CN106565478A - Method for separating and purifying rosmarinic acid from purple perilla - Google Patents
Method for separating and purifying rosmarinic acid from purple perilla Download PDFInfo
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- CN106565478A CN106565478A CN201610922398.3A CN201610922398A CN106565478A CN 106565478 A CN106565478 A CN 106565478A CN 201610922398 A CN201610922398 A CN 201610922398A CN 106565478 A CN106565478 A CN 106565478A
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- rosmarinic acid
- solution
- ethyl acetate
- folium perillae
- extraction
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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
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention belongs to the field of natural organic chemistry, and relates to a method for extracting and separating rosmarinic acid from purple perilla. The method comprises the following steps of performing extraction by taking enzyme as an adjuvant in an acidic condition, then, performing extraction by utilizing ethyl acetate in the acidic condition, and performing primary purification by utilizing macro-porous adsorption resin, so that a high-purity rosmarinic acid product is obtained. The method disclosed by the invention has the advantages that: water is used as an extraction solvent in the acidic condition; compared with the traditional process that extraction is carried out by utilization of ethanol, the production cost is greatly reduced; the enzyme is added and used as the adjuvant in the extraction process; therefore, the loss of rosmarinic acid can be effectively reduced; extraction is carried out by adoption of ethyl acetate, so that the purity of the rosmarinic acid product is increased easily; and elution is carried out by utilization of ethyl acetate, so that the purity of the rosmarinic acid product is obviously increased. The rosmarinic acid prepared by the invention can be widely applied in the fields, such as health foods and cosmetics.
Description
Technical field
The invention belongs to field of natural organic chemistry, is related to a kind of method of the separating and purifying rosmarinic acid from Folium Perillae.
Background technology
Rosmarinic acid is a kind of multi-functional phenolic compound, is also the secondary metabolic derivative in plant body, with certain
Physiologically active.There are multiple phenolic hydroxyl groups in rosmarinic acid structure, and its number has with the antioxidant activity of rosmarinic acid
Important association.Rosmarinic acid is water-soluble substanceses buff powder, meets the aobvious aeruginouss of ferric chloride ferrum cyaniding solution.By spectroscopy
The development of technology, provides very convenient condition, with rosmarinic acid for identification and structural analyses of the mankind to natural product
Structure is progressively determined, and research of the people to rosmarinic acid becomes increasingly active, it is found that rosmarinic acid is widely distributed, and rosmarinic acid
As many medical materials and the main component of Chinese patent medicine, with very strong and be many biological activitys, can extensively apply
In in terms of the antioxidation of beverage, cosmetics and food etc..
Rosmarinic acid is widely distributed in plant, and from high dicotyledon to low tongue, diction class, Tibetan class plant have and contain
There is the report of rosmarinic acid, but be distributed mainly on Labiatae, in Boraginaceae and Umbelliferae.Rosmarinic acid containing in different plants
Amount is different, even if in same plant, the content of the rosmarinic acid of its different parts is also differed, and Folium Perillae is fan
Repeatedly higher plant parts of fragrant acid content.At present conventional extracting method has：It is organic solvent extraction, supercritical extraction, micro-
Ripple method and ultrasonic extraction.Organic solvent extraction is that conventional ethanol and methanol etc. are extracted, while yield is improved, by
It is poisonous in methanol, therefore conventional ethanol is more excellent solvent.Enzymatic Extraction is a kind of effective ways of extraction rosmarinic acid, with anti-
Short, extraction ratio is high, impurity in products is few between seasonable, it is environmentally friendly the features such as.Traditional extracting method typically will heating and organic solvent
Combine, extracted to reach the purpose for improving yield, but organic solvent not only has toxic action, does not meet greenization
Theme, but also the structure of matter can be changed by chemical reaction, and it is inadvisable.Enzymatic Extraction rosmarinic acid is then
On the basis of conventional hot water's restricted-access media, by adding specific enzyme in extracting solution, the purpose for improving extraction efficiency is reached,
It is low with reaction temperature in experimentation, without any organic reagent, the advantage on the less impact of extract, therefore, enzyme process
Have broad application prospects in the extraction of rosmarinic acid.
The content of the invention
It is an object of the invention to provide a kind of method of the separating and purifying rosmarinic acid from Folium Perillae.The present invention is first using acid
Property aqueous solution addition enzyme under conditions of extracted, recycle ethyl acetate extracted, then using polar macroporous absorption
Resin carries out isolating and purifying the highly purified rosmarinic acid product of acquisition.
The technical scheme is that what is be achieved in that, it is comprised the following steps：
(1) extract：The use of pH value is acidic aqueous solution between 3.5～4.5 in addition enzyme after Folium Perillae is pulverized and sieved
Under the conditions of extracted, obtain the extracting solution containing rosmarinic acid；
(2) it is acidified：A certain amount of hydrochloric acid is added in extracting solution, the pH value for adjusting extracting solution is maintained between 4～4.5；
(3) extract：A certain amount of ethyl acetate is added in the acidifying solution of step (2), it is quiet after extracting under certain condition
Put, then by standing a point liquid, merging obtains extract；
(4) resin purification：Solution is first adsorbed with the macroporous adsorbent resin of polarity, then with ethyl acetate to macropore
Adsorbent resin is parsed, and obtains the ethyl acetate solution containing rosmarinic acid；
(5) concentrate：Ethyl acetate solution is carried out into concentrating under reduced pressure, concentrated solution is obtained；
(6) it is dried：Concentrated solution obtains Sorbus domestica anthocyanidin product using being spray-dried.
