CN101486950B - Preparation of Perilla leaf clean oil - Google Patents
Preparation of Perilla leaf clean oil Download PDFInfo
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- CN101486950B CN101486950B CN2009100069097A CN200910006909A CN101486950B CN 101486950 B CN101486950 B CN 101486950B CN 2009100069097 A CN2009100069097 A CN 2009100069097A CN 200910006909 A CN200910006909 A CN 200910006909A CN 101486950 B CN101486950 B CN 101486950B
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Abstract
The invention discloses a preparation method of folium perillae neat oil, which consists of preparing folium perillae powder, organic solvent reflowing, extracting and concentrating, re-suspending, freezing, sucking filtrating and concentrating, and molecular distillation separating and purifying to obtain the folium perillae neat oil. The obtained su cotyledon neat oil is used in the cigarette flavoring, can improve the fragrance and increase the smoothness and fine degree of the smoke, and reveals unique delicate fragrance.
Description
Technical field
The present invention relates to a kind of preparation method of Perilla leaf clean oil.
Background technology
Wild perillaseed is a Labiatae elscholtiza platymiscium, has another name called tortoise leaf grass, dog day grass, and the property sugariness is bitter, per nnial herb.Have important medicinal function, can be used for treating diseases such as swelling and pain in the throat, rheumatism flu, gastritis, arthralgia, cancer are early stage, snake bite and insect sting.And as the seasonings of characteristic, its unique fragrance is widely accepted, and along with the further investigation of its chemical ingredients, wild perillaseed absolute oil also will be utilized effectively in the perfuming cigarette process.
At present; Domestic and international widely used method is: after the raw materials pretreatment; Add certain organic solvent; Extract volatilization and semi-volatility component in the wild perillaseed leaf with while distillation extraction method or steam distillation, extracting liquid filtering obtains wild perillaseed leaf essential oil after concentrating, and organic solvent commonly used is methylene dichloride, ethanol, anhydrous diethyl ether etc.Though this method technology is simple, quality product is not ideal, often has macromolecular substance such as pigment, xylogen, wax, is unfavorable for the application in cigarette.
Molecular distillation technique is as a kind of novel liquid-liquid separation technology; Material can distill under the hypoxemia inert conditions; Therefore; Have that distillation temperature is low, heated time is short, working pressure is low, separation degree and productive rate is high, good product quality, composition changes and does not wait the incomparable advantage of other stripping technique very much before and after the distillation.This technology has been widely used in fields such as petrochemical complex, food spice, the extraction that is particularly suitable for natural product with separate.But the research report that at present both at home and abroad is applied to wild perillaseed absolute oil exploitation about molecular distillation technique seldom.And the thick oil that the present invention utilizes molecular distillation technique that tradition is extracted is handled; The absolute oil that obtains has been removed the impurity (macromolecular substance such as wax, pigment that wherein are unfavorable for the cigarette smoking quality to greatest extent; Solvent); And better kept the effective constituent in the absolute oil, well avoided the destruction of ordinary method effective constituent in its sepn process and the introducing of impurity, more helped its application in perfuming cigarette.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of Perilla leaf clean oil; This preparing method's efficient is high, effective constituent is not destroyed, pollution-free, technology is simple; The wild Perilla leaf clean oil of preparation is best in quality; Be applied to perfuming cigarette, can improve the utility value of wild perillaseed, can compensate coke tar in cigarette again and reduce the fragrance loss that causes.
For achieving the above object, technical scheme provided by the present invention is: a kind of preparation method of Perilla leaf clean oil comprises that preparation perillaseed leaf powder, organic solvent refluxing extraction concentrate, return concentrated, the short-path distillation separation and purification of molten freezing suction filtration, obtain Perilla leaf clean oil.
Said preparation perillaseed leaf powder is: the perillaseed leaf is dried under 40 ℃ of conditions pulverized 20～100 mesh sieves, obtain perillaseed leaf powder.
Said organic solvent refluxing extraction simmer down to: perillaseed leaf powder is packed in the refluxing extraction jar, add the ethanol of 5～10 times of perillaseed leaf grain weight amounts, refluxing extraction concentrated after 24～72 hours, obtained perillaseed leaf cream just.
Dissolve freezing suction filtration simmer down to for said time: adds 8～16 times of perillaseed leaves ethanol of paste volume just, return to dissolve and filter concentratedly after freezing 12～24 hours, it is slightly oily to obtain the perillaseed leaf.
Said short-path distillation separation and purification is: the thick oil of perillaseed leaf is carried out selective separation with molecular distillation technique purify, enrichment obtains Perilla leaf clean oil less than 120～160 ℃ component.
