CN104087420B - A kind of subcritical extraction method improving volatile oil anti-oxidant activity in eaglewood leaf - Google Patents
A kind of subcritical extraction method improving volatile oil anti-oxidant activity in eaglewood leaf Download PDFInfo
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Abstract
The invention provides a kind of with the method for the active eaglewood leaf volatile oil of subcritical abstraction high anti-oxidation, eaglewood leaf is carried out clean, dry and remove branch, be dried to again close to over dry, then dry to constant weight, pulverizing obtains eaglewood leaf powder, be placed in extraction kettle again to add deionized water and carry out subcritical abstraction, suction filtration is carried out after leaving standstill cooling, then residue is repeated to extract once, merge extracted twice liquid, then obtain concentrated solution through concentrating under reduced pressure, then add NaCl and carry out breakdown of emulsion, to collect ether layer after extracted with diethyl ether, then the ether layer Na that will collect
2sO
4dewater, after concentrating under reduced pressure, namely obtain eaglewood leaf volatile oil.Gained eaglewood leaf volatile oil has anti-oxidant, enhancing body immunologic function and antitumor isoreactivity, compares traditional method and has the antioxidant effect significantly improved.The method extraction time is short, and using nontoxic, harmless water as Extraction solvent, quantity of solvent is few, and yield is high, cost is low; And Feedstock treating is simple.
Description
Technical field
The present invention relates to a kind of subcritical extraction method improving volatile oil anti-oxidant activity in eaglewood leaf, belong to Nature inorganic bone technical field.
Background technology
As the agalloch eaglewood of traditional Chinese medical science common medicine, in each version of the Pharmacopoeia of the People's Republic of China, all have the record to its source, function etc., it is mainly derived from Isolated From Thymelaeaceae Species Lignum Aquilariae Resinatum [Aquilariasinensis (Lour.) Gilg] timber containing resin.Agalloch eaglewood fragrant odour, taste is pained, and 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, and always, the vexed pain of its treatment chest abdomen medical, 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, containing the composition 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 carry out harvesting 2 times, so output is larger every year in enormous quantities.As the volatile oil extracted in eaglewood leaf, not only there is relieving inflammation and relaxing pain, the anti-oxidant and effect such as to delay senility, meanwhile, also can be used as spices, be used for making highclass perfumes, perfumed soap, essence and makeup and adding in tobacco flavouring etc. 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 with the general name of steam distillation and the not miscible oily liquids of water.The plant distributions with volatile oil is extensive, and only just there are 56 sections in China, and 136 belong to, containing volatile oil in about 300 kind of plant.Eaglewood leaf volatile oil is the important activeconstituents of a class, has multiple pharmacologically active and the application in 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 respective shortcoming, as low in the rate of recovery, impurity is many, high temperature causes heat-sensitive ingredients destruction, 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 few 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 the destruction that the rate of recovery is low, impurity is many, high temperature causes heat-sensitive ingredients, the dissolvent residual that overcome conventional steam distillation, organic solvent extractionprocess exists, the problems such as disadvantageous effect are brought to active substance, the invention provides a kind of subcritical extraction method improving volatile oil anti-oxidant activity in eaglewood leaf.
The present invention utilizes subcritical energy to heat the solvent contacted with sample, is separated by required compound, enters in solvent from sample matrices.Specifically through following each step:
(1) eaglewood leaf is carried out clean, dry and remove branch, then being placed in 45 ± 1 DEG C, to be dried to water ratio be 5 ~ 10%, then dries to constant weight in 105 ± 1 DEG C, pulverize and obtain eaglewood leaf powder;
(2) the eaglewood leaf powder getting step (1) is placed in extraction kettle, be that 1:40 ~ 1:80 adds deionized water according to solid-liquid ratio, subcritical abstraction 10 ~ 18min is carried out under extraction power is 2.0 ~ 4.0MPa, suction filtration is carried out after leaving standstill cooling, then residue is repeated to extract once, merge extracted twice liquid, then obtain concentrated solution through concentrating under reduced pressure;
(3) after the cooling of step (2) gained concentrated solution, add NaCl and carry out breakdown of emulsion, then to collect ether layer after extracted with diethyl ether, then the ether layer Na that will collect
2sO
4dewater, after concentrating under reduced pressure, namely 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, puts into glass cotton balls in the top of extraction kettle, prevents the eaglewood leaf powder blocking pipe blown out.
