CN101191103B - Method for extracting pine needle essential oil from pine needle - Google Patents
Method for extracting pine needle essential oil from pine needle Download PDFInfo
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- CN101191103B CN101191103B CN2007101686935A CN200710168693A CN101191103B CN 101191103 B CN101191103 B CN 101191103B CN 2007101686935 A CN2007101686935 A CN 2007101686935A CN 200710168693 A CN200710168693 A CN 200710168693A CN 101191103 B CN101191103 B CN 101191103B
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- pine needle
- essential oil
- ionic liquid
- pine
- steam distillation
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Abstract
The invention relates to a method for extracting pine needle essential oil from pine needles. The difference is that: at first, the shade-dried pine needles are crushed and are passed through a 40-mesh sieve, then the hydrophilic ionic liquid is added, the mass-volume ratio of the pine needles and the ionic liquid is 1:2-20 (g: ml), the microwave is adopted to heat the pine needles for complete dissolving, the microwave frequency is 2450MHz, then the conventional steam distillation is adopted to extract the pine needle essential oil, the heating temperature of the microwave is between 80 and 120 DEG C, the hydrophilic ionic liquid is any one of [BMIM]AcO, [BMIM]Cl or[AMIM]Cl. The invention has the advantages that: 1) the preparation method is simple, the obtained pine needle essential oil has good quality and higher yield, the yield is increased by 30 to 49 percent or so compared with that of directly adopting the steam distillation; 2) the hydrophilic ionic liquid can be reclaimed and recycled by adopting the ion exchange method, which can not cause the environmental pollution.
Description
Technical field
The present invention relates to a kind of method of from pine needle, extracting the pine needle essential oil.
Background technology
China is pine tree big country, and pine tree occupies very important position in the forest reserves of China, and for a long time, the pine needle resource fails to obtain good development and utilization, and extracting the pine needle essential oil by pine needle is a kind of effective way of pine needle recycling.The pine needle essential oil is a kind of lurid oily liquids with happy fragrance; Its chemical ingredients more complicated; Mainly comprise terpene alcohol, terpenes, ether, ketone, phenol, phenol fat etc., be widely used in perfume cosmetic industry, spraying essence, perfumed soap, toothpaste, pharmacy and foodstuffs industry.Extract the pine needle essential oil by pine needle at present and mainly adopt steam distillation, organic solvent extractionprocess and supercritical extraction, wherein the steam distillation application is the most extensive, and it is good to obtain pine needle essential oil quality, but yield is lower.
Hydrophilic ionic liquid is a kind of organic liquid material of at room temperature being made up of ion fully, than organic solvent commonly used, because it is non-volatile, can recycle, and is considered to green solvent.Do not see at present that hydrophilic ionic liquid is used for being extracted by pine needle the report of pine needle essential oil.
Summary of the invention
Problem to be solved by this invention is to propose a kind of method of from pine needle, extracting the pine needle essential oil to above-mentioned prior art, and pine needle essential oil quality obtained by this method is good, and the essential oil productive rate is significantly improved.
The present invention by the problem of the above-mentioned proposition of solution the employing solution be: a kind of method of from pine needle, extracting the pine needle essential oil; The pine needle that its difference is at first will to dry in the shade is pulverized; Pulverize the back and cross 40 mesh sieves; To wherein adding hydrophilic ionic liquid, described pine needle and hydrophilic ion liquid mass volume ratio are 1 then: 2-20 (g: ml), adopt microwave heating to pine needle to dissolve fully again; Described microwave frequency 2450MHz adopts conventional steam distillation to extract then and obtains the pine needle essential oil.
Press such scheme, described microwave heating temperature is 80～120 ℃.
Press such scheme, described hydrophilic ionic liquid is [BMIM] AcO, any one among [BMIM] Cl or [AMIM] Cl.
Advantage of the present invention:
1) preparation method is simple, and it is good to obtain pine needle essential oil quality, and yield is higher, and is higher by about 30～49% than the productive rate of direct employing steam distillation;
2) adopt hydrophilic ionic liquid can adopt the ion exchange method recycling use, can not cause environmental pollution basically.
Embodiment
Embodiment 1:
The pine needle that 20g dries in the shade is pulverized; Pulverize the back and cross 40 mesh sieves,, adopt microwave heating (Heating temperature is 120 ℃) to pine needle to dissolve fully more then to wherein adding the hydrophilic ionic liquid of 100ml [BMIM] AcO; Described microwave frequency 2450MHz; Adopting conventional steam distillation to extract then and obtaining lurid oily liquids is pine needle essential oil 102mg, and adopts conventional steam distillation to get lurid oily liquids 68.5mg, and productive rate improves 48.9%; Both specific densities, refractive index is consistent with the UV absorption peak.
Embodiment 2:
The pine needle that 20g dries in the shade is pulverized; Pulverize the back and cross 40 mesh sieves,, adopt microwave heating (Heating temperature is 100 ℃) to pine needle to dissolve fully more then to wherein adding the hydrophilic ionic liquid of 150ml [BMIM] Cl; Described microwave frequency 2450MHz; Adopting conventional steam distillation to extract then and obtaining lurid oily liquids is pine needle essential oil 90mg, and adopts conventional steam distillation to get lurid oily liquids 68.5mg, and productive rate improves 31.4%; Both specific densities, refractive index is consistent with the UV absorption peak.
Embodiment 3:
The pine needle that 20g dries in the shade is pulverized; Pulverize the back and cross 40 mesh sieves,, adopt microwave heating (Heating temperature is 80 ℃) to pine needle to dissolve fully more then to wherein adding the hydrophilic ionic liquid of 120ml [AMIM] Cl; Described microwave frequency 2450MHz; Adopting conventional steam distillation to extract then and obtaining lurid oily liquids is pine needle essential oil 92mg, and adopts conventional steam distillation to get lurid oily liquids 68.5mg, and productive rate improves 34.3%; Both specific densities, refractive index is consistent with the UV absorption peak.
