CN109875110B - Rhodiola rosea extract, preparation method and application thereof and prepared tobacco shreds - Google Patents
Rhodiola rosea extract, preparation method and application thereof and prepared tobacco shreds Download PDFInfo
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Abstract
The invention relates to the technical field of plant extraction, and particularly relates to a rhodiola rosea extract, a preparation method and application thereof, and prepared tobacco shreds. The preparation method of the rhodiola rosea extract comprises the following steps: extracting radix Rhodiolae under reflux, and vacuum filtering to obtain extract; carrying out gas-liquid micro-extraction on the extract to obtain a rhodiola rosea extract; the extraction system of the gas-liquid microextraction consists of inert gas with the flow rate of 1.8-2.5 mL/min and an extraction solvent; the extraction solvent is one or more than two of dichloromethane, methanol or n-hexane. The method provided by the invention can effectively extract volatile and semi-volatile substances in the rhodiola rosea, and the obtained rhodiola rosea extract is used for flavoring cut tobacco to prepare cigarettes, so that the impure gas of tobacco can be effectively reduced, the fragrance harmony of the cigarettes is increased, the irritation of the cigarettes to throats is reduced, and the smoking quality of the cigarettes is improved.
Description
Technical Field
The invention relates to the technical field of plant extraction, in particular to a rhodiola rosea extract, a preparation method and application thereof and prepared tobacco shreds.
Background
With the increasing pressure of work and life, more people use tobacco as a stress-relieving placebo. Smoking is very likely to cause cardiovascular diseases, lung cancer and other respiratory diseases. Not only smokers, but also people who are in a large amount of passive smoking for a long time are high-incidence people of the diseases. However, as the health consciousness of people is continuously improved, more and more tobacco enterprises try to apply various natural ingredients to prepare cigarettes so as to improve the quality of the cigarettes and reduce the stimulation of the cigarettes to human bodies.
Rhodiola rosea, also called arctic root and golden root, is one of Crassulaceae plants, is a Chinese herbal medicine distributed in northwest of Yunnan and Tibet areas of China, has the effects of tonifying qi, activating blood circulation and promoting blood circulation to relieve asthma, and is used for aspects of qi deficiency, blood stasis, chest stuffiness, heartache, stroke, hemiplegia, lassitude, asthma and the like. The radix Rhodiolae also has antioxidant, cold resisting, high temperature resisting, radiation resisting, and antiaging effects, and contains Salidroside as effective component.
The application of rhodiola rosea is mainly focused on medicines with the functions of tonifying qi and activating blood, and promoting blood circulation and relieving asthma, and cosmetics with the functions of resisting oxidation and whitening, and reports that rhodiola rosea extract is used for preparing cigarettes are rare.
Disclosure of Invention
In view of the above, the present invention aims to provide a rhodiola rosea extract, a preparation method and an application thereof, and a prepared tobacco shred. The obtained rhodiola rosea extract is used for flavoring cut tobacco to prepare cigarettes, so that the impure gas of the tobacco can be effectively reduced, the fragrance harmony of the cigarettes is increased, the irritation of the cigarettes to throats is reduced, and the smoking quality of the cigarettes is improved.
In order to realize the purpose of the invention, the invention adopts the following technical scheme:
a preparation method of rhodiola rosea extract comprises the following steps:
extracting radix Rhodiolae under reflux, and vacuum filtering to obtain extract;
carrying out gas-liquid micro-extraction on the extract to obtain a rhodiola rosea extract;
the extraction system of the gas-liquid microextraction consists of inert gas with the flow rate of 1.8-2.5 mL/min and an extraction solvent;
the extraction solvent is one or more than two of dichloromethane, methanol and n-hexane.
The preparation method provided by the invention combines a hot reflux extraction technology with a gas-liquid microextraction technology, adopts a specific extraction solvent and inert gas, and selects a proper inert gas flow rate, so that volatile and semi-volatile substances in the rhodiola rosea can be effectively extracted. The obtained rhodiola rosea extract is volatile and is used for flavoring cut tobacco to prepare cigarettes, so that the impure gas of the cigarettes can be effectively reduced, the fragrance harmony of the cigarettes is increased, the irritation of the cigarettes to throats is reduced, and the smoking quality of the cigarettes is improved.
In some embodiments, the extraction solvent is n-hexane and dichloromethane in a volume ratio of 1: 1.
In the preparation method provided by the invention, the inert gas is selected from nitrogen, helium, argon or carbon dioxide. In some embodiments, the inert gas is nitrogen.
In the preparation method provided by the invention, the gas-liquid micro-extraction time is 3-5 min, and the gas-liquid micro-extraction temperature is 250-300 ℃. In some embodiments, the time for gas-liquid microextraction is 4min, and the temperature for gas-liquid microextraction is 250 ℃.
