The existing process production time is long, with the addition of a large amount of virose preservative and add flocculant in production, and flocculation is got off
Suspended impurity and activated carbon decolorizing absorb the product of part, yield is low；The suspension such as flocculant is removed using filter press miscellaneous
Matter, production environment are very poor, and production environment is extremely difficult to food additive production requirement；Production intermediate ion is exchanged and macroporous resin
It is a large amount of to use, expend substantial amounts of water resource and industrial chemicals resource, while the poisonous waste water of a large amount of resin eluting is difficult with life
Change is processed, and brings heavy financial burden and environmental protection pressure to enterprise.
The content of the invention
It is an object of the invention to provide a kind of melatonin separating technology.
A kind of melatonin separating technology, it is characterised in that extraction process step includes：
Step one, pretreatment：The Semen Juglandiss for obtaining are carried out into liquid nitrogen freezing process；
Step 2, crushing：Crushed after Semen Juglandiss after freezing are added leaching agent；
Step 3, leaching：Semen Juglandiss after crushing are extracted required composition repeatedly that leach in Semen Juglandiss, leachate is obtained；
Step 4, film process：The leachate for obtaining is processed by film, middle salinity and small-molecule substance is removed；
Step 5, desolventing technology：Leachate after film process is carried out into desolventing technology, is put in resin column, carry out desolventing technology；
Step 6, revolving：Leachate after desolventing technology is put in Rotary Evaporators carries out revolving process, by leaching therein
Agent is evaporated, and can be continuing with；
Step 7, drying：The melatonin for obtaining is put in drying baker and is dried, remove the leaching agent not eliminated.
Preferably, the Semen Juglandiss after freezing are crushed by the step 2 by waterproof pulverization.
Preferably, the step 3, is used as leaching agent by petroleum ether, and the Semen Juglandiss after crushing are carried out being put into ultrasound wave dress
Putting carries out leaching process, when being delivered in liquid by supersonic vibration, excites cavitation effect, substantial amounts of so as to produce in a liquid
Cavitation bubble, as these cavitation bubbles are produced and explosion, will produce microjet, and enter to be about to the great solid particle of liquid and hit
It is broken, simultaneously because the vibration of ultrasound wave, makes solid-liquid more fully mix, cell breakage is made, the extraction of cell inclusion is more
It is perfectly sound.
Preferably, the step 4, carries out concentrating and separating process by reverse osmosis membrane, using the Cotton Gossypii of cellulose, wood
Material etc. is raw material, makes acetic acid, Triafol T through esterification and hydrolysis（CA、CTA）, it is reprocessed into reverse osmosis membrane.
Preferably, the step 5, is processed by the ion exchange resin in resin column, and ion exchange resin is with benzene
Ethylene and the cross-linking products that divinylbenzene is skeleton, along with corresponding function group such as sulfonic group or quaternary ammonium, are porous
The skeleton of spongy texture, inside have a large amount of permanent micropores, then import cation exchange groups and make, and have minute aperture and big net
Hole, the aperture of wetting resin is up to 100～500nm.
Preferably, the step 7, is dried process by vacuum drier.
Advantages of the present invention：
1st, filtering accuracy is high, fundamentally ensure that the formedness of the degree of purity and quality of filtrate.
2nd, membrane process is pure physical process, and without phase transformation, energy consumption is low, and system is operated at normal temperatures, overcomes heat to enzyme preparation
The destruction of active substance in product.
3rd, compare traditional filtering technique, product quality is not only improved, and product yield and production efficiency have compared with
For significant raising.
4th, loss of effective components is reduced, reduces BOD and COD contents in waste water.With traditional filtration, concentration technology method phase
Inorganic salt in technical process, organic solvent can be significantly saved than, new technology, the production cost of product is reduced.
5th, the supporting control section advanced design of membranous system, so that the more aobvious simplicity of the operation and maintenance of system, significantly
Reduce the labor intensity of workman.
Description of the drawings
Implementing procedure figure of the accompanying drawing 1 for the present invention.
Specific embodiment
The present invention is further described in detail in conjunction with accompanying drawing 1 and specific embodiment.
