CN113072479A - Method for extracting melatonin from melatonin crystallization mother liquor - Google Patents
Method for extracting melatonin from melatonin crystallization mother liquor Download PDFInfo
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- CN113072479A CN113072479A CN202110322825.5A CN202110322825A CN113072479A CN 113072479 A CN113072479 A CN 113072479A CN 202110322825 A CN202110322825 A CN 202110322825A CN 113072479 A CN113072479 A CN 113072479A
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- melatonin
- mother liquor
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- crystallization mother
- extraction
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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
Abstract
The invention discloses a method for extracting melatonin from melatonin crystallization mother liquor, which comprises the following steps of firstly, freezing pine cone bodies of animals; step two, crushing the frozen pinecone in the step one; step three, adding hot water into the crushed pinecone in the step two, and centrifuging and standing by using a centrifugal machine; step four, taking the supernatant of the centrifugate in the step three; step five, filtering the supernatant obtained in the step four, and filtering out redundant impurities; step six, adding propylene glycol into the filtered supernatant obtained in the step five for extraction; heating the extraction liquid in the step six to evaporate propylene glycol in the extraction liquid so as to separate out melatonin crystals in the extraction liquid; according to the invention, hot water is added into the crushed pinecone, so that melatonin is separated out more favorably, and unnecessary waste is reduced.
Description
Technical Field
The invention relates to the technical field of melatonin extraction, in particular to a method for extracting melatonin from a melatonin crystallization mother liquor.
Background
Melatonin is a substance secreted by the pineal body of the human brain and has very important functions on maintaining the normal circadian rhythm and sleep rhythm of the human body. If the melatonin secretion is disturbed, the sleep time of a person can be reversed, the sleep quality can be deteriorated, and the person can have insomnia. The invention discloses a melatonin separation process which is invented in China with application number 201610845424.7, wherein crushed walnuts are directly extracted during extraction, waste is easily caused, impurities are filtered after extraction, and the extraction effect is easily influenced, so that a method for extracting melatonin from a melatonin crystallization mother liquor is provided for solving the problems.
Disclosure of Invention
The present invention aims at providing a method for extracting melatonin from a melatonin crystallization mother liquor, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a method for extracting melatonin from a melatonin crystallization mother liquor comprises the following extraction steps:
step one, freezing pineal bodies of animals;
step two, crushing the frozen pinecone in the step one;
step three, adding hot water into the crushed pinecone in the step two, and centrifuging and standing by using a centrifugal machine;
step four, taking the supernatant of the centrifugate in the step three;
step five, filtering the supernatant obtained in the step four, and filtering out redundant impurities;
step six, adding propylene glycol into the filtered supernatant obtained in the step five for extraction;
heating the extraction liquid in the step six to evaporate propylene glycol in the extraction liquid so as to separate out melatonin crystals in the extraction liquid;
step eight, drying the melatonin crystals obtained in the step seven;
and step nine, crushing the melatonin crystals dried in the step eight.
Preferably, the temperature of the hot water in the third step is 80-100 ℃.
Preferably, the rotating speed of the centrifuge in the third step is 8000r/min, and the standing time in the third step is 30 min.
Preferably, the heating temperature in the seventh step is between 200 ℃ and 400 ℃.
Preferably, in the fifth step, a nanofiltration membrane is used for filtering the supernatant.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, hot water is added into the crushed pinecone, so that melatonin can be separated out more easily, and unnecessary waste is reduced;
2. the invention puts the crushed pinecone body added with hot water into a centrifuge for centrifugal standing, which is beneficial to filtering out irrelevant impurities in advance;
3. the invention adopts a nanofiltration membrane to filter the supernatant obtained by centrifugation before extraction, further removes the impurities of the crushed pineal bodies, and improves the extraction effect in the next step.
Drawings
Fig. 1 is a flow chart of the melatonin extraction process of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a technical solution: a method for extracting melatonin from a melatonin crystallization mother liquor comprises the following extraction steps:
step one, freezing pineal bodies of animals;
step two, crushing the frozen pinecone in the step one;
step three, adding hot water into the crushed pinecone in the step two, and centrifuging and standing by using a centrifugal machine;
step four, taking the supernatant of the centrifugate in the step three;
step five, filtering the supernatant obtained in the step four, and filtering out redundant impurities;
step six, adding propylene glycol into the filtered supernatant obtained in the step five for extraction;
heating the extraction liquid in the step six to evaporate propylene glycol in the extraction liquid so as to separate out melatonin crystals in the extraction liquid;
step eight, drying the melatonin crystals obtained in the step seven;
and step nine, crushing the melatonin crystals dried in the step eight.
As a technical optimization scheme of the invention, the temperature of hot water in the third step is 80-100 ℃, melatonin is easy to dissolve in the hot water, and by adding the hot water into the crushed pinecone, the separation of the melatonin is facilitated, and unnecessary waste is reduced.
As a technical optimization scheme of the invention, the rotating speed of the centrifuge in the third step is 8000r/min, and the standing time in the third step is 30 min.
As a technical optimization scheme of the invention, the heating temperature in the step seven is between 200-400 ℃, the propylene glycol is evaporated when the temperature exceeds 200 ℃, the propylene glycol is evaporated by heating the extraction liquid obtained in the step six, and the melatonin begins to crystallize under the condition of over-saturation after the solvent is reduced.