The advantage that the present invention has: 1, technology of the present invention is simple; Stable, preparation efficiency is high, and the thick oil that utilizes molecular distillation technique that tradition is extracted is handled; The absolute oil that obtains has been removed the impurity (macromolecular substance such as wax, pigment that wherein are unfavorable for the cigarette smoking quality to greatest extent; Solvent), and better keeps the effective constituent in the absolute oil, well avoided the destruction of ordinary method effective constituent in its sepn process and the introducing of impurity.
2, Perilla leaf clean oil has perfuming effect preferably in cigarette, can enrich cigarette perfume (or spice), improves comfortableness, give the cigarette characteristic smell fragrant with inhale flavor, it is remarkable to mend fragrant effect for the cigarette flavouring, for compensating aroma of low tar cigarette provides a new thinking.
3, embodiment of the present invention, the wild perillaseed resource in abundant Changbai Mountain capable of using is developed the value of wild perillaseed, improves peasant's income.
Description of drawings:
Below in conjunction with accompanying drawing and embodiment the present invention is done further explain, but content of the present invention is not limited to the embodiment that lifted.
Fig. 1 is a process flow sheet of the present invention.
Embodiment:
Embodiment 1
A kind of preparation method of Perilla leaf clean oil and the application in perfuming cigarette thereof; Comprise the pre-treatment of perillaseed leaf raw material, organic solvent refluxing extraction concentrate, return dissolve freezing, suction filtration concentrates, short-path distillation separation and purification, absolute oil GC/MS are analyzed and perfumed applications, concrete process step is following:
(1) the perillaseed leaf is dried under 40 ℃ of conditions pulverizes 20～100 mesh sieves, obtain perillaseed leaf powder.
(2) the perillaseed leaf powder that step (1) is obtained is packed in the refluxing extraction jar, adds ethanol, and refluxing extraction concentrated after 72 hours, obtains perillaseed leaf cream just.
(3) the perillaseed leaf that step (2) is obtained is cream just, adds ethanol, returns to dissolve to filter concentratedly after freezing 12～24 hours, obtains slightly oil of perillaseed leaf.
(4) the perillaseed leaf that step (3) is obtained is oil slightly, carries out selective separation with molecular distillation technique and purify, and enrichment obtains Perilla leaf clean oil less than 150 ℃ component.
(5) Perilla leaf clean oil that step (4) is obtained carries out GC/MS and analyzes; 24 compounds have wherein been identified; Major part is ketone, aldehydes, ester class, sesquiterpene, alcohols and hydrocarbons, and main flavour ingredient has phantol, elsholtzione, dehydroelscholtzione, peruviol etc.
(6) Perilla leaf clean oil of step (5) with ethanol or terepthaloyl moietie or 1, behind the 2-Ucar 35 dilution finite concentration, is used for perfuming cigarette (being sprayed at pipe tobacco).
(7) the schisandra chinensis neat oil perfuming concentration of step (6) is 0.5 ‰～1.0 ‰.
Embodiment 2
A kind of preparation method of Perilla leaf clean oil and the application in perfuming cigarette thereof, it is that perillaseed leaf powder is packed in the refluxing extraction jar, adds ethanol, refluxing extraction obtained perillaseed leaf cream just after 48 hours after concentrating; Add ethanol again and return and dissolve that suction filtration concentrates after freezing 24 hours, obtain slightly oil of perillaseed leaf; Carry out selective separation with molecular distillation technique and purify, enrichment obtains Perilla leaf clean oil less than 120 ℃ component, and absolute oil is analyzed its staple of back evaluation through GC/MS, is used for perfuming cigarette then.
Embodiment 3
A kind of preparation method of Perilla leaf clean oil and the application in perfuming cigarette thereof, it is that perillaseed leaf powder is packed in the refluxing extraction jar, adds ethanol, refluxing extraction obtained perillaseed leaf cream just after 36 hours after concentrating; Add ethanol again and return and dissolve that suction filtration concentrates after freezing 24 hours, obtain slightly oil of perillaseed leaf; Carry out selective separation with molecular distillation technique and purify, enrichment obtains Perilla leaf clean oil less than 160 ℃ component, and absolute oil is analyzed its staple of back evaluation through GC/MS, is used for perfuming cigarette then.
The above only is preferred embodiment of the present invention, is not the present invention is done any pro forma restriction; Though the present invention discloses as above with preferred embodiment; Yet be not in order to limiting the present invention, anyly be familiar with the professional and technical personnel, in not breaking away from technical scheme scope of the present invention; When the technology contents of above-mentioned announcement capable of using is made a little change or is modified to the equivalent embodiment of equivalent variations; In every case be the content that does not break away from technical scheme of the present invention, to any simple modification, equivalent variations and modification that above embodiment did, all still belong in the scope of technical scheme of the present invention according to technical spirit of the present invention.