The present invention follows the example of by the subcritical assisted Extraction improved for the purpose of eaglewood leaf volatile oil anti-oxidant activity, can overcome conventional steam distillation, disadvantageous effect that organic solvent extraction brings active substance; Utilize subcritical energy to heat the solvent contacted with sample, required compound is separated from sample matrices, enters 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, improve 2.14 ~ 3.09 times than wet distillation extraction method, there is the antioxidant effect significantly improved.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 compared to 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.The rate of recovery of this extracting method to target component is high, extraction time is short, and using nontoxic, harmless water as Extraction solvent, quantity of solvent is few, and yield is high, cost is low; And Feedstock treating is simple, simplifies 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 is drawn technology in the leaf that has a extensive future.Carry out compared with extraction with utilizing organic solvent, technical process science of the present invention, rationally, do not need to use Organic chemical solvents 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 constituent is high, good stability, makes the features such as the product diversification of eaglewood leaf volatile oil, seriation.
Accompanying drawing explanation
Fig. 1 is the yield, the DPPH free radical scavenging activity that measure volatile oil in gained eaglewood leaf.
Embodiment
Below provide embodiment, the invention will be further described.
Embodiment 1
(1) eaglewood leaf is carried out clean, dry and remove branch, then be placed in vacuum drying oven and be dried to water ratio for 8% with 45 DEG C, then vacuum drying oven temperature is adjusted to 105 DEG C and dries to constant weight, pulverize and obtain 80 object eaglewood leaf powder;
(2) the eaglewood leaf powder getting step (1) is placed in extraction kettle, after compressing again, glass cotton balls is put in the top of extraction kettle, prevent the eaglewood leaf powder blocking pipe blown out, according to solid-liquid ratio (unit is g/mL) for 1:60 adds deionized water, under extraction power is 3.0MPa, carry out subcritical abstraction 14min, suction filtration is carried out after leaving standstill cooling, then residue is repeated to extract once, merge extracted twice liquid, then obtain concentrated solution through concentrating under reduced pressure;
(3) after the cooling of step (2) gained concentrated solution, add NaCl and leave standstill and carry out breakdown of emulsion, then to collect ether layer after extracted with diethyl ether, then the ether layer Na that will collect
2sO
4dewater, after concentrating under reduced pressure, namely 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 carried out clean, dry and remove branch, then be placed in vacuum drying oven and be dried to water ratio for 5% with 44 DEG C, then vacuum drying oven temperature is adjusted to 106 DEG C and dries to constant weight, pulverize and obtain 60 object eaglewood leaf powder;
(2) the eaglewood leaf powder getting step (1) is placed in extraction kettle, after compressing again, glass cotton balls is put in the top of extraction kettle, prevent the eaglewood leaf powder blocking pipe blown out, according to solid-liquid ratio (unit is g/mL) for 1:40 adds deionized water, under extraction power is 2.0MPa, carry out subcritical abstraction 10min, suction filtration is carried out after leaving standstill cooling, then residue is repeated to extract once, merge extracted twice liquid, then obtain concentrated solution through concentrating under reduced pressure;
(3) after the cooling of step (2) gained concentrated solution, add NaCl and carry out breakdown of emulsion, then to collect ether layer after extracted with diethyl ether, then the ether layer Na that will collect
2sO
4dewater, after concentrating under reduced pressure, namely 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 carried out clean, dry and remove branch, then be placed in vacuum drying oven and be dried to water ratio for 10% with 46 DEG C, then vacuum drying oven temperature is adjusted to 104 DEG C and dries to constant weight, pulverize and obtain 100 object eaglewood leaf powder;
