CN104087420A - Subcritical extraction method capable of improving antioxidant activity of volatile oil in agarwood leaves - Google Patents
Subcritical extraction method capable of improving antioxidant activity of volatile oil in agarwood leaves Download PDFInfo
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- CN104087420A CN104087420A CN201410338081.6A CN201410338081A CN104087420A CN 104087420 A CN104087420 A CN 104087420A CN 201410338081 A CN201410338081 A CN 201410338081A CN 104087420 A CN104087420 A CN 104087420A
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Abstract
The invention provides a subcritical extraction method capable of improving the antioxidant activity of volatile oil in agarwood leaves. The method comprises the following steps of cleaning agarwood leaves, drying and removing branches, and then baking to be almost absolute dry, and then baking to constant weight, pulverizing to obtain agarwood leaf powder, and then placing in the extraction vessel, adding deionized water, carrying out subcritical extraction, standing, cooling, carrying out suction filtration, and then extracting the residue once again, mixing the two extractive solutions, then concentrating under reduced pressure to obtain a concentrated solution, adding NaCl for demulsifying, extracting with ether, collecting the ether layer and then dehydrating collected ether layer with Na2SO4 and concentrating under reduced pressure to obtain agarwood leaf volatile oil. The obtained agarwood leaf volatile oil has antioxidant and immune function enhancing functions, anti-tumor activities and the like; compared with the traditional method, the method disclosed by the invention has more outstanding antioxidant effect. The method has the advantages of short extraction time, small solvent amount, high yield and low cost, takes non-toxic and harmless water as an extraction solvent and the processing of raw materials is simple.
Description
Technical field
The present invention relates to a kind of subcritical extraction method that improves volatile oil anti-oxidant activity in eaglewood leaf, belong to natural goods extractive technique field.
Background technology
Agalloch eaglewood as traditional Chinese medical science common medicine, in each version of < < Pharmacopoeia of People's Republic of China > >, all have the record to its source, function etc., it is mainly derived from the timber that Isolated From Thymelaeaceae Species Lignum Aquilariae Resinatum [Aquilaria sinensis (Lour.) Gilg] contains resin.Agalloch eaglewood fragrant odour, taste is pained, slightly warm in nature has the function effect of promoting the circulation of QI to relieve pain, warming middle-JIAO to arrest vomiting, helping inspiration to relieve asthma, always in the vexed pain of medical its treatment chest abdomen, gastrofrigid vomiting hiccup, the circulation of vital energy in the wrong direction of suffering from a deficiency of the kidney breathe heavily the diseases such as anxious.Extraction volatile oil eaglewood leaf used is the leaf of Isolated From Thymelaeaceae Species Lignum Aquilariae Resinatum, and modern study analysis is verified, contains the compositions such as volatile oil, flavones and glycoside thereof, phenols, triterpenes, polysaccharide, amino acid in eaglewood leaf; Eaglewood leaf, as the dis-medicinal part of agalloch eaglewood, generally speaking, can be plucked 2 times, so output is larger every year in enormous quantities.As the volatile oil extracting in eaglewood leaf, not only there is relieving inflammation and relaxing pain, the anti-oxidant and effect such as delay senility, meanwhile, also can be used as spices, be used for making highclass perfumes, perfumed soap, essence and makeup and add flavouring etc. in tobacco to, there is higher application and economic worth.
Volatile oil is that in plant, a class has aromatic odour, volatilizable at normal temperatures, and can be with the general name of steam distillation and the not miscible oily liquids of water.The plant with volatile oil is widely distributed, China Jiu You 56 sections only, and 136 belong to, and in approximately 300 kind of plant, contain volatile oil.Eaglewood leaf volatile oil is the important activeconstituents of a class, has multiple pharmacologically active and the application aspect medical science is more and more general.The extracting method of current domestic eaglewood leaf volatile oil mainly contains traditional steam distillation, organic solvent extractionprocess and emerging overcritical, subcritical abstraction technology etc.Traditional method ubiquity shortcoming separately, the destruction as low in the rate of recovery, impurity is many, high temperature causes thermo-sensitivity composition, dissolvent residual etc.
The Subcritical Water Extraction technology that the nearly more than ten years develop rapidly both at home and abroad, is a kind of newer not using or lack green abstraction technique with an organic solvent, is applied to the extraction of eaglewood leaf volatile oil, significant to the production modernization of eaglewood leaf volatile oil.
