CN106565489A - Process for extracting rosmarinic acid from perilla - Google Patents
Process for extracting rosmarinic acid from perilla Download PDFInfo
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- CN106565489A CN106565489A CN201610886395.9A CN201610886395A CN106565489A CN 106565489 A CN106565489 A CN 106565489A CN 201610886395 A CN201610886395 A CN 201610886395A CN 106565489 A CN106565489 A CN 106565489A
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- eluent
- rosmarinic acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/56—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/58—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
Abstract
The invention discloses a process for extracting rosmarinic acid from perilla, belonging to the technical field of extraction of medicinal components of plants. The process comprises the following steps: crushing the perilla into coarse powder, then carrying out reflux extraction by utilizing ethyl alcohol with a concentration of 70%, subjecting an extracting solution to adsorption through resin D101, and carrying out alcohol washing so as to obtain a first eluent; subjecting the first eluent to adsorption through resin NK109, and carrying out alcohol washing so as to obtain a second eluent; and subjecting the second eluent to active carbon decoloration, adjusting the pH value of a decoloring solution, carrying out repeated extraction by utilizing ethyl acetate for 4 times, subjecting an ethyl acetate layer solution to low-temperature crystallization and recrystallization, and subjecting a crystal to drying so as to be able to obtain the rosmarinic acid with a content of 95 to 98%. The process for extracting the rosmarinic acid from the perilla disclosed by the invention has the characteristics of rapidness, low temperature, low energy consumption and high extraction rate, improves the extraction purity of the rosmarinic acid by utilizing the resin NK109 in a static adsorption method, and can prepare the rosmarinic acid with contents for different requirements at the same time.
Description
The invention belongs to the extractive technique field of plant efficacy component, and in particular to a kind of extraction work of purple common perilla rosemary acid
Skill.
【Background technology】
Folium Perillae be health ministry promulgate in the first batch be both food and one of the 60 of medicine kinds of Chinese medicine, Folium Perillae contains various
Chemical composition with physiologically active, and the non-oxidizability of Folium Perillae is the outstanding person in herbaceous plant, rosmarinic acid tool therein
There is very strong non-oxidizability.The wild Perilla of China and cultivation Perilla very abundant, how rational exploitation and utilization money
Source, becomes a problem of people's growing interest.Traditional rosmarinic acid extracting method has that standard deviation is big, extracted amount is few, carries
The problems such as toxic solvent, Product quality and safety are taken without guarantee, high cost.Research improves purple common perilla rosemary acid extraction rate, efficiency
And reduces cost, workable extracting method, the production to purple common perilla rosemary acid product is significant.
【The content of the invention】
The extraction process of a kind of purple common perilla rosemary acid that the present invention is provided, to solve traditional rosmarinic acid extracting method standard
Difference is big, extracted amount is few, Extraction solvent is poisonous, Product quality and safety without ensureing, high cost the problems such as, current Perilla exploitation profit
Use unreasonable problem.The extraction process of the present invention, separation and Extraction process is simple, extraction rate fast, efficiency high, low cost, utilizes
Static adsorptive method determines NK109 resins pole and is appropriate to the purification of rosmarinic acid, at the same can prepare various different demands into
Divide the rosmarinic acid of content, product yield is high, purity is high, meets the industrialization production requirements of rosmarinic acid.
To solve above technical problem, the present invention adopts following technical method：
A kind of extraction process of purple common perilla rosemary acid, comprises the following steps：
S1：It is coarse powder shape that Folium Perillae is crushed, and crosses 50 mesh sieves, the 70% of 8-12 times of its weight ethanol is added, in water-bath
Under the conditions of reflux, extract, after D101 macroporous resin adsorption, the ethanol of Jing 70% eluting at 70 DEG C is obtained once extracting solution
Eluent；
S2：By an eluent in step S1 after NK109 resin absorptioies, the ethanol of Jing 70% is washed at 70 DEG C
It is de-, secondary eluent is obtained；
S3：Secondary eluent in step S2 is carried out into activated carbon decolorizing, the pH value of destaining solution is adjusted, using ethyl acetate
Extract 4 times repeatedly, taking ethyl acetate layer liquid carries out crystallization and recrystallization in the case where temperature is for 6-10 DEG C, and the fan that 95-98% is obtained changes
Fragrant acid.
