CN101457177A - Method for extracting water-soluble volatilization component from shortleaf kyllinga - Google Patents
Method for extracting water-soluble volatilization component from shortleaf kyllinga Download PDFInfo
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- CN101457177A CN101457177A CNA2008100739728A CN200810073972A CN101457177A CN 101457177 A CN101457177 A CN 101457177A CN A2008100739728 A CNA2008100739728 A CN A2008100739728A CN 200810073972 A CN200810073972 A CN 200810073972A CN 101457177 A CN101457177 A CN 101457177A
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Abstract
The invention discloses a method for extracting water-soluble volatile components from Kyllinga brevifolia comprising the following steps: chopping dry Kyllinga brevifolia and soaking for 4-36hours, extracting for 1-12hours in a steam distillation device, receiving oil phase parts of a distillate to obtain the Kyllinga brevifolia volatile oil; redistilling residual distillate after the distillation and receiving the distillate, extracting the distillate by organic solvent after the distillate salting out, vacuum concentrating the extract at a temperature of 50-70 DEG C in a water-bath and obtaining oil-like components which are Kyllinga brevifolia volatile components. The Kyllinga brevifolia water-soluble volatile components have finer and softer aroma and better application effect in tobacco flavoring comparing to the volatile oil extracted by conventional steam distillation method, moreover because the antioxidant ability of the Kyllinga brevifolia volatile components is greatly stronger than the volatile oil extracted by conventional steam distillation method, the harm of smoking to health can be reduced in the tobacco flavoring application, which accords with the long-run development trend of the tobacco industry.
Description
Technical field
The present invention relates to from natural tobacco aromatics using, extract the method for water-soluble volatile component, the particularly a kind of method that can from Shortleaf Kyllinga Herb, extract water-soluble volatile component.
Background technology
Volatile oil is the important source material of allotment flavouring essence for tobacco, widespread use in flavouring essence for tobacco.The production of volatile oil at present all is to adopt traditional wet distillation technology, generally only collects in the distillate oil phase part as the product of volatile oil.The shortcoming of this technology maximum is that the water-soluble volatile component in the raw material is difficult for extracting.Volatile component of plant can be divided into two big classes, and a class is oxygen-free terpene compound, and is water insoluble, do not have significant fragrance, is not the fragrance ingredient of volatile oil.Another kind of is oxygen containing terpenoid, though content is not high usually, gives off a strong fragrance, and has represented the distinctive fragrance of volatile oil, is most valuable part in the essential oil.The biological activity such as anti-oxidant, antibiotic that studies show that this class material is far above oxygen-free terpene compound.These oxygenatedchemicalss are slightly soluble in water, are impossible they are fully isolating by simple mechanics means, and are slightly soluble in this part essential oil of water, because the water oil ratio of distillate is little, to distillate ratio shared in the essential oil be appreciable whole.
Shortleaf Kyllinga Herb (kyllinga brevifolia Rottb) is the herb of Cyperaceae per nnial herb Shortleaf Kyllinga Herb, mainly originates in East China, Central China, south China, each provinces and regions, southwest.Shortleaf Kyllinga Herb can make in the blood plasmodium eliminate or reduce, and the traditional Chinese medical science is commonly used for diaphoretic for the treatment of colds and influenza, and treatment malaria and flu among the peoplely are used as the wound medication.Shortleaf Kyllinga Herb contains volatile oil, its main component of essential oil is α-Pai Xi, beta-pinene, phantol, alpha-terpineol, thymol, α-caryophyllene, β-caryophyllene, beta-elemene, cypress camphor, palmitic acid, phytol, oleic acid, 3,7,11,15-tetramethyl--2,6,10,14-16 carbon tetraene-1-alcohol etc., wherein multiple oxygenatedchemicals composition can use in tobacco flavoring.Can increase delicate fragrance as phantol, improve jealously, improve hot note flavor.Alpha-terpineol can improve flue gas, increases blue or green fragrant, the fresh flavor of cigarette.Organic acid such as palmitic acid, oleic acid can in and the contained alkaline matter of flue gas, suppressing flue gas stimulates.These contain the oxygen volatile constituent and are slightly soluble in water, and adopting wet distillation technology is they all can't be extracted.The present invention adopts organic solvent extractionprocess to extract the water-soluble volatile component of Shortleaf Kyllinga Herb from distillate when adopting wet distillation technology to extract Shortleaf Kyllinga Herb volatile oil.