Summary of the invention
For overcoming the destruction that the rate of recovery is low, impurity is many, high temperature causes thermo-sensitivity composition, dissolvent residual that conventional steam distillation, organic solvent extractionprocess exist, active substance being brought to the problems such as disadvantageous effect, the invention provides a kind of subcritical extraction method that improves volatile oil anti-oxidant activity in eaglewood leaf.
The solvent that the present invention utilizes subcritical energy heating to contact with sample, required compound is separated from sample matrices, enter in solvent.Concrete through following each step:
(1) eaglewood leaf is cleaned, is dried and removes branch, then being placed in 45 ± 1 ℃, to be dried to water ratio be 5～10%, then dry to constant weight in 105 ± 1 ℃, pulverize and obtain eaglewood leaf powder;
(2) the eaglewood leaf powder of getting step (1) is placed in extraction kettle, according to solid-liquid ratio, be that 1:40～1:80 adds deionized water, extracting power, be under 2.0～4.0MPa, to carry out subcritical abstraction 10～18min, standingly carry out suction filtration after cooling, then residue is repeated to extract once, merge extracted twice liquid, then obtain concentrated solution through concentrating under reduced pressure;
(3) after step (2) gained concentrated solution is cooling, add NaCl to carry out breakdown of emulsion, then to collect ether layer after extracted with diethyl ether, then by the ether layer Na collecting
2sO
4dewater, after concentrating under reduced pressure, obtain eaglewood leaf volatile oil.
The eaglewood leaf powder size of described step (1) is 60～100 orders.
In described step (2), eaglewood leaf powder is placed in extraction kettle, then after compressing, in the top of extraction kettle, puts into glass cotton balls, prevents the eaglewood leaf powder blocking pipe blowing out.
The present invention improves the subcritical assisted Extraction that eaglewood leaf volatile oil anti-oxidant activity is object to follow the example of, and can overcome the disadvantageous effect that conventional steam distillation, organic solvent extraction bring active substance; The solvent that utilizes subcritical energy heating to contact with sample, required compound is separated from sample matrices, enter in solvent.
The present invention has following advantage and beneficial effect: the eaglewood leaf volatile oil that the present invention prepares has anti-oxidant, enhancing body immunologic function and antitumor isoreactivity, and apply in food, makeup, tobacco and field of medicaments, gained antioxidant effect improves 1.53～2.22 times than traditional ether soxhlet extraction, than wet distillation extraction method, improve 2.14～3.09 times, there is the antioxidant effect significantly improving.As shown in Figure 1, in DPPH free radical system, the IC50 of eaglewood leaf volatile oil is 40.07～58.03 μ g/mL, and than traditional method, the DPPH free radical scavenging activity of gained eaglewood leaf volatile oil of the present invention is low, and functionally active is high.This extracting method is high to the rate of recovery of target component, extraction time is short, and usings nontoxic, harmless water as extracting solvent, and quantity of solvent is few, and yield is high, cost is low; And raw material processing is simple, has simplified sample pretreatment step.Present method have non-environmental-pollution, technique simple, efficient, save time, cost is low and be easy to the advantages such as large-scale industrial production, is environmental protection, volatile oil extractive technique in the leaf that has a extensive future.With utilize organic solvent to extract to compare, technical process science of the present invention, reasonable, do not need to use organic chemistry solvent to extract, noresidue, pollution-free, and can make full use of and extract plurality of active ingredients and keep its original activity, and the extraction yield of various effective constituents is high, good stability, make the features such as the product diversification of eaglewood leaf volatile oil, seriation.
Accompanying drawing explanation
Fig. 1 is for measuring yield, the DPPH free radical scavenging activity of volatile oil in gained eaglewood leaf.
Embodiment
Below provide embodiment, the invention will be further described.