Preferably, the number of times of reflux, extract, described in step S1 be 3 times, when a length of 2.5-4h.
Preferably, an eluent described in step S1 is obtained the rosmarinic acid of 25-28% after concentrate drying.
It is highly preferred that the temperature of the drying be 80-95 DEG C, when a length of 3-5h.
Preferably, secondary eluent described in step S2 is obtained the rosmarinic acid of 50-66% after concentrate drying.
It is highly preferred that the temperature of the drying be 80-95 DEG C, when a length of 3-5h.
Preferably, the pH value of destaining solution described in step S3 is adjusted to 3.5-5.
The invention has the advantages that：
(1) the extraction process extraction process of purple common perilla rosemary acid of the invention is simple, extraction rate is fast, efficiency high, cost
It is low；
(2) extraction process that the present invention is provided determines NK109 resins pole and is appropriate to rosmarinic acid using static adsorptive method
Purification, improve the yield and purity of extract；
(3) process provided by the present invention can prepare various different demands contents in same production process route
Rosmarinic acid.
【Specific embodiment】
It is specifically described with reference to specific embodiment.
Embodiment 1
S1：It is coarse powder shape that Folium Perillae is crushed, and crosses 50 mesh sieves, ethanol of the addition equivalent to the 70% of 8 times of its weight, in water
Reflux, extract, 3 times under the conditions of bath, each extraction time is 2.5h, and extraction finishes rear united extraction liquid, and gained extracting solution passes through
After D101 macroporous resin adsorption, the ethanol of Jing 70% affords an eluent at 70 DEG C, and one time eluent passes through concentration,
3h is dried in the case where temperature is for 95 DEG C, 25.2% rosmarinic acid is obtained；
S2：By an eluent in step S1 after NK109 resin absorptioies, then the ethanol of Jing Jing 70% is at 70 DEG C
Secondary eluent is afforded, secondary eluent is dried 3h, 56% Herba Rosmarini Officinalis is obtained by concentration in the case where temperature is for 95 DEG C
Acid；
S3：Secondary eluent in step S2 is carried out into activated carbon decolorizing, destaining solution pH value is adjusted to 3.5, by destaining solution
Extracted repeatedly 4 times using ethyl acetate, take ethyl acetate layer liquid crystallize under 6 DEG C of ambient temperature, recrystallization, be obtained 95.4%
Rosmarinic acid.
Embodiment 2
S1：It is coarse powder shape that Folium Perillae is crushed, 50 mesh sieves excessively, ethanol of the addition equivalent to the 70% of 10 times of its weight,
Reflux, extract, 3 times under water bath condition, each extraction time is 3h, and extraction finishes rear united extraction liquid, and gained extracting solution passes through
After D101 macroporous resin adsorption, the ethanol of Jing 70% affords an eluent at 70 DEG C, and one time eluent passes through concentration,
4h is dried in the case where temperature is for 92 DEG C, 27.6% rosmarinic acid is obtained；
S2：By an eluent in step S1 after NK109 resin absorptioies, then the ethanol of Jing 70% is washed at 70 DEG C
De- to obtain secondary eluent, secondary eluent is dried 4h, 60.5% Herba Rosmarini Officinalis is obtained by concentration in the case where temperature is for 92 DEG C
Acid；
S3：Secondary eluent in step S2 is carried out into activated carbon decolorizing, destaining solution pH value is adjusted to 4, by destaining solution profit
Extracted repeatedly 4 times with ethyl acetate, take ethyl acetate layer liquid crystallize under 8 DEG C of ambient temperature, recrystallization, be obtained 96.3%
Rosmarinic acid.