Specific embodiment making step is as follows：
A kind of melatonin separating technology, it is characterised in that extraction process step includes：
Step one, pretreatment：The Semen Juglandiss for obtaining are carried out into liquid nitrogen freezing process；
Step 2, crushing：Crushed after Semen Juglandiss after freezing are added leaching agent；
Step 3, leaching：Semen Juglandiss after crushing are extracted required composition repeatedly that leach in Semen Juglandiss, leachate is obtained；
Step 4, film process：The leachate for obtaining is processed by film, middle salinity and small-molecule substance is removed；
Step 5, desolventing technology：Leachate after film process is carried out into desolventing technology, is put in resin column, carry out desolventing technology；
Step 6, revolving：Leachate after desolventing technology is put in Rotary Evaporators carries out revolving process, by leaching therein
Agent is evaporated, and can be continuing with；
Step 7, drying：The melatonin for obtaining is put in drying baker and is dried, remove the leaching agent not eliminated.
Semen Juglandiss after freezing are crushed by the step 2 by waterproof pulverization.The step 3, is made by petroleum ether
For leaching agent, the Semen Juglandiss after crushing are carried out being put into ultrasonic unit carries out leaching process, is delivered to liquid by supersonic vibration
When middle, cavitation effect is excited, so as to produce substantial amounts of cavitation bubble in a liquid, as these cavitation bubbles are produced and explosion,
Microjet will be produced, is entered to be about to the great solid particle of liquid and is smashed, simultaneously because the vibration of ultrasound wave, makes solid-liquid more abundant
Mixing, make cell breakage, the extraction of cell inclusion is more perfectly sound.The step 4, carries out concentration point by reverse osmosis membrane
From process, Cotton Gossypii, timber of cellulose etc. are adopted for raw material, make acetic acid, triacetate fiber through esterification and hydrolysis
Element（CA、CTA）, it is reprocessed into reverse osmosis membrane.The step 5, is processed by the ion exchange resin in resin column, from
Cross-linking products of the sub-exchange resin with styrene and divinylbenzene as skeleton, along with corresponding function group such as sulfonic group or
Quaternary ammonium, is the skeleton of mandruka columnar structure, and there are a large amount of permanent micropores inside, then imports cation exchange groups and make, and is had
Minute aperture and big mesh, the aperture of wetting resin is up to 100～500nm.The step 7, is dried place by vacuum drier
Reason.
The present invention specifically shows and describes the present invention with reference to preferred embodiment, it is clear that the present invention is implemented not
Limited by aforesaid way, as long as employing the various unsubstantialities improvement that method of the present invention design and technical scheme are carried out,
Or it is not improved the design of invention and technical scheme are directly applied to into other occasions, protection scope of the present invention it
It is interior.
Claims (6)
1. a kind of melatonin separating technology, it is characterised in that extraction process step includes：
Step one, pretreatment：The Semen Juglandiss for obtaining are carried out into liquid nitrogen freezing process；
Step 2, crushing：Crushed after Semen Juglandiss after freezing are added leaching agent；
Step 3, leaching：Semen Juglandiss after crushing are extracted required composition repeatedly that leach in Semen Juglandiss, leachate is obtained；
Step 4, film process：The leachate for obtaining is processed by film, middle salinity and small-molecule substance is removed；
Step 5, desolventing technology：Leachate after film process is carried out into desolventing technology, is put in resin column, carry out desolventing technology；
Step 6, revolving：Leachate after desolventing technology is put in Rotary Evaporators carries out revolving process, by leaching therein
Agent is evaporated, and can be continuing with；
Step 7, drying：The melatonin for obtaining is put in drying baker and is dried, remove the leaching agent not eliminated.
2. according to claims 1, a kind of melatonin separating technology, the step 2, after waterproof pulverization will be freezed
Semen Juglandiss crushed.