Volatile oil is because water insoluble application aspect a lot of is restricted, and water-soluble volatile component is better than general volatile oil in this respect far away, can be greatly improved in application facet.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of method of extracting water-soluble volatile component from Shortleaf Kyllinga Herb.
The present invention solves the problems of the technologies described above by the following technical programs:
The present invention adopts organic solvent extractionprocess to extract the water-soluble volatile component of Shortleaf Kyllinga Herb from distillate when adopting wet distillation technology to extract Shortleaf Kyllinga Herb volatile oil; Earlier with the chopping of exsiccant Shortleaf Kyllinga Herb, being soaked in water is placed on that distillation extraction goes out Shortleaf Kyllinga Herb volatile oil in the wet distillation device, carries out according to the following steps again: a. with described distillation afterwards remaining distillate distill again, collect distillate; B. a certain amount of sodium-chlor of adding or Repone K are saltoutd in the distillate; C. then with the distillate organic solvent extraction, extraction liquid is concentrating under reduced pressure under the water bath condition of certain temperature, and the oily matter that obtains is the water-soluble volatile component of Shortleaf Kyllinga Herb.
The extraction yield of the water-soluble volatile component of Shortleaf Kyllinga Herb will be higher than the volatile oil contents that direct employing wet distillation technology is extracted, the water-soluble volatile component that extracts is a reddish-brown oily matter, has the Shortleaf Kyllinga Herb characteristic perfume, fragrance is fine and smooth more soft, experimental studies have found that, the biological activity of the water-soluble volatile component of Shortleaf Kyllinga Herb will be higher than the volatile oil that adopts wet distillation technology directly to extract far away, particularly aspect anti-oxidant activity, the anti-oxidant activity of water-soluble volatile component is more than 20 times of volatile oil that directly extract.
When adopting wet distillation technology to extract Shortleaf Kyllinga Herb volatile oil, utilize the remaining distillate in distillation back to extract the water-soluble volatile component of Shortleaf Kyllinga Herb, the Shortleaf Kyllinga Herb raw material is fully used; The water-soluble volatile component fragrance of the Shortleaf Kyllinga Herb of extracting is fine and smooth more soft, can enrich cigarette perfume (or spice), obviously promote flue gas concentration, effect is better on perfuming cigarette, and because the resistance of oxidation of the water-soluble volatile component of Shortleaf Kyllinga Herb will be better than the Shortleaf Kyllinga Herb oil that general steam distillation extracts greatly, on perfuming cigarette, use and to reduce the harm of smoking, meet the long-run development trend of tobacco industry for health.
Embodiment
The present invention will be described in further detail by following examples, but scope of the present invention is not limited to these embodiment certainly.
Embodiment 1
Accurately take by weighing 0.5 kilogram of exsiccant Shortleaf Kyllinga Herb herb, soaked 10 hours with 5 kg water the chopping back.Place the wet distillation device then, adopt steam distillation to extract 6 hours, collect the oil phase part in the distillate, obtain 1.0 gram Shortleaf Kyllinga Herb volatile oil.To distill the remaining distillate in back and distill again, collect distillate.Add 0.5 kilogram of sodium-chlor in the distillate and saltout, use ethyl acetate extraction then, the above-mentioned extraction liquid of concentrating under reduced pressure under 70 ℃ water bath condition, the 1.5 gram reddish-brown oily matter that obtain are the water-soluble volatile component of Shortleaf Kyllinga Herb.
