CN105062687A - Method for extracting eucalyptus oil and hydrolyzing tannin to prepare ellagic acid at the same time - Google Patents
Method for extracting eucalyptus oil and hydrolyzing tannin to prepare ellagic acid at the same time Download PDFInfo
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- CN105062687A CN105062687A CN201510451301.0A CN201510451301A CN105062687A CN 105062687 A CN105062687 A CN 105062687A CN 201510451301 A CN201510451301 A CN 201510451301A CN 105062687 A CN105062687 A CN 105062687A
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Abstract
The invention discloses a method for extracting eucalyptus oil and hydrolyzing tannin to prepare ellagic acid at the same time. The method is characterized by comprising the following steps: drying blue gum leaves in the shade, then grinding the blue gum leaves, adding a 3-methyl-1-(4-butylsulfonyl)imidazolium sulfate ionic liquid water solution into the grinded leaves, extracting the leaves by a water steam distillation technology under the assistance of microwaves, condensing to obtain blue gum essential oil, separating an extracting solution from the residues, subjecting the extracting solution to macroporous resin adsorption, then washing the macroporous resin by an ethanol solution to carry out desorption, condensing the desorbed solution, and freeze-drying the condensate in vacuum so as to obtain the ellagic acid extract. In the provided technology, a Bronsted strongly acidic 3-methyl-1-(4-butylsulfonyl)imidazolium sulfate ionic fluid water solution is taken as the extracting agent, and the acidic ionic liquid solution is used as a solvent and a catalyst at the same time. The microwave-assisted water steam distillation extraction can obtain a plurality of target compounds at the same time, the resource is comprehensively utilized, and compared with the common extraction methods, the provided extraction method has the advantages of short time and high efficiency.
Description
Technical field
The present invention relates to field of natural product chemistry, particularly relate to and a kind ofly extract essential oil from blue gum blade and the method for ellagic acid is prepared in hydrolysis simultaneously.
Background technology
The kind that blue gum (formal name used at school: Eucalyptusglobulus) is Myrtaceae eucalyptus subordinate is Australia's cultivation one of seeds the most widely.Eucalyptus is Myrtaceae (Myrtacea) plant, and NATURAL DISTRIBUTION is in countries such as Australia, and be a kind of important economic tree, leaf and fruit can be used as medicine, so far existing more than 120 countries and regions introducing culture.The whole world existing eucalyptus plantation area more than 600 hectare, produces timber ten thousand stere more than 6000 per year.Various countries facts have proved that eucalyptus is one of famous seeds that the speed of growth is the fastest in the world.China's Transplanting Eucalyptus has the history of 106 years, is developed so far, and eucalyptus has been planted in 600 Duo Ge counties of existing 20 provinces, autonomous regions and municipalities at present, and artificial area reaches 800,000 hectares.Wherein, blue gum is that China introduces a fine variety one of the most successful eucalypt species.
Eucalyptus globulus Labill leaf oil has high Development volue, and tool acrid odors, is rich in eucalyptol, is the key variety of China's export spices always.Main component 1, 8-Cineole in eucalyptus oil is the activeconstituents of most worthy in multiple cough drops, is the medicine that treatment flu, cough, rhinitis etc. are commonly used; Eucalyptus oil is conducive to when being inhaled into thoracic cavity cleaning congested respiratory tract, and the control of this feature on diseases such as respiratory tract infection, cough, sinusitis paranasal sinusitis, laryngalgia and pulmonary tuberculosis, typhoid fever and malaria has important impact; Eucalyptus oil is added in massage oil and ointment, lip can be treated and hand is chapped from the cold and other tetter; Eucalyptus oil has stronger bacteriostatic action, and being aided with other raw material can in order to develop the products such as efficient emulsifying agent, sterilant, freshener, washing composition.Therefore, be widely used in food, medicine and daily-use chemical industry industry.
