CN101602982A - The step-by-step extracting method of purple perilla and extract obtained application in cigarette - Google Patents
The step-by-step extracting method of purple perilla and extract obtained application in cigarette Download PDFInfo
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- CN101602982A CN101602982A CNA2008100479805A CN200810047980A CN101602982A CN 101602982 A CN101602982 A CN 101602982A CN A2008100479805 A CNA2008100479805 A CN A2008100479805A CN 200810047980 A CN200810047980 A CN 200810047980A CN 101602982 A CN101602982 A CN 101602982A
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- flue gas
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- 235000004347 Perilla Nutrition 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 20
- 244000124853 Perilla frutescens Species 0.000 title 1
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- 230000000694 effects Effects 0.000 claims abstract description 35
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Abstract
The invention discloses the step-by-step extracting method and the extract obtained application in cigarette of purple perilla, belong to technical field of cigarette flavors.The purple perilla step-by-step extracting method is: 1. soak at room temperature; 2. extraction volatile oil obtains extract A; 3. filter and obtain filtrate; 4. carry out alcohol precipitation after concentrating, get extract B; 5. cross film, concentrate, get extract C.To add after extract A, the independent or compound proportioning of B, C in the pipe tobacco, make cigarette have the peculiar fragrance of purple perilla, or have and coordinate to enrich fragrance, soft convergence flue gas, reducing stimulates, and increases the effect of aftertaste, or has antioxygenation, or have the effect that reduces the flue gas free radical, or has the comprehensive action of above effect.The present invention extracts that the raw material Perilla Leaf is easy to get and is cheap, and the purple perilla result of use is good, safe; Fragrance, pleasant impression and comfort to cigarette all have positive effect preferably.Can reduce the free radical in the cigarette again to a certain extent, play the effect of lowering harm and decreasing coking.
Description
Technical field
The invention belongs to technical field of cigarette flavors, be specifically related to a kind of step-by-step extracting method of special medicinal material purple perilla and extract obtained as the application of tobacco aromatics using in cigarette.
Background technology
Purple perilla is a Labiatae annual herb plant, has another name called Huis Soviet Union, red Soviet Union, purple Soviet Union, red Soviet Union, perillaseed etc., is the warm crop of happiness, and adaptability is strong, requires not strict to envrionment conditions and edaphic condition.The Food and Argriculture OrganizationFAO and the World Health Organization united and held nutrition code executive session the 13 time in February, 1979, content of erucic acid in the edible vegetable oil has been discussed less than 5% draft standard, the development research of for this reason not having the novel oil crops purple perilla of erucic acid has obtained paying attention to and developing rapidly.Except the conduct novel oil crops of no erucic acid, purple perilla also has other multiple utility value: contain 8 essential seed amino acids of grownup and 9 necessary seed amino acids of baby in the purple perilla, its content and kind are all surpassing Radix Dauci Sativae and red three-coloured amaranth in varying degrees; Purple perilla volatile oil can exert an influence to tumour necrosis factor, strengthens the curative effect of radiotherapy to tumour, stops cell carcinogenesis and anticancer growth; In Japan,, bright fragrant tasty and refreshing, tasteful with the fresh blade salted white of purple perilla.At present, food service industry utilizes work to become the hot topic that countries in the world are paid close attention to the research and development of purple perilla.Yet Folium perillae extract is not appeared in the newspapers so far yet as the technology that essence spice for cigarette is applied in tobacco industry.
Can produce the free radical of high density during cigarette burning, materials such as the directly or indirectly attack of these free radicals, damaging cells and enzyme combine with DNA and to make cell transformation and produce sudden change.Therefore study the flue gas free radical, the free-radical scavengers of exploitation high effect nontoxic, for reducing smoking property of cigarette harm, the contradiction of alleviating between smoking and the health has crucial meaning.At present, it is many to adopt plant additive to reduce the research of flue gas free radical, all has the effect of falling free radical as the kendir reported, tea-polyphenol, Liquiritigenin, xenthophylls etc. as cigaret additive, and its reduction amplitude is about 7%-20%.The adding technology of these plant additives all is that the form of making microcapsule joins in the filter tip complex process mostly.This mainly is because at first, most plant additives all are liposoluble, are sprayed directly in the pipe tobacco and have any problem on the technology; Secondly these plant additives add in the pipe tobacco, can change the suction flavor of cigarette, even bring very bad influence.The natural phant that can reduce free radical has a lot, can reduce the cigarette free radical simultaneously, again can to cigarette odor-absorbing bring good positive effect but seldom.Though the natural phant of having reported at present that falls the cigarette free radical is a lot, really uses it for suitability for industrialized production, brings but almost not having of direct distinct economic, its key reason is exactly to solve the negative effect of plant additive to cigarette odor-absorbing.