With the Shortleaf Kyllinga Herb volatile oil that extracts and the water-soluble volatile component of Shortleaf Kyllinga Herb respectively in 0.012% ratio of pipe tobacco weight, be sprayed at according to the processing sequence of conventional perfuming and roll into cigarette on the sample pipe tobacco and prop up, and under constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) condition balance 48 hours.The sensory evolution result show added Shortleaf Kyllinga Herb volatile oil and water-soluble volatile component in the pipe tobacco after, can enrich cigarette perfume (or spice), obviously promote flue gas concentration.
Embodiment 2
Accurately take by weighing 10 kilograms of exsiccant Shortleaf Kyllinga Herb herbs, steeped 20 hours with 40 kilograms water logging the chopping back.Place the wet distillation device then, adopt steam distillation to extract 12 hours, collect the oil phase part in the distillate, obtain 25.3 gram Shortleaf Kyllinga Herb volatile oil.To distill the remaining distillate in back and distill again, collect distillate.Add 2 kilograms of sodium-chlor in the distillate and saltout, with sherwood oil (30-60) extraction, the above-mentioned extraction liquid of concentrating under reduced pressure under 55 ℃ water bath condition, the 40.8 gram reddish-brown oily matter that obtain are the water-soluble volatile component of Shortleaf Kyllinga Herb.
With the Shortleaf Kyllinga Herb hair oil that extracts and the water-soluble volatile component of Shortleaf Kyllinga Herb respectively in 0.05% ratio of pipe tobacco weight, be sprayed at according to the processing sequence of conventional perfuming and roll into cigarette on the sample pipe tobacco and prop up, and under constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) condition balance 48 hours.Effect is with embodiment 1.
Embodiment 3
Accurately take by weighing 1 kilogram of exsiccant Shortleaf Kyllinga Herb herb, soaked 24 hours with 4 kg water the chopping back.Place the wet distillation device then, adopt steam distillation to extract 6 hours, collect the oil phase part in the distillate, obtain 2.1 gram Shortleaf Kyllinga Herb volatile oil.To distill the remaining raffinate in back and distill again, collect distillate.Add 0.5 kilogram of Repone K in the distillate and saltout, use extracted with diethyl ether then, the above-mentioned extraction liquid of concentrating under reduced pressure under 60 ℃ water bath condition, the 4.0 gram reddish-brown oily matter that obtain are the water-soluble volatile component of Shortleaf Kyllinga Herb.
With the Shortleaf Kyllinga Herb volatile oil that extracts and the water-soluble volatile component of Shortleaf Kyllinga Herb respectively in 0.05% ratio of pipe tobacco weight, be sprayed at according to the processing sequence of conventional perfuming and roll into cigarette on the sample pipe tobacco and prop up, and under constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) condition balance 48 hours.Effect is with embodiment 1.
Embodiment 4
Accurately take by weighing 2 kilograms of exsiccant Shortleaf Kyllinga Herb herbs, soaked 4 hours with 18 kg water the chopping back.Place the wet distillation device then, adopt steam distillation to extract 8 hours, collect the oil phase part in the distillate, obtain 5.3 gram Shortleaf Kyllinga Herb volatile oil.To distill the remaining distillate in back and distill again, collect distillate.Add 1.2 kilograms of sodium-chlor in the distillate and saltout, use dichloromethane extraction, the above-mentioned extraction liquid of concentrating under reduced pressure under 70 ℃ water bath condition, the 8.1 gram reddish-brown oily matter that obtain are the water-soluble volatile component of Shortleaf Kyllinga Herb.
With the Shortleaf Kyllinga Herb volatile oil that extracts and the water-soluble volatile component of Shortleaf Kyllinga Herb respectively in 0.03% ratio of pipe tobacco weight, be sprayed at according to the processing sequence of conventional perfuming and roll into cigarette on the sample pipe tobacco and prop up, and under constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) condition balance 48 hours.Effect is with embodiment 1.