In some embodiments, the solvent for the hot reflux extraction is 70-75% ethanol, and the extraction time is 2-3 h. In some embodiments, the solvent for the hot reflux extraction is 70% ethanol, and the extraction time is 2 h.
In some embodiments, in the hot reflux extraction, the mass-volume ratio of the rhodiola rosea to the 60-80% ethanol is 5Kg: 4000-5000 mL. In some embodiments, the mass volume ratio of the rhodiola rosea to the 70% ethanol is 5Kg to 5000 ml.
The invention also provides the rhodiola root extract prepared by the preparation method.
In one embodiment of the invention, the influence of rhodiola rosea extracts with different proportions on the cigarette smoking evaluation result is examined, and the result shows that the rhodiola rosea extracts prepared by the method are added with fragrance to tobacco shreds to prepare cigarettes, so that the impure gas of the tobacco can be effectively reduced, the fragrance harmony of the cigarettes is increased, the irritation of the cigarettes to throats is reduced, and the smoking quality of the cigarettes is improved. Therefore, the invention also provides the application of the rhodiola rosea extract in preparing cigarettes.
The invention also provides tobacco shreds containing the rhodiola root extract.
In the tobacco shreds provided by the invention, the mass fraction of the rhodiola rosea extract is 0.01-0.1%
The preparation method of the cut tobacco provided by the invention comprises the following steps: diluting radix Rhodiolae extract with ethanol, and spraying tobacco shred.
The invention also provides a cigarette made of the tobacco shred.
The invention provides a rhodiola rosea extract, a preparation method and application thereof and prepared cut tobacco. The preparation method of the rhodiola rosea extract comprises the following steps: extracting radix Rhodiolae under reflux, and vacuum filtering to obtain extract; carrying out gas-liquid micro-extraction on the extract to obtain a rhodiola rosea extract; the extraction system of the gas-liquid microextraction consists of inert gas with the flow rate of 1.8-2.5 mL/min and an extraction solvent; the extraction solvent is dichloromethane, methanol or n-hexane. Through cigarette evaluation tests, the results show that the rhodiola rosea extract prepared by the method is added into tobacco shreds to be flavored into cigarettes, so that the impure gas of the tobaccos can be effectively reduced, the fragrance harmony of the cigarettes is increased, the irritation of the cigarettes to throats is reduced, and the smoking quality of the cigarettes is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a bar graph comparing the content of volatile and semi-volatile components in rhodiola rosea extracts of examples 1 to 3 and comparative examples 1 to 2, wherein 1 is furfural, 2 is furfuryl alcohol, 3 is 2-cyclopentene-1, 4-dione, 4 is styrene, 5 is benzyl alcohol, 6 is 2-formyl-5-methylfuran, 7 is allyl benzene, 8 is o-vinyltoluene, 9 is phenethyl alcohol, 10 is 1-octanol, 11 is o-cymene, 12 is cinnamyl alcohol, 13 is p-hydroxyacetophenone, 14 is-methyl-3-hydroxy-4-pyrone, 15 is anisol, 16 is limonene, 17 is geranial, 18 is (1,1, 5-trimethyl-4, 6-dienheptanol, 19 is geraniol, 20 is 2, 6-dimethoxyphenol, 21 is linalool oxide, 22 is alpha-terpineol, 23 is alloy albizzia alkane, and 24 is linalool oxide;
FIG. 2 is a schematic view of a gas-liquid microextraction device;
FIG. 3 is a total ion chromatogram of example 1.
Detailed Description
The invention discloses a rhodiola rosea extract, a preparation method and application thereof and prepared cut tobacco, and a person skilled in the art can realize the preparation by properly improving process parameters by referring to the content. It is expressly intended that all such similar substitutes and modifications which would be obvious to one skilled in the art are deemed to be included in the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
The description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
The test materials adopted by the invention are all common commercial products and can be purchased in the market.
The invention is further illustrated by the following examples:
example 1
Drying 3Kg of rhodiola rosea, extracting for 2h by 70% ethanol hot reflux, and carrying out vacuum filtration to obtain 500g of extract. Placing 5mg of the extract in a sample cell of an ME-101 gas-liquid microextraction instrument (see figure 2), and sealing the opening of the sample cell by using a spacer; then, a polytetrafluoroethylene pipeline with the outer diameter of 1/16mm and the inner diameter of 0.25mm is used for connecting the sample pool with the receiving phase, and two ends of the polytetrafluoroethylene pipeline are connected with needle tubes; the receiving phase is 200 μ L liner tube, and 50 μ L n-hexane is added into the receiving phase for gas-liquid micro-extraction to obtain radix Rhodiolae extract. Wherein the extraction time of gas-liquid microextraction is 4 min; the extraction temperature was 250 ℃, the receiving phase condensing temperature was-4 ℃ and the nitrogen flow rate blown into the sample cell was 2 mL/min.