Ellagic acid belongs to polyphenol dilactone, it is the dimerization derivative of gallic acid, extensively be present in the plant tissues such as various nut, mushy fruit mainly with condensed forms (as Ellagitannins, glycosides etc.), there is anti-oxidant, anticancer, antibacterial, antiviral, the multiple pharmacologically active such as antiproliferative, enhancing immunocompetence.Because in natural plant raw material, ellagic acid content is not high, technical process relative complex, the production cost of separating and purifying high-purity ellagic acid extract are too high, making main in current industrial production is raw material with gallic acid, adopts the method transforming or synthesize, manufacture ellagic acid extract.
Publication number be CNIO3333175 patent describes the method that the blue declining pomace of a kind of mushroom mycelium solid state fermentation prepares ellagic acid and gallic acid, concrete steps are: 1, solid fermentation: a, preparation be long has mushroom aerial hyphae height to be the substratum disk of 1.0-2.Omm; B, preparation solution A and solid B; C, the cultured products of preparation containing ellagic acid and gallic acid.2, the extraction preparation of ellagic acid and gallic acid: namely complete the method that mushroom mycelium solid state fermentation blueberry pomace prepares ellagic acid and gallic acid, this legal system for gallic acid and ellagic acid technique loaded down with trivial details, there is production process and require high, the shortcoming such as production cost is high.
Publication number is that CN102807570A describes the fragrant method really preparing ellagic acid of a kind ofization, and adopt water extraction, evaporation concentration, acidification hydrolization and crystallization, polishing purification prepares ellagic acid, uses mineral acid (hydrochloric acid or sulfuric acid) catalytic hydrolysis to prepare ellagic acid; Publication number is the preparation method that CN103524521A describes a kind of blackberry ellagic acid, take blackberry pomace as raw material, alkaline solution through certain second (first) determining alcohol extracts, recycling design, acidifying, precipitation, centrifugal, polyamide resin on supernatant liquor, uses water, buck wash-out respectively, acidifying after buck elutriant is concentrated, precipitation, precipitate molten with alkali, that acid is heavy method repurity, obtain blackberry ellagic acid purified product after drying; Publication number is the method extracting ellagic acid in CN104341431A pomegranate skin, and step is: Feedstock treating, the process of high pressure microjet micronizing, high pressure extract, hydrolysis, purifying, collection crystallization, drying, obtain ellagic acid.Above three kinds of methods use mineral acid catalytic hydrolysis to prepare ellagic acid, the problem such as also exist that environmental pollution is serious, equipment loss is comparatively large and energy consumption is higher.
acidic ion liquid refers in the structure be made up of sulfonic group and carboxylic acid group the ionic liquid having the acidic functionality being with active oxygen.This acidic ion liquid except having except widespread use in organic acid catalysis reaction; Also can in order to synthesize gold, platinum nano material, as lithium battery electroless plating in electrochemistry and in separating and extracting etc.The appearance of existing acidic ion liquid also overcomes the reaction times that traditional catalyst brings longer, etching apparatus, spent acid solution contaminate environment, product and is separated with catalyzer difficulty and the shortcoming such as catalyzer is not easy to be recycled and product color is dark, also has apply more widely in catalysis and organic synthesis field.At present, the research that acidic ion liquid is applied to the Extraction and separation aspect of natural active matter rarely has report.
The present invention, has selected for raw material with blue gum blade
strongly-acid 3-methyl isophthalic acid-(4-butyl sulphonyl) imidazole sulfates ionic liquid aqueous solution is extraction agent, make use of the dual-use function that acidic ionic liquid liquid solution has solvent and catalyzer.Microwave-assisted wet distillation method is extracted simultaneously and is obtained multiple target compounds, reaches the object of the comprehensive utilization of resource, compared with conventional extraction processes, have efficient, the advantage such as save time.
Summary of the invention
The object of the present invention is to provide and a kind ofly extract essential oil from blue gum blade and the method for ellagic acid is prepared in hydrolysis simultaneously.
