CN104547286A - Method for preparing Chinese Eaglewood leaf extract - Google Patents
Method for preparing Chinese Eaglewood leaf extract Download PDFInfo
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- CN104547286A CN104547286A CN201410820053.8A CN201410820053A CN104547286A CN 104547286 A CN104547286 A CN 104547286A CN 201410820053 A CN201410820053 A CN 201410820053A CN 104547286 A CN104547286 A CN 104547286A
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- lignum aquilariae
- aquilariae resinatum
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Abstract
The invention discloses a method for preparing Chinese Eaglewood leaf extract. The method comprises the following steps: firstly, ultrasonically treating the Chinese Eaglewood leaf; secondly, carrying out CO2 supercritical extraction with the ultrasonic treatment solution and high-purity ethanol as an entrainer; finally, carrying out molecular distillation and concentration to obtain the Chinese Eaglewood leaf extract. According to the method, the ultrasonic treatment, the CO2 supercritical extraction and the molecular distillation technology are combined to extract active ingredients in the Chinese Eaglewood leaf, the obtained extract has high content of active ingredients and a high extraction rate of raw materials; the extraction rate of the obtained Chinese Eaglewood leaf extract obtained by the method is 20 to 40% higher than that obtained by the prior art, and the method is simple to operate.
Description
Technical field
The present invention relates to a kind of extracting method of effective ingredients in plant, specifically a kind of preparation method of Lignum Aquilariae Resinatum leaf extract.
Background technology
Lignum Aquilariae Resinatum is that thymelaeceae (Thymelaeaceae) Lignum Aquilariae Resinatum belongs to (Aquilaria) Lignum Aquilariae Resinatum (Aquilaria sinensis (Lour.) Gilg) and congener Lignum Aquilariae Resinatum (Aquilria agallocha Roxb.) resiniferous timber.The biological element amount that Lignum Aquilariae Resinatum leaf contains needed by human is extremely abundant, as calcium, zinc, ferrum, manganese etc. and vitamin, be the supplement of the good particular nutrient of human body, and multiple disadvantage factor in human body can be eliminated that there is QI invigorating benefit essence, adjusting blood lipid, dredging internal organs function, relieving mental strain and helping sleep, blood fat reducing, help sleep, effect of skin care.
Lignum Aquilariae Resinatum leaf can be used for Chinese medicine health-care, the medicine or tea etc. of preparing various adjusting blood lipid blood glucose etc.The extracting method of Lignum Aquilariae Resinatum leaf effective ingredient still mainly solvent extraction method at present.Disclose one in CN104004594A with Rhizoma Atractylodis macrocephalae Herba Pelargonii Graveolentis for raw material, use enzyme process to carry out broken wall treatment to raw material, obtain extractum in conjunction with circumfluence distillation, then use supercritical extraction extracts Lignum Aquilariae Resinatum leaf essential oil from extractum.CN101011499B discloses a kind of method of Lignum Aquilariae Resinatum leaf extract, is by the leaf of Lignum Aquilariae Resinatum percolation or reflux, extract, after soaking, reconcentration and get final product, and is wherein the ethanol of 10 ~ 80% for the solvent of percolation or reflux, extract, is weight percentage.The traditional batch technique that solvent method extracts after continuing to use for many years always and pulverizing, the object that raw material is first pulverized is to accelerate extraction rate, but also brings the problems such as reinforced discharging labor intensity is large, solid-liquor separation is difficult, solvent consumption is large, energy consumption is large, efficiency is low, production is unstable simultaneously.
Summary of the invention
The object of the invention is the preparation method providing a kind of Lignum Aquilariae Resinatum leaf extract.