Embodiment 4:
The pine needle that 20g dries in the shade is pulverized; Pulverize the back and cross 40 mesh sieves,, adopt microwave heating (Heating temperature is 80 ℃) to pine needle to dissolve fully more then to wherein adding the hydrophilic ionic liquid of 100ml [BMIM] AcO; Described microwave frequency 2450MHz; Adopting conventional steam distillation to extract then and obtaining lurid oily liquids is pine needle essential oil 98mg, and adopts conventional steam distillation to get lurid oily liquids 68.5mg, and productive rate improves 43.1%; Both specific densities, refractive index is consistent with the UV absorption peak.
Embodiment 5:
The pine needle that 20g dries in the shade is pulverized; Pulverize the back and cross 40 mesh sieves,, adopt microwave heating (Heating temperature is 105 ℃) to pine needle to dissolve fully more then to wherein adding the hydrophilic ionic liquid of 40ml [BMIM] Cl; Described microwave frequency 2450MHz; Adopting conventional steam distillation to extract then and obtaining lurid oily liquids is pine needle essential oil 96mg, and adopts conventional steam distillation to get lurid oily liquids 68.5mg, and productive rate improves 40.1%; Both specific densities, refractive index is consistent with the UV absorption peak.
Embodiment 6:
The pine needle that 20g dries in the shade is pulverized; Pulverize the back and cross 40 mesh sieves,, adopt microwave heating (Heating temperature is 100 ℃) to pine needle to dissolve fully more then to wherein adding the hydrophilic ionic liquid of 400ml [BMIM] AcO; Described microwave frequency 2450MHz; Adopting conventional steam distillation to extract then and obtaining lurid oily liquids is pine needle essential oil 99mg, and adopts conventional steam distillation to get lurid oily liquids 68.5mg, and productive rate improves 44.5%; Both specific densities, refractive index is consistent with the UV absorption peak.
The hydrophilic ionic liquid that the foregoing description 1-6 is adopted all adopts industry or laboratory chemical reagent, and its weight percent concentration is more than 95%.
Claims (2)
1. method of from pine needle, extracting the pine needle essential oil; The pine needle that it is characterized in that at first will drying in the shade is pulverized, and pulverizes the back and crosses 40 mesh sieves, then to wherein adding hydrophilic ionic liquid; Described hydrophilic ionic liquid is [BMIM] AcO; Among [BMIM] Cl or [AMIM] Cl any one, described pine needle and hydrophilic ion liquid mass volume ratio are 1: 2-20 (g: ml), adopt microwave heating to pine needle to dissolve fully again; Described microwave frequency 2450MHz adopts conventional steam distillation to extract then and obtains the pine needle essential oil.
2. by the described method of from pine needle, extracting the pine needle essential oil of claim 1, it is characterized in that described microwave heating temperature is 80～120 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101686935A CN101191103B (en) | 2007-12-10 | 2007-12-10 | Method for extracting pine needle essential oil from pine needle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101686935A CN101191103B (en) | 2007-12-10 | 2007-12-10 | Method for extracting pine needle essential oil from pine needle |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101191103A CN101191103A (en) | 2008-06-04 |
| CN101191103B true CN101191103B (en) | 2012-01-11 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2007101686935A Expired - Fee Related CN101191103B (en) | 2007-12-10 | 2007-12-10 | Method for extracting pine needle essential oil from pine needle |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101411468B (en) * | 2008-12-01 | 2012-07-04 | 浙江师范大学 | Pine needle extract of slash pine and use thereof in food fresh keeping |
| CN101880597B (en) * | 2010-07-08 | 2012-06-27 | 河北科技大学 | Method for extracting rice bran oil by using ionic liquid and supercritical carbon dioxide (CO2) |
| EP2726588B1 (en) | 2011-06-28 | 2015-07-29 | Givaudan SA | Ionic liquids for agricultural residue removal |
| CN103215120A (en) * | 2013-05-09 | 2013-07-24 | 刘映良 | Extracting process of pine needle volatile oil of masson pine by steam distillation method |
| CN103725418A (en) * | 2013-12-20 | 2014-04-16 | 茂名市德威圣科技有限责任公司 | Method for extracting jack fruit aromatherapy oil from ionic liquid |
| CN104232311B (en) * | 2014-09-02 | 2016-09-21 | 华南理工大学 | A kind of extracting method of ginger essential oil |
| CN104490947A (en) * | 2014-12-12 | 2015-04-08 | 广西科技大学 | Application of pinus crassicorticea pine needle essential oil |
| CN108851195B (en) * | 2018-07-26 | 2021-05-18 | 湖北中烟工业有限责任公司 | Preparation method of alfalfa refined extract for cigarettes |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1510119A (en) * | 2002-09-14 | 2004-07-07 | 白山市科学技术研究所 | Firconcrete, extrait, essential oil and preparing method thereof |
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2007
- 2007-12-10 CN CN2007101686935A patent/CN101191103B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1510119A (en) * | 2002-09-14 | 2004-07-07 | 白山市科学技术研究所 | Firconcrete, extrait, essential oil and preparing method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 刘晓庚 等.酶法提取松针精油的实验室研究.《林产化学与工业》.2005,第25卷(第3期),111-114. * |
| 樊金拴.巴山冷杉精油提取工艺研究.《西北林学院学报》.1998,第13卷(第3期),45-49. * |
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| CN101191103A (en) | 2008-06-04 |
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