In order to achieve the above object, the technical solution used in the present invention comprises: pulverize after being dried in the shade by blue gum blade, add 3-methyl isophthalic acid-(4-butyl sulphonyl) imidazole sulfates ionic liquid aqueous solution, microwave-assisted wet distillation extracts, and obtains Eucalyptus globulus Labill leaf oil through condensation; Extracting solution is separated with residue, macroporous resin adsorption, and ethanolic soln is resolved, and desorbed solution concentrates final vacuum lyophilize and namely obtains ellagic acid extract.
Advantage of the present invention is:
1. the present invention use the method for microwave-assisted 3-methyl isophthalic acid-(4-butyl sulphonyl) imidazole sulfates ionic liquid aqueous solution extract eucalyptus oil and simultaneously Hydrolysable Tannins prepare ellagic acid, make use of acidic ionic liquid liquid solution and there is the characteristics such as the dual-use function of solvent and catalyzer, compared with conventional extraction processes, have efficient, the advantage such as save time.
2, extracting solution macroporous resin adsorption acidic ethanol is resolved, and ethanol and ionic liquid reclaim and can reuse, and have saved production cost, have reached the object of the comprehensive utilization of resource.
Accompanying drawing illustrates (nothing)
Embodiment
Below the invention process is described in further detail:
Pulverize after being dried in the shade by blue gum blade, add 3-methyl isophthalic acid-(4-butyl sulphonyl) imidazole sulfates ionic liquid aqueous solution, microwave-assisted wet distillation extracts, and obtains Eucalyptus globulus Labill leaf oil through condensation; Extracting solution is separated with residue, macroporous resin adsorption, and ethanolic soln is resolved, and desorbed solution concentrates final vacuum lyophilize and namely obtains ellagic acid extract.Below, the present invention will be further detailed by embodiment, but it is not limited to any one or similar example of these embodiments.
Embodiment 1:
Blue gum blade after 100g is pulverized, add 1.5L1mol/L3-methyl isophthalic acid-(4-butyl sulphonyl) imidazole sulfates ionic liquid aqueous solution, under microwave 500W, vapor distill extraction extracts 0.75h, the essential oil of condensation after extracting, filter and remove filter residue, the extracting solution of ellagic acid must be contained, with the absorption of ADS17 macroporous resin adsorption post after extracting solution concentrating under reduced pressure, adsorption column blade diameter length ratio is 1:8, loading flow velocity 10BV/h; With 6BV water with 4BV/h removal of impurities, with pH value to be 2 volume fractions be 60% ethanol resolve, desorbed solution concentrates final vacuum drying and obtains 0.32g ellagic acid, obtains 0.46g eucalyptus oil simultaneously.
Embodiment 2:
Blue gum blade after 20kg is pulverized, add 1.0L1mol/L3-methyl isophthalic acid-(4-butyl sulphonyl) imidazole sulfates ionic liquid aqueous solution, under microwave 400W, vapor distill extraction extracts 1h, the essential oil of condensation after extracting, filter and remove filter residue, the extracting solution of ellagic acid must be contained, with the absorption of ADS17 macroporous resin adsorption post after concentrating under reduced pressure extracting solution concentrating under reduced pressure, adsorption column blade diameter length ratio is 1:10, loading flow velocity 6BV/h; With 4BV water with 6BV/h removal of impurities, with pH value to be 3 volume fractions be 50% ethanol resolve, desorbed solution concentrates final vacuum drying and obtains 75.02g ellagic acid, obtains 98.27g eucalyptus oil simultaneously.
Claims (7)
1. one kind is extracted essential oil from blue gum blade and the method for ellagic acid is prepared in hydrolysis simultaneously, it is characterized in that: pulverize after blue gum blade is dried in the shade, add 3-methyl isophthalic acid-(4-butyl sulphonyl) imidazole sulfates ionic liquid aqueous solution, microwave-assisted wet distillation extracts, and obtains Eucalyptus globulus Labill leaf oil through condensation; Extracting solution is separated with residue, macroporous resin adsorption, and ethanolic soln is resolved, and desorbed solution concentrates final vacuum lyophilize and namely obtains ellagic acid extract.