Embodiment 5
Accurately take by weighing 1.5 kilograms of exsiccant Shortleaf Kyllinga Herb herbs, soaked 12 hours with 5 kg water the chopping back.Place the wet distillation device then, adopt steam distillation to extract 2 hours, collect the oil phase part in the distillate, obtain 2.6 gram Shortleaf Kyllinga Herb volatile oil.To distill the remaining distillate in back and distill again, collect distillate.Adding 0.5 kilogram of sodium-chlor in the distillate saltouts, it is sherwood oil (30-60) with weight ratio then: the organic solvent extraction of methylene dichloride=60: 40, the above-mentioned extraction liquid of concentrating under reduced pressure under 50 ℃ water bath condition, the 4.5 gram reddish-brown oily matter that obtain are the water-soluble volatile component of Shortleaf Kyllinga Herb.
With the Shortleaf Kyllinga Herb volatile oil that extracts and the water-soluble volatile component of Shortleaf Kyllinga Herb respectively in 0.01% ratio of pipe tobacco weight, be sprayed at according to the processing sequence of conventional perfuming and roll into cigarette on the sample pipe tobacco and prop up, and under constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) condition balance 48 hours.Effect is with embodiment 1.
Embodiment 6
Accurately take by weighing 3 kilograms of exsiccant Shortleaf Kyllinga Herb herbs, soaked 36 hours with 30 kg water the chopping back.Place the wet distillation device then, adopt steam distillation to extract 6 hours, collect the oil phase part in the distillate, obtain 6.2 gram Shortleaf Kyllinga Herb volatile oil.To distill the remaining distillate in back and distill again, collect distillate.Adding 1.5 kilograms of sodium-chlor in the distillate, is ether with weight ratio then: the organic solvent extraction of methylene dichloride=60: 40, the above-mentioned extraction liquid of concentrating under reduced pressure under 50 ℃ water bath condition, obtain 9 to restrain the reddish-brown oily matter be the water-soluble volatile component of Shortleaf Kyllinga Herb.
With the Shortleaf Kyllinga Herb volatile oil that extracts and the water-soluble volatile component of Shortleaf Kyllinga Herb respectively in 0.03% ratio of pipe tobacco weight, be sprayed at according to the processing sequence of conventional perfuming and roll into cigarette on the sample pipe tobacco and prop up, and under constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) condition balance 48 hours.Effect is with embodiment 1.
Embodiment 7
Accurately take by weighing 0.5 kilogram of exsiccant Shortleaf Kyllinga Herb herb, soaked 24 hours with 2 kg water the chopping back.Place the wet distillation device then, adopt steam distillation to extract 4 hours, collect the oil phase part in the distillate, obtain 1.1 gram Shortleaf Kyllinga Herb volatile oil.To distill the remaining distillate in back and distill again, collect distillate.Add 0.2 kilogram of sodium-chlor in the distillate, use n-hexane extraction then, the above-mentioned extraction liquid of concentrating under reduced pressure under 50 ℃ water bath condition, the 1.8 gram reddish-brown oily matter that obtain are the water-soluble volatile component of Shortleaf Kyllinga Herb.
With the Shortleaf Kyllinga Herb volatile oil that extracts and the water-soluble volatile component of Shortleaf Kyllinga Herb respectively in 0.02% ratio of pipe tobacco weight, be sprayed at according to the processing sequence of conventional perfuming and roll into cigarette on the sample pipe tobacco and prop up, and under constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) condition balance 48 hours.Effect is with embodiment 1.
Embodiment 8
Accurately take by weighing 1.0 kilograms of exsiccant Shortleaf Kyllinga Herb herbs, soaked 10 hours with 5 kg water the chopping back.Place the wet distillation device then, adopt steam distillation to extract 12 hours, collect the oil phase part of distillate, obtain 2.4 gram Shortleaf Kyllinga Herb volatile oil.To distill the remaining distillate in back and distill again, collect distillate.Add 0.5 kilogram of sodium-chlor in the distillate and saltout, use dichloromethane extraction then, the above-mentioned extraction liquid of concentrating under reduced pressure under 50 ℃ water bath condition, the 4.5 gram reddish-brown oily matter that obtain are the water-soluble volatile component of Shortleaf Kyllinga Herb.