In the step (1), enzyme usage amount is the 0.5～2.5% of Folium Perillae raw materials quality, and Extracting temperature is 80～90 DEG C,
Raw material: extracting solution=1: 25～30 (m/v), extraction time is 45～60min.
In the step (2), described hydrochloric acid mass fraction is 18%, and addition is about the 3% of liquor capacity, solution temperature
Degree is maintained at 40 DEG C, then stands and is cooled to extraction after room temperature.
In the step (4), after adding ethyl acetate, the ethyl acetate volume fraction of solution be maintained at 70～80% it
Between.
Specific embodiment
Embodiment 1
Folium Perillae after 0.5kg is pulverized and sieved is put in round-bottomed flask with the Extraction solvent sour water (pH=3.5) of 7.5kg,
And 200g enzymes are put into in round-bottomed flask, Extracting temperature is 80 DEG C, and extraction time is 45min, is extracted 2 times, collects extracting solution；Will
The extracting solution collected is adjusted using acidic aqueous solution (18% hydrochloric acid), is allowed to pH value between 4～4.5, then to it
Middle ethyl acetate is extracted, and addition is 2 times of extracting liquid volume, and liquid is divided after standing, and extract is merged；By extract
Purification is carried out with NK109 types macroporous adsorbent resin, ethyl acetate desorbed solution is collected；Desorbed solution vacuum-concentrcted, vacuum for-
0.08～-0.07Mpa, at 30 ± 2 DEG C, recycling design obtains concentrate to thickening temperature；Again concentrate is utilized into blast drier
It is dried, temperature is 60 DEG C, obtains the Folium Perillae rosmarinic acid product 0.13kg that rosmarinic acid contents are 58.9%.
Embodiment 2
Folium Perillae after 0.5kg is pulverized and sieved is put in round-bottomed flask with the Extraction solvent sour water (pH=4.5) of 6.25kg,
And 250g enzymes are put into in round-bottomed flask, Extracting temperature is 90 DEG C, and extraction time is 60min, is extracted 2 times, collects extracting solution；Will
The extracting solution collected is adjusted using acidic aqueous solution (18% hydrochloric acid), is allowed to pH value between 4～4.5, then to it
Middle ethyl acetate is extracted, and addition is 2 times of extracting liquid volume, and liquid is divided after standing, and extract is merged；By extract
Purification is carried out with NK109 types macroporous adsorbent resin, ethyl acetate desorbed solution is collected；Desorbed solution vacuum-concentrcted, vacuum for-
0.08～-0.07Mpa, at 30 ± 2 DEG C, recycling design obtains concentrate to thickening temperature；Again concentrate is utilized into blast drier
It is dried, temperature is 60 DEG C, obtains the Folium Perillae rosmarinic acid product 0.16kg that rosmarinic acid contents are 54.6%.
Claims (4)
1. a kind of method of the separating and purifying rosmarinic acid from Folium Perillae, it comprises the following steps：
(1) extract：The use of pH value is the condition of acidic aqueous solution between 3.5～4.5 in addition enzyme after Folium Perillae is pulverized and sieved
Under extracted, obtain the extracting solution containing rosmarinic acid；
(2) it is acidified：A certain amount of hydrochloric acid is added in extracting solution, the pH value for adjusting extracting solution is maintained between 4～4.5；
(3) extract：A certain amount of ethyl acetate is added in the acidifying solution of step (2), is stood after extracting under certain condition, so
Afterwards by standing a point liquid, merging obtains extract；
(4) resin purification：Solution is first adsorbed with the macroporous adsorbent resin of polarity, then with ethyl acetate to macroporous absorption
Resin is parsed, and obtains the ethyl acetate solution containing rosmarinic acid；
(5) concentrate：Ethyl acetate solution is carried out into concentrating under reduced pressure, concentrated solution is obtained；
(6) it is dried：Concentrated solution adopts forced air drying, obtains Folium Perillae rosmarinic acid product.
2. the method for a kind of separating and purifying rosmarinic acid from Folium Perillae according to claim 1, it is characterised in that：The step
Suddenly in (1), enzyme usage amount is the 0.5～2.5% of Folium Perillae raw materials quality, and Extracting temperature is 80～90 DEG C, raw material: extracting solution=1:
25～30 (m/v), extraction time is 45～60min.
3. the method for a kind of separating and purifying rosmarinic acid from Folium Perillae according to claim 1, it is characterised in that：The step
Suddenly in (2), described hydrochloric acid mass fraction is 18%, and addition is about the 3% of liquor capacity, and solution temperature is maintained at 40 DEG C,
Then stand to be cooled to after room temperature and extract.
4. the method for a kind of separating and purifying rosmarinic acid from Folium Perillae according to claim 1, it is characterised in that：The step
Suddenly in (4), after adding ethyl acetate, the ethyl acetate volume fraction of solution is maintained between 70～80%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610922398.3A CN106565478A (en) | 2016-10-17 | 2016-10-17 | Method for separating and purifying rosmarinic acid from purple perilla |
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| CN201610922398.3A CN106565478A (en) | 2016-10-17 | 2016-10-17 | Method for separating and purifying rosmarinic acid from purple perilla |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115232673A (en) * | 2022-07-06 | 2022-10-25 | 玉溪农业职业技术学院(云南省玉溪烟草栽培学校) | Aromatic perilla extract composition with antibacterial function and preparation method thereof |
-
2016
- 2016-10-17 CN CN201610922398.3A patent/CN106565478A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115232673A (en) * | 2022-07-06 | 2022-10-25 | 玉溪农业职业技术学院(云南省玉溪烟草栽培学校) | Aromatic perilla extract composition with antibacterial function and preparation method thereof |
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Application publication date: 20170419 |