3., according to claims 1, a kind of melatonin separating technology, the step 3 are used as leaching agent by petroleum ether,
Semen Juglandiss after crushing are carried out being put into ultrasonic unit and carries out leaching process, when being delivered in liquid by supersonic vibration, excited
Cavitation effect, so as to produce substantial amounts of cavitation bubble in a liquid, as these cavitation bubbles are produced and explosion, will produce micro- penetrating
Stream, enters to be about to the great solid particle of liquid and smashes, simultaneously because the vibration of ultrasound wave, makes solid-liquid more fully mix, make
Cell breakage, the extraction of cell inclusion are more perfectly sound.
4., according to claims 1, a kind of melatonin separating technology, the step 4 are concentrated by reverse osmosis membrane
Separating treatment, adopts Cotton Gossypii, timber of cellulose etc. for raw material, makes acetic acid, three acetic acid through esterification and hydrolysis fine
Dimension element（CA、CTA）, it is reprocessed into reverse osmosis membrane.
5., according to claims 1, a kind of melatonin separating technology, the step 5 are handed over by the ion in resin column
Change resin to be processed, cross-linking products of the ion exchange resin with styrene and divinylbenzene as skeleton, along with corresponding work(
Energy group such as sulfonic group or quaternary ammonium, are the skeleton of mandruka columnar structure, and there are a large amount of permanent micropores inside, then imports
Cation exchange groups are made, and have minute aperture and a big mesh, and the aperture of wetting resin is up to 100～500nm.
6., according to claims 1, a kind of melatonin separating technology, the step 7 are done by vacuum drier
Dry process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610845424.7A CN106543068A (en) | 2016-09-24 | 2016-09-24 | A kind of melatonin separating technology |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610845424.7A CN106543068A (en) | 2016-09-24 | 2016-09-24 | A kind of melatonin separating technology |
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| CN106543068A true CN106543068A (en) | 2017-03-29 |
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| CN201610845424.7A Pending CN106543068A (en) | 2016-09-24 | 2016-09-24 | A kind of melatonin separating technology |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107382817A (en) * | 2017-08-20 | 2017-11-24 | 合肥信达膜科技有限公司 | A kind of inexpensive epiphysin separation method |
| CN113072479A (en) * | 2021-03-26 | 2021-07-06 | 罗田县新普生药业有限公司 | Method for extracting melatonin from melatonin crystallization mother liquor |
| CN116751149A (en) * | 2023-06-06 | 2023-09-15 | 北京逯博士行为医学科技研究院有限公司 | Preparation method of natural melatonin |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103859555A (en) * | 2012-12-18 | 2014-06-18 | 中国林业科学研究院林业研究所 | Method for removing walnut kernel pellicles |
| CN105038974A (en) * | 2015-08-09 | 2015-11-11 | 查光圣 | Pecan oil super-critical fluid extraction technology |
-
2016
- 2016-09-24 CN CN201610845424.7A patent/CN106543068A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103859555A (en) * | 2012-12-18 | 2014-06-18 | 中国林业科学研究院林业研究所 | Method for removing walnut kernel pellicles |
| CN105038974A (en) * | 2015-08-09 | 2015-11-11 | 查光圣 | Pecan oil super-critical fluid extraction technology |
Non-Patent Citations (3)
| Title |
|---|
| W.SETYANINGSIH ET AL.: "A new microwave-assisted extraction method for melatonin determination in rice grains", 《JOURNAL OF CEREAL SCIENCE》 * |
| 李敏等: "核桃营养价值研究进展", 《中国粮油学报》 * |
| 王俊儒: "《天然产物提取分离与鉴定技术》", 31 May 2005, 西北农林科技大学出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107382817A (en) * | 2017-08-20 | 2017-11-24 | 合肥信达膜科技有限公司 | A kind of inexpensive epiphysin separation method |
| CN113072479A (en) * | 2021-03-26 | 2021-07-06 | 罗田县新普生药业有限公司 | Method for extracting melatonin from melatonin crystallization mother liquor |
| CN116751149A (en) * | 2023-06-06 | 2023-09-15 | 北京逯博士行为医学科技研究院有限公司 | Preparation method of natural melatonin |
| CN116751149B (en) * | 2023-06-06 | 2024-03-15 | 北京逯博士行为医学科技研究院有限公司 | Preparation method of natural melatonin |
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Application publication date: 20170329 |