The applicant is by research, discovery directly is sprayed onto Folium perillae extract on the pipe tobacco, the effect that reduces the flue gas free radical is arranged, and the suction flavor of rareer is cigarette has produced good positive positive effect, and cigarette being smelt or smoke all has one unique fragrance.The more important thing is that the cigarette preproduction that has added this Folium perillae extract has carried out industrial test production, can bring foreseeable remarkable economic efficiency for enterprise.
Summary of the invention
At the above-mentioned deficiency of prior art, one of the technical problem to be solved in the present invention provides the method that a kind of purple perilla extracts step by step, and it carries out purple perilla the substep extraction and obtain three kinds of Folium perillae extract of different nature.Another technical problem that the present invention will solve is that three kinds of Folium perillae extract that will be extracted are applied in the cigarette, both made cigarette have the effect of antioxygenation and reduction flue gas free radical, can give cigarette special fragrance again, can also promote the smoking quality of cigarette simultaneously.
Technical scheme of the present invention is that the purple perilla step-by-step extracting method carries out according to the following steps:
(1) Perilla Leaf is ground into meal; In the Perilla Leaf meal, add Perilla Leaf meal weight 10-14 water doubly, soak at room temperature 14-18 hour;
(2) the purple perilla mixed liquor after will soaking carries out water vapour distillation volatile oil, extracting temperature is 110-130 ℃, time is 6-10 hour, the volatile oil that obtains is faint yellow limpid transparence, with 70% the dissolve with ethanol that accounts for 100 times of amounts of its weight, the ethanolic soln of gained volatile oil is an extract A with volatile oil;
(3) the purple perilla mixed liquor that will extract behind the volatile oil filters, and keeps filtrate; Add former purple perilla weight 8-10 distilled water doubly in the filter residue, under 110-130 ℃ temperature, carried out refluxing extraction 2-4 hour, filter, with gained filtrate with last time kept the filtrate merging;
(4) getting in the above-mentioned merging filtrate half, is 60-68 ℃ in temperature, and vacuum tightness is to be concentrated into the concentration that contains raw material purple perilla 1.0g in every ml soln under the 380-450ps i; Add concentrated solution weight 6-8 dehydrated alcohol doubly and carry out alcohol precipitation, leave standstill after-filtration half an hour, is 60-68 ℃ with filtrate in temperature, vacuum tightness is the 0.4-1% that is concentrated into original volume under the 380-450psi, obtain medicinal extract, medicinal extract is dissolved in 70% the ethanol of 100 times of weight, the ethanolic soln that obtains is an extract B;
(5) get second half of above-mentioned merging filtrate, cross the hollow-fibre membrane of one time 0.65 μ m earlier, to continue molecular weight cut-off be 3000 hollow-fibre membrane with crossing penetrating fluid behind the film, obtain penetrating fluid for the second time, penetrating fluid is 60-68 ℃ in temperature for the second time, and vacuum tightness is the 0.5-1.5% that is concentrated into original volume under the 380-450psi, obtains medicinal extract, medicinal extract is dissolved in 70% the ethanol of 100 times of weight, the gained ethanolic soln is an extract C.
The inventive method resulting three kinds of Folium perillae extract A, B, C are complicated mixtures, can't further describe its concrete composition and composition.Briefly, extract A is the ethanolic soln that volatile oil that purple perilla obtains with water extraction makes; Extract B is the filtrate after purple perilla extracts volatile oil, and alcohol precipitation returns the ethanolic soln that the medicinal extract that obtains after molten the concentrating makes; Extract C is that purple perilla extracts filtrate behind the volatile oil to cross the molecular weight that obtains behind the film be 3000 ethanolic solns with interior mixture.
Above-mentioned three kinds of purple perillas substep extract A, B, the C integrated application in cigarette: with extract A, or extract B, or extract C, or the mixture of extract A, B, C, add in the cigarette shreds with 0.01%～0.1% ratio, can make cigarette have the peculiar fragrance of purple perilla, or have and coordinate to enrich fragrance, soft convergence flue gas, reducing stimulates, and increases the effect of aftertaste, or has antioxygenation, or have the effect that reduces the flue gas free radical, or has the comprehensive action of above effect.