Embodiment 1
(1) eaglewood leaf is cleaned, is dried and removes branch, then be placed in vacuum drying oven take 45 ℃ be dried to water ratio as 8%, then vacuum drying oven temperature is adjusted to 105 ℃ and dries to constant weight, pulverize and to obtain 80 object eaglewood leaf powder;
(2) the eaglewood leaf powder of getting step (1) is placed in extraction kettle, after compressing again, in the top of extraction kettle, put into glass cotton balls, preventing the eaglewood leaf powder blocking pipe blowing out, for 1:60 adds deionized water, is 3.0MPa under to carry out subcritical abstraction 14min extracting power according to solid-liquid ratio (unit is g/mL), standingly carry out suction filtration after cooling, then residue is repeated to extract once, merge extracted twice liquid, then obtain concentrated solution through concentrating under reduced pressure;
(3), after step (2) gained concentrated solution is cooling, add the standing breakdown of emulsion that carries out of NaCl, then to collect ether layer after extracted with diethyl ether, then by the ether layer Na collecting
2sO
4dewater, after concentrating under reduced pressure, obtain eaglewood leaf volatile oil.
The yield of gained eaglewood leaf volatile oil is that 13.25%, DPPH free radical scavenging activity is shown in Fig. 1.
Embodiment 2
(1) eaglewood leaf is cleaned, is dried and removes branch, then be placed in vacuum drying oven take 44 ℃ be dried to water ratio as 5%, then vacuum drying oven temperature is adjusted to 106 ℃ and dries to constant weight, pulverize and to obtain 60 object eaglewood leaf powder;
(2) the eaglewood leaf powder of getting step (1) is placed in extraction kettle, after compressing again, in the top of extraction kettle, put into glass cotton balls, preventing the eaglewood leaf powder blocking pipe blowing out, for 1:40 adds deionized water, is 2.0MPa under to carry out subcritical abstraction 10min extracting power according to solid-liquid ratio (unit is g/mL), standingly carry out suction filtration after cooling, then residue is repeated to extract once, merge extracted twice liquid, then obtain concentrated solution through concentrating under reduced pressure;
(3) after step (2) gained concentrated solution is cooling, add NaCl to carry out breakdown of emulsion, then to collect ether layer after extracted with diethyl ether, then by the ether layer Na collecting
2sO
4dewater, after concentrating under reduced pressure, obtain eaglewood leaf volatile oil.
The yield of gained eaglewood leaf volatile oil is that 12.60%, DPPH free radical scavenging activity is shown in Fig. 1.
Embodiment 3
(1) eaglewood leaf is cleaned, is dried and removes branch, then be placed in vacuum drying oven take 46 ℃ be dried to water ratio as 10%, then vacuum drying oven temperature is adjusted to 104 ℃ and dries to constant weight, pulverize and to obtain 100 object eaglewood leaf powder;
(2) the eaglewood leaf powder of getting step (1) is placed in extraction kettle, after compressing again, in the top of extraction kettle, put into glass cotton balls, preventing the eaglewood leaf powder blocking pipe blowing out, for 1:80 adds deionized water, is 4.0MPa under to carry out subcritical abstraction 18min extracting power according to solid-liquid ratio (unit is g/mL), standingly carry out suction filtration after cooling, then residue is repeated to extract once, merge extracted twice liquid, then obtain concentrated solution through concentrating under reduced pressure;
(3) after step (2) gained concentrated solution is cooling, add NaCl to carry out breakdown of emulsion, then to collect ether layer after extracted with diethyl ether, then by the ether layer Na collecting
2sO
4dewater, after concentrating under reduced pressure, obtain eaglewood leaf volatile oil.
The yield of gained eaglewood leaf volatile oil is that 12.85%, DPPH free radical scavenging activity is shown in Fig. 1.
Embodiment 4
(1) eaglewood leaf is cleaned, is dried and removes branch, then be placed in vacuum drying oven take 45 ℃ be dried to water ratio as 6%, then vacuum drying oven temperature is adjusted to 105 ℃ and dries to constant weight, pulverize and to obtain 60 object eaglewood leaf powder;
(2) the eaglewood leaf powder of getting step (1) is placed in extraction kettle, after compressing again, in the top of extraction kettle, put into glass cotton balls, preventing the eaglewood leaf powder blocking pipe blowing out, for 1:40 adds deionized water, is 2.0MPa under to carry out subcritical abstraction 10min extracting power according to solid-liquid ratio (unit is g/mL), standingly carry out suction filtration after cooling, then residue is repeated to extract once, merge extracted twice liquid, then obtain concentrated solution through concentrating under reduced pressure;
(3), after step (2) gained concentrated solution is cooling, add the standing breakdown of emulsion that carries out of NaCl, then to collect ether layer after extracted with diethyl ether, then by the ether layer Na collecting
2sO
4dewater, after concentrating under reduced pressure, obtain eaglewood leaf volatile oil.