2. a kind ofly extract essential oil from blue gum blade and the method for ellagic acid is prepared in hydrolysis according to according to claim 1 simultaneously, it is characterized in that: the blue gum blade after pulverizing uses microwave-assisted wet distillation to assist 3-methyl isophthalic acid-(4-butyl sulphonyl) imidazole sulfates ionic liquid aqueous solution to extract, and the concentration of 3-methyl isophthalic acid-(4-butyl sulphonyl) imidazole sulfates ionic liquid aqueous solution is 0.5-1.5mol/L.
3. a kind ofly extract essential oil from blue gum blade and the method for ellagic acid is prepared in hydrolysis according to according to claim 1 simultaneously, it is characterized in that: the solid-liquid ratio of 3-methyl isophthalic acid-(4-butyl sulphonyl) imidazole sulfates ionic liquid aqueous solution and blade powder is 1:6-1:30g/mL, microwave power is 120-700W, and the microwave time is 0.25-1h.
4. a kind ofly extract essential oil from blue gum blade and the method for ellagic acid is prepared in hydrolysis according to according to claim 1 simultaneously, it is characterized in that: macroporous resin adsorption is ADS17.
5. a kind ofly extract essential oil from blue gum blade and the method for ellagic acid is prepared in hydrolysis according to according to claim 1, it is characterized in that: adsorption column blade diameter length ratio 1:5-1:12, loading flow velocity is 4-10BV/h simultaneously.
6. a kind ofly extract essential oil from blue gum blade and the method for ellagic acid is prepared in hydrolysis according to according to claim 1, it is characterized in that: wash removing impurity with water, washing water consumption is 3-8BV, and washing speed is 2-6BV/h simultaneously.
7. a kind ofly extract essential oil from blue gum blade and the method for ellagic acid is prepared in hydrolysis according to according to claim 1 simultaneously, it is characterized in that: the volume fraction of desorbed solution to be pH be 1-5 is the ethanol of 20%-80%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108300561A (en) * | 2018-01-17 | 2018-07-20 | 南京工业大学 | Method for extracting peony seed oil by aqueous enzymatic method |
| CN111689981A (en) * | 2020-05-21 | 2020-09-22 | 成都市明典世家生物科技有限公司 | Method for extracting 1, 8-cineole from tea tree oil |
| CN113041279A (en) * | 2021-05-28 | 2021-06-29 | 湖南绿蔓生物科技股份有限公司 | Method for separating effective components from momordica grosvenori flowers |
| CN117815149A (en) * | 2024-03-04 | 2024-04-05 | 广州汇芬生物科技有限公司 | Composition with mite removing effect and application thereof in preparation of mite removing emulsion |
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2015
- 2015-07-29 CN CN201510451301.0A patent/CN105062687A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108300561A (en) * | 2018-01-17 | 2018-07-20 | 南京工业大学 | Method for extracting peony seed oil by aqueous enzymatic method |
| CN111689981A (en) * | 2020-05-21 | 2020-09-22 | 成都市明典世家生物科技有限公司 | Method for extracting 1, 8-cineole from tea tree oil |
| CN111689981B (en) * | 2020-05-21 | 2022-11-22 | 成都市明典世家生物科技有限公司 | Method for extracting 1, 8-cineole from tea tree oil |
| CN113041279A (en) * | 2021-05-28 | 2021-06-29 | 湖南绿蔓生物科技股份有限公司 | Method for separating effective components from momordica grosvenori flowers |
| CN117815149A (en) * | 2024-03-04 | 2024-04-05 | 广州汇芬生物科技有限公司 | Composition with mite removing effect and application thereof in preparation of mite removing emulsion |
| CN117815149B (en) * | 2024-03-04 | 2024-06-04 | 广州汇芬生物科技有限公司 | Composition with mite removing effect and application thereof in preparation of mite removing emulsion |
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