Purple perilla substep extract A, B, the C integrated application in cigarette: extract A is applied in the cigarette shreds separately, or when containing extract A in the extract mixing liquid, make cigarette have the peculiar fragrance of purple perilla after the adding, and have and coordinate to enrich fragrance, soft convergence flue gas, reducing stimulates, and increases the effect of aftertaste.
Purple perilla substep extract A, B, the C integrated application in cigarette: extract B is applied in the cigarette shreds separately, or is applied to when containing extract B in the extract mixing liquid in the cigarette shreds, can make cigarette have antioxygenation.
Purple perilla substep extract A, B, the C integrated application in cigarette: extract C is applied in the cigarette shreds separately, or be applied to when containing extract C in the extract mixing liquid in the cigarette shreds, can make cigarette have antioxygenation and reduce the effect of flue gas free radical.
Purple perilla step-by-step extracting method of the present invention is simple, implements easily; Perilla Leaf is easy to get and is cheap, no matter is volatile oil or filtrate, all is fully utilized, and is therefore with low cost; Purple perilla be the first batch of promulgation of the Ministry of Health be food be again one of 60 kinds of Chinese medicines of medicine, be not subjected to the restriction of dosage, pH during use, effective, safe; Apply it to cigarette flavoring or reinforced in, fragrance, pleasant impression and the comfort of cigarette all had positive effect preferably.Simultaneously, extract C can reduce the free radical in the cigarette again to a certain extent, plays the effect of lowering harm and decreasing coking.Therefore, purple perilla is low, effective, the safe novel essence spice for cigarette material of a kind of cost, has DEVELOPMENT PROSPECT preferably aspect the flavoring and casing of tobacco industry and the lowering harm and decreasing coking.
Embodiment
Below in conjunction with embodiment the relevant technologies problem is described in further detail.The applicant has carried out composition analysis to Folium perillae extract, and the result is as follows:
Extract A volatile oil, gas chromatograph-mass spectrometer with U.S. Agilent company is analyzed, and main component has α-Pai Xi (α-pinene), beta-pinene (β-pinene), phantol (linalool), VANILLYL ALCOHOL MIN 98 (citronelol), perillaldehyde (perillaldehyde), perillalcohol (perilla alcohol), β-cloves alkene (β-caryophyllene), α-humulone (α-humulene), nerolidol (morolidol), limonene (limonene) or the like.Wherein perillalcohol is a kind of the have treatment and monoterpenes compound of preventing cancer effect, and the antitumous effect characteristics of broad-spectrum, efficient, low toxicity are arranged.And other alcohols and aldehyde material are again well to cause fragrant precursor in the cigarette as nerolidol, β-cloves alkene, perillaldehyde, phantol etc., give distinctive local flavor of cigarette and fragrance, can give cigarette hot sweet gas breath as cloves alkene.The comprehensive flavor characteristic that constitutes extract A of these effective constituents.
Carrying out alcohol precipitation in the extract B and return molten experiment, is that these produce dysgenic macromolecular cpd to cigarette odor-absorbing in order to remove the pectin, protein and the polyose that contain in the solution.Extract C carried out film handle be for only keep molecular weight 3000 with interior compound.Find by composition analysis, all contain flavonoid compound among extract B and the C, have antioxygenation, remove the rosmarinic acid of free radical effect and perillalcohol with antitumous effect.