The yield of gained eaglewood leaf volatile oil is that 11.42%, DPPH free radical scavenging activity is shown in Fig. 1.
Claims (3)
1. with a method for the active eaglewood leaf volatile oil of subcritical abstraction high anti-oxidation, it is characterized in that through following each step:
(1) eaglewood leaf is cleaned, is dried and removes branch, then being placed in 45 ± 1 ℃, to be dried to water ratio be 5～10%, then dry to constant weight in 105 ± 1 ℃, pulverize and obtain eaglewood leaf powder;
(2) the eaglewood leaf powder of getting step (1) is placed in extraction kettle, according to solid-liquid ratio, be that 1:40～1:80 adds deionized water, extracting power, be under 2.0～4.0MPa, to carry out subcritical abstraction 10～18min, standingly carry out suction filtration after cooling, then residue is repeated to extract once, merge extracted twice liquid, then obtain concentrated solution through concentrating under reduced pressure;
(3) after step (2) gained concentrated solution is cooling, add NaCl to carry out breakdown of emulsion, then to collect ether layer after extracted with diethyl ether, then by the ether layer Na collecting
2sO
4dewater, after concentrating under reduced pressure, obtain eaglewood leaf volatile oil.
2. the method with the active eaglewood leaf volatile oil of subcritical abstraction high anti-oxidation according to claim 1, is characterized in that: the eaglewood leaf powder size of described step (1) is 60～100 orders.
3. the method with the active eaglewood leaf volatile oil of subcritical abstraction high anti-oxidation according to claim 1, is characterized in that: in described step (2), eaglewood leaf powder is placed in extraction kettle, then after compressing, in the top of extraction kettle, puts into glass cotton balls.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104593156A (en) * | 2015-02-04 | 2015-05-06 | 杨祝华 | Method for extracting chimonanthus salicifolius essential oil |
| CN107746749A (en) * | 2017-09-28 | 2018-03-02 | 江永百润福天然植物科技发展有限公司 | A kind of preparation method and Lignum Aquilariae Resinatum extract from agalloch eaglewood residue production Lignum Aquilariae Resinatum extract |
| CN113456551A (en) * | 2021-07-23 | 2021-10-01 | 佛山市梦莎美容化妆品有限公司 | Method for extracting sunscreen component from agilawood leaves and sunscreen composition |
| CN114774202A (en) * | 2022-06-22 | 2022-07-22 | 海南众志承生物科技有限公司 | Preparation method of Hainan Huanghua pear essential oil |
| CN115851380A (en) * | 2023-02-28 | 2023-03-28 | 云南云科特色植物提取实验室有限公司 | Saussurea lappa volatile oil and preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104593156A (en) * | 2015-02-04 | 2015-05-06 | 杨祝华 | Method for extracting chimonanthus salicifolius essential oil |
| CN107746749A (en) * | 2017-09-28 | 2018-03-02 | 江永百润福天然植物科技发展有限公司 | A kind of preparation method and Lignum Aquilariae Resinatum extract from agalloch eaglewood residue production Lignum Aquilariae Resinatum extract |
| CN113456551A (en) * | 2021-07-23 | 2021-10-01 | 佛山市梦莎美容化妆品有限公司 | Method for extracting sunscreen component from agilawood leaves and sunscreen composition |
| CN114774202A (en) * | 2022-06-22 | 2022-07-22 | 海南众志承生物科技有限公司 | Preparation method of Hainan Huanghua pear essential oil |
| CN115851380A (en) * | 2023-02-28 | 2023-03-28 | 云南云科特色植物提取实验室有限公司 | Saussurea lappa volatile oil and preparation method and application thereof |
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Effective date of registration: 20161228 Address after: 335000 Yingtan Economic Development Zone, Jiangxi, Longgang area south of the Eagle Road Patentee after: YINGTAN ZHONGTOU SCIENCE & TECHNOLOGY CO., LTD. Address before: 561000 Anshun high tech Development Zone Industrial Park, Guizhou Patentee before: GUIZHOU HUASHUO BIOLOGICAL SCIENCE & TECHNOLOGY CO., LTD. |