As a technical optimization scheme of the invention, the supernatant is filtered by using a nanofiltration membrane in the fifth step, and the supernatant is filtered before extraction, so that impurities of crushed pineal bodies can be removed, and the extraction effect in the next step is improved.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A method for extracting melatonin from a melatonin crystallization mother liquor is characterized by comprising the following steps: the extraction steps are as follows:
step one, freezing pineal bodies of animals;
step two, crushing the frozen pinecone in the step one;
step three, adding hot water into the crushed pinecone in the step two, and centrifuging and standing by using a centrifugal machine;
step four, taking the supernatant of the centrifugate in the step three;
step five, filtering the supernatant obtained in the step four, and filtering out redundant impurities;
step six, adding propylene glycol into the filtered supernatant obtained in the step five for extraction;
heating the extraction liquid in the step six to evaporate propylene glycol in the extraction liquid so as to separate out melatonin crystals in the extraction liquid;
step eight, drying the melatonin crystals obtained in the step seven;
and step nine, crushing the melatonin crystals dried in the step eight.
2. The method for extracting melatonin from melatonin crystallization mother liquor as claimed in claim 1, wherein: the temperature of the hot water in the third step is 80-100 ℃.
3. The method for extracting melatonin from melatonin crystallization mother liquor as claimed in claim 1, wherein: the rotating speed of the centrifuge in the third step is 8000r/min, and the standing time in the third step is 30 min.
4. The method for extracting melatonin from melatonin crystallization mother liquor as claimed in claim 1, wherein: the heating temperature in the seventh step is between 200 ℃ and 400 ℃.
5. The method for extracting melatonin from melatonin crystallization mother liquor as claimed in claim 1, wherein: and in the fifth step, a nanofiltration membrane is used for filtering the supernatant.
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| CN202110322825.5A CN113072479A (en) | 2021-03-26 | 2021-03-26 | Method for extracting melatonin from melatonin crystallization mother liquor |
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| CN202110322825.5A CN113072479A (en) | 2021-03-26 | 2021-03-26 | Method for extracting melatonin from melatonin crystallization mother liquor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115152835A (en) * | 2022-07-05 | 2022-10-11 | 贵阳学院 | Method for preserving Dictyophora rubrovalvata by using melatonin |
| 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 (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5498423A (en) * | 1991-05-09 | 1996-03-12 | Neurim Pharmaceuticals (1991) Ltd. | Method for correcting plasma melatonin levels and pharmaceutical formulation comprising melatonin |
| JPH10101644A (en) * | 1996-09-26 | 1998-04-21 | Iyaku Bunshi Sekkei Kenkyusho:Kk | Pineal hormone agonist |
| JPH1112252A (en) * | 1997-06-19 | 1999-01-19 | Noriko Kaneshiro | Extraction of melatonin |
| CN104230742A (en) * | 2014-08-14 | 2014-12-24 | 广东东阳光药业有限公司 | Naphthalene derivatives and application of naphthalene derivatives to medicine |
| US20160053009A1 (en) * | 2013-03-15 | 2016-02-25 | Salimetrics, Llc | Melatonin monoclonal antibody, detection, methods and uses thereof |
| CN106543068A (en) * | 2016-09-24 | 2017-03-29 | 合肥信达膜科技有限公司 | A kind of melatonin separating technology |
| 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 |
| CN110229092A (en) * | 2019-06-03 | 2019-09-13 | 罗田县新普生药业有限公司 | A kind of method of efficient production epiphysin |
| US20200407327A1 (en) * | 2019-05-31 | 2020-12-31 | Ikena Oncology, Inc. | Tead inhibitors and uses thereof |
| WO2021038601A1 (en) * | 2019-08-30 | 2021-03-04 | Vijayendrakumar Virendrakumarji Redasani | Liquid pharmaceutical compositions of melatonin for oral and parenteral administration |
-
2021
- 2021-03-26 CN CN202110322825.5A patent/CN113072479A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5498423A (en) * | 1991-05-09 | 1996-03-12 | Neurim Pharmaceuticals (1991) Ltd. | Method for correcting plasma melatonin levels and pharmaceutical formulation comprising melatonin |
| JPH10101644A (en) * | 1996-09-26 | 1998-04-21 | Iyaku Bunshi Sekkei Kenkyusho:Kk | Pineal hormone agonist |
| JPH1112252A (en) * | 1997-06-19 | 1999-01-19 | Noriko Kaneshiro | Extraction of melatonin |
| US20160053009A1 (en) * | 2013-03-15 | 2016-02-25 | Salimetrics, Llc | Melatonin monoclonal antibody, detection, methods and uses thereof |
| CN104230742A (en) * | 2014-08-14 | 2014-12-24 | 广东东阳光药业有限公司 | Naphthalene derivatives and application of naphthalene derivatives to medicine |
| CN106543068A (en) * | 2016-09-24 | 2017-03-29 | 合肥信达膜科技有限公司 | A kind of melatonin separating technology |
| 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 |
| US20200407327A1 (en) * | 2019-05-31 | 2020-12-31 | Ikena Oncology, Inc. | Tead inhibitors and uses thereof |
| CN110229092A (en) * | 2019-06-03 | 2019-09-13 | 罗田县新普生药业有限公司 | A kind of method of efficient production epiphysin |
| WO2021038601A1 (en) * | 2019-08-30 | 2021-03-04 | Vijayendrakumar Virendrakumarji Redasani | Liquid pharmaceutical compositions of melatonin for oral and parenteral administration |
Non-Patent Citations (2)
| Title |
|---|
| 占今舜;张彬;: "浅谈褪黑素在动物生产中的应用", 饲料博览, no. 07, pages 41 - 43 * |
| 杨一思;杨鹏;张;: "医药保健品褪黑素工业合成路线的探究", 黄冈师范学院学报, no. 06, pages 22 - 25 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115152835A (en) * | 2022-07-05 | 2022-10-11 | 贵阳学院 | Method for preserving Dictyophora rubrovalvata by using melatonin |
| 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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