The technical solution adopted in the present invention is: a kind of preparation method of Lignum Aquilariae Resinatum leaf extract, is following concrete steps:
(1) select the fresh leaf of fresh, dry Lignum Aquilariae Resinatum leaf, clean, get prophyll or be processed into coarse powder further, being placed on volume fraction is in the alcoholic solution of 20 ~ 90%, and at supersound process 2 ~ 100min, ultrasonic end, retains sonification fluid, for subsequent use;
(2) take out the Lignum Aquilariae Resinatum leaf after supersound process or coarse powder, being dried to moisture is 5 ~ 70%, pulverizes, obtains Lignum Aquilariae Resinatum leaf powder, be placed in CO
2in supercritical extraction reactor, be that entrainer carries out supercritical CO with the ethanol mixed solution that 1:5 is mixed to get by volume of the sonification fluid of step (1) and volume fraction 40 ~ 95%
2extraction, obtains volatile oil;
(3) extraction terminates, and through distilling under reduced pressure, reclaims ethanol; Volatile oil is placed in molecular distillation equipment and carries out molecular distillation, adopt technological parameter to be: distillation pressure 100 ~ 200Pa, vapo(u)rizing temperature 20 ~ 80 DEG C, knifing speed 100r/min, condensation temperature 10 DEG C, preheat temperature 25 DEG C, material flow 1.0ml/min, obtains Lignum Aquilariae Resinatum leaf extract.
Preferred extraction process parameter is as follows: pressure of storage tank 8Mpa, extraction kettle pressure 35MPa, extraction kettle temperature 42 DEG C, extraction-container pressure are 10MPa, extraction-container temperature is 38 DEG C, cooling water temperature 2 DEG C, CO
2flow 28kg/h, extraction time 150min.
Preferably, described step (1) adopts volume fraction to be the alcoholic solution of 75 ~ 90%.
Preferably, during described molecular distillation, distillation pressure 110Pa, vapo(u)rizing temperature 30 DEG C.
Lignum Aquilariae Resinatum leaf of the present invention is the leaf that thymelaeceae (Thymelaeaceae) Lignum Aquilariae Resinatum genus (Aquilaria) Lignum Aquilariae Resinatum (Aquilaria sinensis (Lour.) Gilg) and/or congener Lignum Aquilariae Resinatum (Aquilria agallocha Roxb.) are set.
The present invention adopts supersound process, CO
2supercritical extraction combines with molecular distillation technique the active component extracted in Lignum Aquilariae Resinatum leaf, the extract active constituent content obtained is high, raw material abstraction rate is high, and the Lignum Aquilariae Resinatum leaf extract extraction yield that extraction obtains comparatively prior art can improve 20 ~ 40%, and method is simple to operation.
Detailed description of the invention
Be described in further details the present invention below by embodiment, these embodiments are only used for the present invention is described, do not limit the scope of the invention.
Embodiment 1: adopt following method to prepare Lignum Aquilariae Resinatum leaf extract of the present invention:
(1) select the fresh leaf of fresh, dry Lignum Aquilariae Resinatum leaf, clean, remove petiole, being placed on volume fraction by solid-to-liquid ratio 1:5 is in the alcoholic solution of 75%, supersound process 10min under frequency 55kHz, ultrasonic end, retains sonification fluid, for subsequent use;
(2) take out the Lignum Aquilariae Resinatum leaf after supersound process, being dried to moisture is 20%, pulverizes, crosses 80 mesh sieves, obtain Lignum Aquilariae Resinatum leaf powder, be placed in CO
2in supercritical extraction reactor, be that entrainer carries out supercritical CO with the ethanol mixed solution that 1:5 is mixed to get by volume of the sonification fluid of step (1) and volume fraction 95%
2extraction, obtains volatile oil; Wherein, the supercritical extraction process parameter of employing is as follows: pressure of storage tank 8Mpa, extraction kettle pressure 35MPa, extraction kettle temperature 42 DEG C, extraction-container pressure are 10MPa, extraction-container temperature is 38 DEG C, cooling water temperature 2 DEG C, CO
2flow 28kg/h, extraction time 150min;
(3) extraction terminates, and through distilling under reduced pressure, reclaims ethanol; Volatile oil is placed in molecular distillation equipment and carries out molecular distillation, adopt technological parameter to be: distillation pressure 110Pa, vapo(u)rizing temperature 30 DEG C, knifing speed 100r/min, condensation temperature 10 DEG C, preheat temperature 25 DEG C, material flow 1.0ml/min, obtains Lignum Aquilariae Resinatum leaf extract.
