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
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- YJPIGAIKUZMOQA-UHFFFAOYSA-N Melatonin Natural products COC1=CC=C2N(C(C)=O)C=C(CCN)C2=C1 YJPIGAIKUZMOQA-UHFFFAOYSA-N 0.000 title claims abstract description 46
- DRLFMBDRBRZALE-UHFFFAOYSA-N melatonin Chemical compound COC1=CC=C2NC=C(CCNC(C)=O)C2=C1 DRLFMBDRBRZALE-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229960003987 melatonin Drugs 0.000 title claims abstract description 46
- 238000002425 crystallisation Methods 0.000 title claims abstract description 13
- 230000008025 crystallization Effects 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title claims abstract description 13
- 239000012452 mother liquor Substances 0.000 title claims abstract description 13
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000000605 extraction Methods 0.000 claims abstract description 26
- 239000006228 supernatant Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 239000013078 crystal Substances 0.000 claims abstract description 10
- 210000004560 pineal gland Anatomy 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 8
- 241001465754 Metazoa Species 0.000 claims abstract description 4
- 230000008014 freezing Effects 0.000 claims abstract description 4
- 238000007710 freezing Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 4
- 238000001728 nano-filtration Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 239000002699 waste material Substances 0.000 abstract description 4
- 238000001556 precipitation Methods 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 238000005457 optimization Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 241000758791 Juglandaceae Species 0.000 description 1
- 208000013738 Sleep Initiation and Maintenance disease Diseases 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000027288 circadian rhythm Effects 0.000 description 1
- 206010022437 insomnia Diseases 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000033764 rhythmic process Effects 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 230000003860 sleep quality Effects 0.000 description 1
- 230000004622 sleep time Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 235000020234 walnut Nutrition 0.000 description 1
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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)
- Indole Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
本发明公开了一种从褪黑素结晶母液中提取褪黑素的方法，包括步骤一、取动物的松果体进行冷冻；步骤二、将步骤一中冷冻的松果体粉碎；步骤三、往步骤二中粉碎的松果体内加入热水并使用离心机进行离心静置；步骤四、取步骤三中离心液的上清液；步骤五、对步骤四中取得的上清液进行过滤，滤去多余杂质；步骤六、向步骤五中过滤后的上清液加入丙二醇进行萃取；步骤七、对步骤六中的萃取液进行加热，使萃取液中的丙二醇蒸发，使萃取液中的褪黑素晶体析出；本发明通过往粉碎的松果体内加入热水，更利于褪黑素的析出，减少不必要的浪费。
The invention discloses a method for extracting melatonin from melatonin crystallization mother liquor, which includes step 1, taking the pineal gland of an animal for freezing; step 2, pulverizing the pineal gland frozen in step 1; step 3, Add hot water to the pineal body crushed in step 2 and use a centrifuge to centrifuge and stand; step 4, take the supernatant of the centrifuge in step 3; step 5, filter the supernatant liquid obtained in step 4, Filter off excess impurities; step 6, add propylene glycol to the filtered supernatant in step 5 for extraction; step 7, heat the extract in step 6 to evaporate the propylene glycol in the extract, and make the extract in the extract fade. Melatonin crystals are precipitated; in the present invention, by adding hot water into the crushed pineal body, it is more conducive to the precipitation of melatonin and reduces unnecessary waste.
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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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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 (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 |
| CN115974756A (en) * | 2023-01-05 | 2023-04-18 | 福建科宏生物工程股份有限公司 | A kind of purification method of melatonin and its 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 |
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| 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 |
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| 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 |
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2021
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Cited By (4)
| 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 |
| CN115974756A (en) * | 2023-01-05 | 2023-04-18 | 福建科宏生物工程股份有限公司 | A kind of purification method of melatonin and its 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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