(2) the eaglewood leaf powder getting step (1) is placed in extraction kettle, after compressing again, glass cotton balls is put in the top of extraction kettle, prevent the eaglewood leaf powder blocking pipe blown out, according to solid-liquid ratio (unit is g/mL) for 1:80 adds deionized water, under extraction power is 4.0MPa, carry out subcritical abstraction 18min, suction filtration is carried out after leaving standstill cooling, then residue is repeated to extract once, merge extracted twice liquid, then obtain concentrated solution through concentrating under reduced pressure;
(3) after the cooling of step (2) gained concentrated solution, add NaCl and carry out breakdown of emulsion, then to collect ether layer after extracted with diethyl ether, then the ether layer Na that will collect
2sO
4dewater, after concentrating under reduced pressure, namely 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 carried out clean, dry and remove branch, then be placed in vacuum drying oven and be dried to water ratio for 6% with 45 DEG C, then vacuum drying oven temperature is adjusted to 105 DEG C and dries to constant weight, pulverize and obtain 60 object eaglewood leaf powder;
(2) the eaglewood leaf powder getting step (1) is placed in extraction kettle, after compressing again, glass cotton balls is put in the top of extraction kettle, prevent the eaglewood leaf powder blocking pipe blown out, according to solid-liquid ratio (unit is g/mL) for 1:40 adds deionized water, under extraction power is 2.0MPa, carry out subcritical abstraction 10min, suction filtration is carried out after leaving standstill cooling, then residue is repeated to extract once, merge extracted twice liquid, then obtain concentrated solution through concentrating under reduced pressure;
(3) after the cooling of step (2) gained concentrated solution, add NaCl and leave standstill and carry out breakdown of emulsion, then to collect ether layer after extracted with diethyl ether, then the ether layer Na that will collect
2sO
4dewater, after concentrating under reduced pressure, namely 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 carried out clean, dry and remove branch, then being placed in 45 ± 1 DEG C, to be dried to water ratio be 5 ~ 10%, then dries to constant weight in 105 ± 1 DEG C, pulverize and obtain eaglewood leaf powder;
(2) the eaglewood leaf powder getting step (1) is placed in extraction kettle, be that 1:40 ~ 1:80 adds deionized water according to solid-liquid ratio, subcritical abstraction 10 ~ 18min is carried out under extraction power is 2.0 ~ 4.0MPa, suction filtration is carried out after leaving standstill cooling, then residue is repeated to extract once, merge extracted twice liquid, then obtain concentrated solution through concentrating under reduced pressure;
(3) after the cooling of step (2) gained concentrated solution, add NaCl and carry out breakdown of emulsion, then to collect ether layer after extracted with diethyl ether, then the ether layer Na that will collect
2sO
4dewater, after concentrating under reduced pressure, namely obtain eaglewood leaf volatile oil.
2. according to claim 1 with the method for the active eaglewood leaf volatile oil of subcritical abstraction high anti-oxidation, it is characterized in that: the eaglewood leaf powder size of described step (1) is 60 ~ 100 orders.
3. according to claim 1 with the method for the active eaglewood leaf volatile oil of subcritical abstraction high anti-oxidation, it is characterized in that: in described step (2), eaglewood leaf powder is placed in extraction kettle, then after compressing, put into glass cotton balls in the top of extraction kettle.
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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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| CN103184102A (en) * | 2013-01-14 | 2013-07-03 | 中山市国林沉香科学研究所 | A kind of extraction method of agarwood essential oil and application of agarwood essential oil |
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| 亚临界水萃取在天然产物有效成分提取中的研究新进展;李新莹等;《食品工业科技》;20120822(第23期);第415页右栏第1段 * |
| 沉香叶挥发油化学成分的GC-MS分析;刘玉峰等;《中国现代中药》;20070831;第9卷(第8期);第7页摘要、第2.1小节 * |
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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. |