Embodiment 2: adopt following method to prepare Lignum Aquilariae Resinatum leaf extract of the present invention:
(1) select the fresh leaf of fresh, dry Lignum Aquilariae Resinatum leaf, clean, remove petiole, being placed on volume fraction by solid-to-liquid ratio 1:3 is in the alcoholic solution of 90%, supersound process 10min under frequency 55kHz, ultrasonic end, retains sonification fluid, for subsequent use;
(2) take out the Lignum Aquilariae Resinatum leaf after supersound process, being dried to moisture is 20%, pulverizes, crosses 80 mesh sieves, obtain Lignum Aquilariae Resinatum leaf powder, be placed in CO
2in supercritical extraction reactor, be that entrainer carries out supercritical CO with the ethanol mixed solution that 1:5 is mixed to get by volume of the sonification fluid of step (1) and volume fraction 95%
2extraction, obtains volatile oil; Wherein, the supercritical extraction process parameter of employing is as follows: pressure of storage tank 8Mpa, extraction kettle pressure 35MPa, extraction kettle temperature 42 DEG C, extraction-container pressure are 10MPa, extraction-container temperature is 38 DEG C, cooling water temperature 2 DEG C, CO
2flow 28kg/h, extraction time 150min;
(3) extraction terminates, and through distilling under reduced pressure, reclaims ethanol; Volatile oil is placed in molecular distillation equipment and carries out molecular distillation, adopt technological parameter to be: distillation pressure 120Pa, vapo(u)rizing temperature 35 DEG C, knifing speed 100r/min, condensation temperature 10 DEG C, preheat temperature 25 DEG C, material flow 1.0ml/min, obtains Lignum Aquilariae Resinatum leaf extract.
Claims (5)
1. a preparation method for Lignum Aquilariae Resinatum leaf extract, is characterized in that: adopt following concrete steps:
(1) select the fresh leaf of fresh, dry Lignum Aquilariae Resinatum leaf, clean, get prophyll or be processed into coarse powder further, being placed on volume fraction is in the alcoholic solution of 20 ~ 90%, and at supersound process 2 ~ 100min, ultrasonic end, retains sonification fluid, for subsequent use;
(2) take out the Lignum Aquilariae Resinatum leaf after supersound process or coarse powder, being dried to moisture is 5 ~ 70%, pulverizes, obtains Lignum Aquilariae Resinatum leaf powder, be placed in CO
2in supercritical extraction reactor, be that entrainer carries out supercritical CO with the ethanol mixed solution that 1:5 is mixed to get by volume of the sonification fluid of step (1) and volume fraction 40 ~ 95%
2extraction, obtains volatile oil;
(3) extraction terminates, and through distilling under reduced pressure, reclaims ethanol; Volatile oil is placed in molecular distillation equipment and carries out molecular distillation, adopt technological parameter to be: distillation pressure 100 ~ 200Pa, vapo(u)rizing temperature 20 ~ 80 DEG C, knifing speed 100r/min, condensation temperature 10 DEG C, preheat temperature 25 DEG C, material flow 1.0ml/min, obtains Lignum Aquilariae Resinatum leaf extract.
2. method according to claim 1, is characterized in that: described extraction process parameter is as follows: pressure of storage tank 8Mpa, extraction kettle pressure 35MPa, extraction kettle temperature 42 DEG C, extraction-container pressure are 10MPa, extraction-container temperature is 38 DEG C, cooling water temperature 2 DEG C, CO
2flow 28kg/h, extraction time 150min.