Embodiment 3
S1：It is coarse powder shape that Folium Perillae is crushed, 50 mesh sieves excessively, ethanol of the addition equivalent to the 70% of 12 times of its weight,
Reflux, extract, 3 times under water bath condition, each extraction time is 4h, and extraction finishes rear united extraction liquid, and gained extracting solution passes through
After D101 macroporous resin adsorption, the ethanol of Jing 70% affords an eluent at 70 DEG C, and one time eluent passes through concentration,
4.5h is dried in the case where temperature is for 90 DEG C, 25% rosmarinic acid is obtained；
S2：By an eluent in step S1 after NK109 resin absorptioies, then the ethanol of Jing 70% is washed at 70 DEG C
De- to obtain secondary eluent, secondary eluent is dried 4.5h, 59% Herba Rosmarini Officinalis is obtained by concentration in the case where temperature is for 90 DEG C
Acid；
S3：Secondary eluent in step S2 is carried out into activated carbon decolorizing, destaining solution pH value is adjusted to 5, by destaining solution profit
Extracted repeatedly 4 times with ethyl acetate, take ethyl acetate layer liquid crystallize under 10 DEG C of ambient temperature, recrystallization, be obtained 97.5%
Rosmarinic acid.
Embodiment 4
S1：It is coarse powder shape that Folium Perillae is crushed, and crosses 50 mesh sieves, ethanol of the addition equivalent to the 70% of 9 times of its weight, in water
Reflux, extract, 3 times under the conditions of bath, each extraction time is 3.5h, and extraction finishes rear united extraction liquid, and gained extracting solution passes through
After D101 macroporous resin adsorption, the ethanol of Jing 70% affords an eluent at 70 DEG C, and one time eluent passes through concentration,
5h is dried in the case where temperature is for 88 DEG C, 27% rosmarinic acid is obtained；
S2：By an eluent in step S1 after NK109 resin absorptioies, then the ethanol of Jing 70% is washed at 70 DEG C
De- to obtain secondary eluent, secondary eluent passes through, and in the case where temperature is for 88 DEG C 5h is dried, and 63% rosmarinic acid is obtained；
S3：Secondary eluent in step S2 is carried out into activated carbon decolorizing, destaining solution pH value is adjusted to 4.5, by destaining solution
Extracted repeatedly 4 times using ethyl acetate, take ethyl acetate layer liquid crystallize under 7 DEG C of ambient temperature, recrystallization, be obtained 96.8%
Rosmarinic acid.
Embodiment 5
S1：It is coarse powder shape that Folium Perillae is crushed, 50 mesh sieves excessively, ethanol of the addition equivalent to the 70% of 11 times of its weight,
Reflux, extract, 3 times under water bath condition, each extraction time is 3h, and extraction finishes rear united extraction liquid, and gained extracting solution passes through
After D101 macroporous resin adsorption, the ethanol of Jing 70% affords an eluent at 70 DEG C, and one time eluent passes through concentration,
5h is dried in the case where temperature is for 80 DEG C, 26.4% rosmarinic acid is obtained；
S2：By an eluent in step S1 after NK109 resin absorptioies, then the ethanol of Jing 70% is washed at 70 DEG C
De- to obtain secondary eluent, secondary eluent is dried 5h, 62% rosmarinic acid is obtained by concentration in the case where temperature is for 80 DEG C；
S3：Secondary eluent in step S2 is carried out into activated carbon decolorizing, destaining solution pH value is adjusted to 3, by destaining solution profit
Extracted repeatedly 4 times with ethyl acetate, take ethyl acetate layer liquid crystallize under 9 DEG C of ambient temperature, recrystallization, be obtained 96.7%
Rosmarinic acid.
Above content is to combine specific preferred implementation further description made for the present invention, it is impossible to assert
The present invention be embodied as be confined to these explanation, for person of an ordinary skill in the technical field, without departing from
On the premise of present inventive concept, some simple deduction or replace can also be made, should all be considered as belonging to the present invention by being submitted to
Claims determine scope of patent protection.
Claims (7)
1. a kind of extraction process of purple common perilla rosemary acid, it is characterised in that comprise the following steps：
S1：It is coarse powder shape that Folium Perillae is crushed, and crosses 50 mesh sieves, the 70% of 8-12 times of its weight ethanol is added, in water bath condition
Lower reflux, extract, after D101 macroporous resin adsorption, the ethanol of Jing 70% eluting at 70 DEG C is obtained an eluting to extracting solution
Liquid；
S2：By an eluent in step S1 after NK109 resin absorptioies, the ethanol of Jing 70% eluting at 70 DEG C, system
Obtain secondary eluent；
S3：Secondary eluent in step S2 is carried out into activated carbon decolorizing, the pH value of destaining solution is adjusted, using ethyl acetate repeatedly
Extraction 4 times, taking ethyl acetate layer liquid carries out crystallization and recrystallization in the case where temperature is for 6-10 DEG C, and the rosmarinic acid of 95-98% is obtained.