Example 2
Drying 3Kg of rhodiola rosea, extracting for 2h by 70% ethanol hot reflux, and carrying out vacuum filtration to obtain 500g of extract. Placing 5mg of the extract in a sample cell of a micro-extraction device (see figure 2), and sealing the opening of the sample cell by using a spacer; then, a polytetrafluoroethylene pipeline with the outer diameter of 1/16mm and the inner diameter of 0.25mm is used for connecting the sample pool with the receiving phase, and two ends of the polytetrafluoroethylene pipeline are connected with needle tubes; the receiving phase is 200 μ L liner tube, and 50 μ L n-hexane is added into the receiving phase for gas-liquid micro-extraction to obtain radix Rhodiolae extract. Wherein the extraction time of gas-liquid microextraction is 5 min; the extraction temperature was 280 ℃, the receiving phase condensing temperature was-4 ℃ and the nitrogen flow rate blown into the sample cell was 2.5 mL/min.
Example 3
Drying 3Kg of rhodiola rosea, extracting for 2h by 70% ethanol hot reflux, and carrying out vacuum filtration to obtain 500g of extract. Placing 5mg of the extract in a sample cell of a micro-extraction device (see figure 2), and sealing the opening of the sample cell by using a spacer; then, a polytetrafluoroethylene pipeline with the outer diameter of 1/16mm and the inner diameter of 0.25mm is used for connecting the sample pool with the receiving phase, and two ends of the polytetrafluoroethylene pipeline are connected with needle tubes; the receiving phase is 200 μ L liner tube, and 50 μ L n-hexane is added into the receiving phase for gas-liquid micro-extraction to obtain radix Rhodiolae extract. Wherein the extraction time of gas-liquid microextraction is 5 min; the extraction temperature was 300 deg.C, the receiving phase condensing temperature was-4 deg.C, and the flow rate of nitrogen blown into the sample cell was 1.8 mL/min.
Comparative example 1
Drying 3Kg of rhodiola rosea, extracting for 2h by 70% ethanol hot reflux, and carrying out vacuum filtration to obtain 500g of extract. Placing 5mg of the extract in a sample cell of a micro-extraction device (see figure 2), and sealing the opening of the sample cell by using a spacer; then, a polytetrafluoroethylene pipeline with the outer diameter of 1/16mm and the inner diameter of 0.25mm is used for connecting the sample pool with the receiving phase, and two ends of the polytetrafluoroethylene pipeline are connected with needle tubes; the receiving phase is 200 μ L liner tube, and 50 μ L dichloromethane is added into the receiving phase for gas-liquid micro-extraction to obtain radix Rhodiolae extract. Wherein the extraction time of gas-liquid microextraction is 3 min; the extraction temperature was 200 ℃, the receiving phase condensing temperature was-4 ℃ and the flow rate of nitrogen blown into the sample cell was 1.5 mL/min.
Comparative example 2
Drying 3Kg of rhodiola rosea, extracting for 2h by 70% ethanol hot reflux, and carrying out vacuum filtration to obtain 500g of extract. Placing 5mg of the extract in a sample cell of a micro-extraction device (see figure 2), and sealing the opening of the sample cell by using a spacer; then, a polytetrafluoroethylene pipeline with the outer diameter of 1/16mm and the inner diameter of 0.25mm is used for connecting the sample pool with the receiving phase, and two ends of the polytetrafluoroethylene pipeline are connected with needle tubes; the receiving phase is 200 μ L liner tube, and 50 μ L dichloromethane is added into the receiving phase for gas-liquid micro-extraction to obtain radix Rhodiolae extract. Wherein the extraction time of gas-liquid microextraction is 5 min; the extraction temperature was 150 ℃, the receiving phase condensing temperature was-4 ℃ and the flow rate of nitrogen blown into the sample cell was 1.0 mL/min.
Example 4 active ingredient detection test
And performing gas chromatography-mass spectrometry detection on the rhodiola rosea extract to be analyzed prepared in the examples 1-3 and the comparative examples 1-2 by adopting the Nippon Shimadzu GCMS-QP2010 Ultra.
Wherein, the conditions of the gas chromatography are as follows:
the sample injection amount of the gas chromatography is 2 mu L; gas chromatography conditions: a chromatographic column: DB-5MS capillary quartz column (30m 0.25mm 0.25 u m); helium, flow rate: 1.2 mL/min; no shunt sample introduction, the sample introduction amount is 2 mu L; the temperature of the injection port is 280 ℃, the temperature programming is started from 45 ℃, the temperature is kept for 3min, the temperature is increased to 250 ℃ at the speed of 5 ℃/min, the temperature is kept for 4min, the temperature is increased to 280 ℃ at the speed of 9 ℃/min, and the temperature is kept for 14 min.