3. method according to claim 1, is characterized in that: described step (1) adopts volume fraction to be the alcoholic solution of 75 ~ 90%.
4. method according to claim 1, is characterized in that: during described molecular distillation, distillation pressure 110Pa, vapo(u)rizing temperature 30 DEG C.
5. method according to claim 1, is characterized in that: described Lignum Aquilariae Resinatum leaf is the leaf that thymelaeceae (Thymelaeaceae) Lignum Aquilariae Resinatum genus (Aquilaria) Lignum Aquilariae Resinatum (Aquilaria sinensis (Lour.) Gilg) and/or congener Lignum Aquilariae Resinatum (Aquilria agallocha Roxb.) are set.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410820053.8A CN104547286A (en) | 2014-12-25 | 2014-12-25 | Method for preparing Chinese Eaglewood leaf extract |
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| CN201410820053.8A CN104547286A (en) | 2014-12-25 | 2014-12-25 | Method for preparing Chinese Eaglewood leaf extract |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107446706A (en) * | 2017-09-25 | 2017-12-08 | 广西壮族自治区农业科学院农产品加工研究所 | A kind of extracting method of mango core essential oil and its application in banana fresh-keeping |
| CN108102788A (en) * | 2018-01-22 | 2018-06-01 | 重庆汇达柠檬科技集团有限公司 | The extracting method of essential oil in a kind of lemonlike citrus leaf |
| CN111481483A (en) * | 2020-05-19 | 2020-08-04 | 广州市天然芳香科学技术研究院有限公司 | Aquilaria sinensis hydrolat and preparation method thereof |
| CN115463181A (en) * | 2021-06-10 | 2022-12-13 | 长沙学院 | Preparation method of agilawood leaf extract |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2013035771A (en) * | 2011-08-05 | 2013-02-21 | Api Co Ltd | Aquilaria leaf composition and production method thereof, and method for producing aquilaria leaf extract |
| CN103351954A (en) * | 2013-07-11 | 2013-10-16 | 大连卓尔高科技有限公司 | Process for extracting eaglewood essential oil by using supercritical carbon dioxide |
-
2014
- 2014-12-25 CN CN201410820053.8A patent/CN104547286A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013035771A (en) * | 2011-08-05 | 2013-02-21 | Api Co Ltd | Aquilaria leaf composition and production method thereof, and method for producing aquilaria leaf extract |
| CN103351954A (en) * | 2013-07-11 | 2013-10-16 | 大连卓尔高科技有限公司 | Process for extracting eaglewood essential oil by using supercritical carbon dioxide |
Non-Patent Citations (3)
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| 刘明石等: "超临界CO2萃取沉香叶挥发油工艺条件优化研究", 《中国酿造》 * |
| 李天祥等: "分子蒸馏分离超临界CO2萃取的米槁精油及其成分分析", 《精细化工》 * |
| 林芳花等: "沉香叶提取工艺及其抗氧化活性实验研究", 《中国野生植物资源》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107446706A (en) * | 2017-09-25 | 2017-12-08 | 广西壮族自治区农业科学院农产品加工研究所 | A kind of extracting method of mango core essential oil and its application in banana fresh-keeping |
| CN108102788A (en) * | 2018-01-22 | 2018-06-01 | 重庆汇达柠檬科技集团有限公司 | The extracting method of essential oil in a kind of lemonlike citrus leaf |
| CN111481483A (en) * | 2020-05-19 | 2020-08-04 | 广州市天然芳香科学技术研究院有限公司 | Aquilaria sinensis hydrolat and preparation method thereof |
| CN115463181A (en) * | 2021-06-10 | 2022-12-13 | 长沙学院 | Preparation method of agilawood leaf extract |
| CN115463181B (en) * | 2021-06-10 | 2024-01-30 | 长沙学院 | Preparation method of agilawood leaf extract |
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