2. the extraction process of purple common perilla rosemary acid according to claim 1, it is characterised in that：Backflow described in step S1 is carried
The number of times for taking be 3 times, when a length of 2.5-4h.
3. the extraction process of purple common perilla rosemary acid according to claim 1, it is characterised in that：Once wash described in step S1
De- liquid is obtained the rosmarinic acid of 25-28% after concentrate drying.
4. the extraction process of purple common perilla rosemary acid according to claim 3, it is characterised in that：The temperature of the drying is
80-95 DEG C, when a length of 3-5h.
5. the extraction process of purple common perilla rosemary acid according to claim 1, it is characterised in that：It is secondary described in step S2 to wash
De- liquid is obtained the rosmarinic acid of 50-66% after concentrate drying.
6. the extraction process of purple common perilla rosemary acid according to claim 5, it is characterised in that：The temperature of the drying is
80-95 DEG C, when a length of 3-5h.
7. the extraction process of purple common perilla rosemary acid according to claim 1, it is characterised in that：Destaining solution described in step S3
PH value be adjusted to 3.5-5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610886395.9A CN106565489A (en) | 2016-10-10 | 2016-10-10 | Process for extracting rosmarinic acid from perilla |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610886395.9A CN106565489A (en) | 2016-10-10 | 2016-10-10 | Process for extracting rosmarinic acid from perilla |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107382729A (en) * | 2017-08-11 | 2017-11-24 | 四川省中医药科学院 | A kind of medicine for the method and preparation that Rosmarinic acid is extracted from labiate |
| CN107628954A (en) * | 2017-10-12 | 2018-01-26 | 南京财经大学 | A kind of method that polyphenol substance is isolated and purified in the jasmine tea from lavender |
| CN107935855A (en) * | 2018-01-04 | 2018-04-20 | 湖北瑞晟生物有限责任公司 | A kind of technique that Rosmarinic acid is extracted from rosemary |
Citations (4)
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|---|---|---|---|---|
| JP2003180286A (en) * | 2001-12-21 | 2003-07-02 | Meiji Seika Kaisha Ltd | Method for producing phenol-containing extract from salt-pickled red perilla |
| CN1796362A (en) * | 2004-12-23 | 2006-07-05 | 青岛大学 | Technique for producing purple common perilla rosemary acid |
| CN101863767A (en) * | 2010-03-23 | 2010-10-20 | 南京泽朗农业发展有限公司 | Preparation process of rosmarinic acid |
| CN102850219A (en) * | 2012-09-28 | 2013-01-02 | 中北大学 | Method for extracting rosmarinic acid from folia perillae acutae |
-
2016
- 2016-10-10 CN CN201610886395.9A patent/CN106565489A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003180286A (en) * | 2001-12-21 | 2003-07-02 | Meiji Seika Kaisha Ltd | Method for producing phenol-containing extract from salt-pickled red perilla |
| CN1796362A (en) * | 2004-12-23 | 2006-07-05 | 青岛大学 | Technique for producing purple common perilla rosemary acid |
| CN101863767A (en) * | 2010-03-23 | 2010-10-20 | 南京泽朗农业发展有限公司 | Preparation process of rosmarinic acid |
| CN102850219A (en) * | 2012-09-28 | 2013-01-02 | 中北大学 | Method for extracting rosmarinic acid from folia perillae acutae |
Non-Patent Citations (1)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107382729A (en) * | 2017-08-11 | 2017-11-24 | 四川省中医药科学院 | A kind of medicine for the method and preparation that Rosmarinic acid is extracted from labiate |
| CN107628954A (en) * | 2017-10-12 | 2018-01-26 | 南京财经大学 | A kind of method that polyphenol substance is isolated and purified in the jasmine tea from lavender |
| CN107935855A (en) * | 2018-01-04 | 2018-04-20 | 湖北瑞晟生物有限责任公司 | A kind of technique that Rosmarinic acid is extracted from rosemary |
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