The conditions of mass spectrum in the gas chromatography-mass spectrum detection are as follows:
an ion source: electron Impact (EI); ion source temperature: 200 ℃; interface temperature: 280 ℃; ionization energy: 70 eV; the detection mode is as follows: full scan (scan, 50-600 amu).
The results are shown in FIG. 1 and Table 1.
TABLE 1 content of volatile and semi-volatile components (%)
EXAMPLE 5 preparation of cigarettes
The rhodiola rosea extracts of the embodiments 1 to 3 and the comparative examples 1 to 2 are respectively dissolved and diluted by 95 percent ethanol, the tobacco shreds are sprayed according to the mass ratio of 0.01 percent, 0.1 percent and 1 percent of the rhodiola rosea extract to the tobacco shreds, cigarettes are prepared according to a conventional process, and the tobacco shreds without the rhodiola rosea extract are prepared into cigarettes as a control sample. 5 professional smokers are invited to smoke the prepared cigarettes, the overall description result is shown in the table 2, the smoking standard is shown in the table 3, and the smoking result is shown in the table 4.
TABLE 2 review of the results of the Subtraction
TABLE 3 nine cents System Single Material Smoke test and score Standard
TABLE 4 sensory evaluation results
As shown in the figure 1 and the results in tables 1-4, the rhodiola rosea extract prepared by the method has obviously higher content of 24 common components compared with the rhodiola rosea extract prepared by the comparative examples 1-2, and the results show that the preparation method can more effectively extract the aroma substances of the rhodiola rosea. The rhodiola rosea extract prepared by the invention is used for preparing cigarettes, can effectively reduce the miscellaneous gas of tobacco and increase the fragrance harmony of the cigarettes, and has higher use value.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (6)
1. A tobacco shred comprises a rhodiola rosea extract, and the rhodiola rosea extract is prepared by the following steps:
extracting radix Rhodiolae under reflux, and vacuum filtering to obtain extract;
carrying out gas-liquid micro-extraction on the extract to obtain a rhodiola rosea extract;
the extraction system of the gas-liquid microextraction consists of inert gas with the flow rate of 1.8-2.5 mL/min and an extraction solvent;
the extraction solvent is n-hexane;
the gas-liquid micro-extraction time is 3-5 min, and the gas-liquid micro-extraction temperature is 250-300 ℃.
2. The tobacco thread according to claim 1, wherein the inert gas is selected from nitrogen, helium, argon or carbon dioxide.
3. The tobacco shred according to claim 1, wherein the solvent for the hot reflux extraction is 70-75% ethanol, and the extraction time is 2-3 h.
4. The tobacco shred according to claim 3, wherein the mass volume ratio of the rhodiola rosea to 70% ethanol is 5Kg: 4000-5000 ml.
5. The cut tobacco according to claim 1, wherein the mass fraction of the rhodiola rosea extract is 0.01-0.1%.
6. A cigarette made from the tobacco shred of any one of claims 1 to 5.
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| CN102643719A (en) * | 2012-05-09 | 2012-08-22 | 云南烟草科学研究院 | Macadimia nut flower extract and application thereof |
| CN104987952A (en) * | 2015-05-31 | 2015-10-21 | 陕西理工学院 | Method for extracting volatile oil and salidroside from rhodiola whole herb |
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| CN1246325C (en) * | 2003-03-28 | 2006-03-22 | 上海纳贝生物技术有限责任公司 | Preparation method of hongjintian effective component extract |
| CN101580525B (en) * | 2009-06-06 | 2011-06-29 | 中国科学院西北高原生物研究所 | Method for extracting salidroside, polysaccharose and tannin-type substances from rhodiola root crude drugs |
| CN101928638B (en) * | 2009-06-23 | 2013-04-17 | 湖北中烟工业有限责任公司 | Rhodiola rosea extract and application thereof as tobacco product additive |
| CN101813584B (en) * | 2010-04-23 | 2012-07-25 | 延边大学 | Gas flow type dynamic liquid phase micro-extraction method |
| US9380813B2 (en) * | 2014-02-11 | 2016-07-05 | Timothy McCullough | Drug delivery system and method |
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| CN102643719A (en) * | 2012-05-09 | 2012-08-22 | 云南烟草科学研究院 | Macadimia nut flower extract and application thereof |
| CN104987952A (en) * | 2015-05-31 | 2015-10-21 | 陕西理工学院 | Method for extracting volatile oil and salidroside from rhodiola whole herb |
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