With the Shortleaf Kyllinga Herb volatile oil that extracts and the water-soluble volatile component of Shortleaf Kyllinga Herb respectively in 0.03% ratio of pipe tobacco weight, be sprayed at according to the processing sequence of conventional perfuming and roll into cigarette on the sample pipe tobacco and prop up, and under constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) condition balance 48 hours.Effect is with embodiment 1.
Claims (4)
1. method of from Shortleaf Kyllinga Herb, extracting water-soluble volatile component, with the chopping of exsiccant Shortleaf Kyllinga Herb, being soaked in water is placed on that distillation extraction goes out Shortleaf Kyllinga Herb volatile oil in the wet distillation device, it is characterized in that further comprising the steps of:
A. the remaining distillate in described distillation back is distilled again, collect distillate;
B. a certain amount of sodium-chlor of adding or Repone K are saltoutd in the distillate;
C. then with the distillate organic solvent extraction, extraction liquid is concentrating under reduced pressure under the water bath condition of certain temperature, and the oily matter that obtains is the water-soluble volatile component of Shortleaf Kyllinga Herb.
2. the method for from Shortleaf Kyllinga Herb, extracting water-soluble volatile component according to claim 1, it is characterized in that: described dry Shortleaf Kyllinga Herb chopping was soaked in water 4～36 hours, Shortleaf Kyllinga Herb: the weight ratio of water=1: 3～20 placed wet distillation device distillation extraction 1～12 hour.
3. the method for from Shortleaf Kyllinga Herb, extracting water-soluble volatile component according to claim 1 and 2, it is characterized in that: the add-on of described sodium-chlor or Repone K is 5%～35% of a distillate weight, and described extraction liquid carries out concentrating under reduced pressure under 50～70 ℃ of water bath condition.
4. the method for extracting water-soluble volatile component from Shortleaf Kyllinga Herb according to claim 1 is characterized in that: the described organic solvent that is used for extracting is any one or a few of sherwood oil, normal hexane, ethyl acetate, methylene dichloride, ether.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNA2008100739728A CN101457177A (en) | 2008-12-10 | 2008-12-10 | Method for extracting water-soluble volatilization component from shortleaf kyllinga |
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| CNA2008100739728A CN101457177A (en) | 2008-12-10 | 2008-12-10 | Method for extracting water-soluble volatilization component from shortleaf kyllinga |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102250690A (en) * | 2011-06-09 | 2011-11-23 | 安徽中草香料有限公司 | Preparation process of celery leaf oil |
| CN102499459A (en) * | 2011-10-28 | 2012-06-20 | 浙江中烟工业有限责任公司 | Natural plant essential oil, preparation method thereof and application of natural plant essential oil to cigarettes |
| CN103504464A (en) * | 2013-09-30 | 2014-01-15 | 广东中烟工业有限责任公司 | Method for preparing cut tobacco with wetness keeping and cough relieving effects |
-
2008
- 2008-12-10 CN CNA2008100739728A patent/CN101457177A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102250690A (en) * | 2011-06-09 | 2011-11-23 | 安徽中草香料有限公司 | Preparation process of celery leaf oil |
| CN102499459A (en) * | 2011-10-28 | 2012-06-20 | 浙江中烟工业有限责任公司 | Natural plant essential oil, preparation method thereof and application of natural plant essential oil to cigarettes |
| CN103504464A (en) * | 2013-09-30 | 2014-01-15 | 广东中烟工业有限责任公司 | Method for preparing cut tobacco with wetness keeping and cough relieving effects |
| CN103504464B (en) * | 2013-09-30 | 2015-09-30 | 广东中烟工业有限责任公司 | A kind of preparation method with the pipe tobacco of humectation antitussive action |
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Open date: 20090617 |