Claims (2)
1. the preparation method of a wild Perilla leaf clean oil comprises that the wild perillaseed leaf powder of preparation, organic solvent refluxing extraction concentrate, return concentrated, the short-path distillation separation and purification of molten freezing suction filtration, obtain wild Perilla leaf clean oil;
Said organic solvent refluxing extraction simmer down to: wild perillaseed leaf powder is packed in the refluxing extraction jar, add the ethanol of 5～10 times of wild perillaseed leaf grain weight amounts, refluxing extraction concentrated after 24～72 hours, obtained wild perillaseed leaf cream just;
Dissolve freezing suction filtration simmer down to for said time: just add 8～16 times of wild perillaseed leaves ethanol of paste volume just in the cream toward wild perillaseed leaf, return to dissolve and filter concentratedly after freezing 12～24 hours, it is slightly oily to obtain wild perillaseed leaf;
Said short-path distillation separation and purification is: the thick oil of wild perillaseed leaf is carried out selective separation with molecular distillation technique purify, enrichment obtains wild Perilla leaf clean oil less than 160 ℃ component.
2. the preparation method of wild Perilla leaf clean oil according to claim 1, it is characterized in that: the wild perillaseed leaf of said preparation powder is: wild perillaseed leaf is dried under 40 ℃ of conditions pulverized 20～100 mesh sieves, obtain wild perillaseed leaf powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2009100069097A CN101486950B (en) | 2009-02-05 | 2009-02-05 | Preparation of Perilla leaf clean oil |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009100069097A CN101486950B (en) | 2009-02-05 | 2009-02-05 | Preparation of Perilla leaf clean oil |
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| CN101486950A CN101486950A (en) | 2009-07-22 |
| CN101486950B true CN101486950B (en) | 2012-05-23 |
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| CN2009100069097A Active CN101486950B (en) | 2009-02-05 | 2009-02-05 | Preparation of Perilla leaf clean oil |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104489901B (en) * | 2014-12-03 | 2016-06-29 | 河南中烟工业有限责任公司 | One grows tobacco taste tobacco juice for electronic smoke |
| CN109105949A (en) * | 2018-07-05 | 2019-01-01 | 湖北中烟工业有限责任公司 | A kind of stage extraction preparation method and applications of extractive of perilla |
| CN109722340B (en) * | 2019-01-04 | 2022-01-28 | 云南中烟工业有限责任公司 | Preparation method and application of elsholtzia rugulosa tobacco flavor |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101040036A (en) * | 2004-10-19 | 2007-09-19 | 味之素株式会社 | Method of concentrating minor ingredient contained in oily matter obtained from plant tissue |
| CN101249110A (en) * | 2008-04-07 | 2008-08-27 | 四川省中医药科学院 | Volatile oil component extracting separation method of plants medicinal materials and application thereof |
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2009
- 2009-02-05 CN CN2009100069097A patent/CN101486950B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101040036A (en) * | 2004-10-19 | 2007-09-19 | 味之素株式会社 | Method of concentrating minor ingredient contained in oily matter obtained from plant tissue |
| CN101249110A (en) * | 2008-04-07 | 2008-08-27 | 四川省中医药科学院 | Volatile oil component extracting separation method of plants medicinal materials and application thereof |
Non-Patent Citations (4)
| Title |
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| 彭安顺 等.天然香料的精制和分离.《精细有机品化学》.石油大学出版社,1996,(第1版),223. * |
| 朱甘培.十种中国香薷属植物挥发油的气相色谱-质谱分析.《中国中药杂志》.1990,第15卷(第11期),37-39,63. * |
| 胡浩斌等.香芝麻蒿挥发油的提取分离及抑菌作用.《中国医院药学杂志》.2006,第26卷(第01期),14-16. * |
| 那微等.GC-MS分析尾叶香茶菜挥发油成分.《吉林农业大学学报》.2005,第27卷(第04期),413-415. * |
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Effective date of registration: 20190917 Address after: 133001 No. 795 Tianchi Road, Jilin, Yanji Patentee after: Jilin Tobacco Industry Co., Ltd. Address before: 133001 Jilin Tobacco Industry Co., Ltd. technology center, No. 1099, Jilin Road, Jilin, Changchun Co-patentee before: Yanji Changbaishan Technology Service Co., Ltd. Patentee before: Jilin Tobacco Industry Co., Ltd. |