Contain flavonoid compound in the Folium perillae extract, therefore have stronger antioxygenation.The applicant adopts Sodium Nitrite-aluminum nitrate colorimetric spectrophotometry, makes standard substance with rutin, measures content of total flavone in the extract down in the wavelength of 510nm.Experiment is found, does not detect flavones in the extract A, and contains a certain amount of flavonoid compound respectively in the extract B, C, and the general flavone content in the extract B is higher than (the seeing Table 1) of extract C.Take phenanthroline system hydroxyl radical free radical to remove experiment, three kinds of extracts are carried out oxidation-resistance measure (seeing Table 2), find that extract A does not have the oxidation-resistance ability, (described external free radical is meant outside the human body but extract B and C have the external free radical of stronger removing, and the free radical that produces outside the main flume, it comprises the free radical that experiment reagent is formulated, and the free radical that produces outside other non-mainstream flue gas) ability.Simultaneously, extract B and C are sprayed onto respectively in the pipe tobacco, measure the ability that it removes the flue gas alkyl diradical.Experiment finds that extract B does not almost reduce the ability of flue gas free radical, and extract C has the effect (seeing Table 3) that reduces the flue gas alkyl diradical preferably.This shows: because cigarette needs burning in aspiration procedure, cigarette burning process and product thereof are very complicated systems, though flavonoid compound has the effect that reduces external free radical, it also not necessarily has the ability that reduces the flue gas free radical; Secondly, in Folium perillae extract, having the effective constituent that reduces flue gas free radical effect perhaps is not flavonoid compound, but some other composition, or the synergy of several compositions.At last, with a kind of natural plant extracts, because its preparation technology's difference, the residing system difference of its contained chemical ingredients and this chemical ingredients, it is in the cigarette burning process, the scission reaction that each compound takes place also varies, so the effect of the reduction flue gas free radical of this system performance is also made a world of difference.
Content of total flavone in table 1, the extract
| Extract | General flavone content (%) |
| ????A | ????0 |
| ????B | ????19.51 |
| ????C | ????11.01 |
Annotate: general flavone content (%) accounts for the percentage composition of medicinal extract (promptly not using the extract medicinal extract of alcohol dilution) quality for the quality of the total flavones of mensuration
The oxidation-resistance of table 2, extract is measured
Table 3, extract reduce the experiment of flue gas free radical
| Free radical | Blank | Extract B | Extract C |
| Content (spin/ props up) | ??30.358×10 14 | ????29.268×10 14 | ????17.9654 |
| Reduced rate (%) | ??- | ????3.59 | ????40.82 |
The applicant adopts the different fit systems of substep extract A, B, C to carry out flavoring and casing with the middle-grade blank pipe tobacco of flavoring and casing not, and to the sample cigarette contrast experiment that smokes panel test.The concrete embodiment that adds sees Table 4, and wherein the addition of extract A, B, C is a weight percentage.This interpolation embodiment just enumerates different array modes, in same embodiment, also can carry out the adjusting of addition according to concrete pipe tobacco prescription and odour characteristics.
The compound prescription embodiment of table 4 extract
| ????A(％) | ????B(％) | ????C(％) | Addition manner | |
| Embodiment 1 | ????100 | ????0 | ????0 | Perfuming |
| Embodiment 2 | ????0 | ????100 | ????0 | Reinforced |
| Embodiment 3 | ????0 | ????0 | ????100 | Reinforced |
| Embodiment 4 | ????50 | ????50 | ????0 | Perfuming |
| Embodiment 5 | ????50 | ????0 | ????50 | Perfuming |
| Embodiment 6 | ????50 | ????50 | Reinforced | |
| Embodiment 7 | ????20 | ????40 | ????40 | Perfuming |
According to the described compound prescription embodiment of table 4, with three different flavoring and casing ratios of compound prescription extract: 0.01%, 0.05%, 0.1% (weight percentage) rolls sample.The personnel that participation is smoked panel test are totally 10 people, and wherein one is national judging panel, 5 provincial judging panels, 4 level of factory judging panels.Smoking result all is with respect to the same processing mode of process, and the blank cigarette that does not only add extract is reference (concrete outcome sees Table 5,6,7).Experiment finds, substep extract and compound prescription thereof joined in the cigarette can produce different flavoring and casing effects.Because extract A is a volatile oil, so embodiment 1 effect when applied amount is 0.01% (weight percentage) is best, can effectively play and coordinate to enrich fragrance, reducing stimulates, and increases the effect of aftertaste; Embodiment 4 and 5 effect when applied amount is 0.05% (weight percentage) is best; And embodiment 2,3,6,7 effect when applied amount is 0.1% (weight percentage) is best.Compound prescription embodiment difference, the flavouring effect that plays has nothing in common with each other, and the blending personnel can be as required and products characteristics, selects different compound prescription embodiment and compound proportion to carry out flavoring and casing.But, generally speaking, add the cigarette product behind the Folium perillae extract, no matter smell or smoke, all have consistent unique perfume.
Table 5,0.01% applied amount smoking result
| Embodiment | Smell perfume (or spice) | Odour characteristics | The flue gas feature | Inhale the flavor feature |
| ??1 | Fragrant and sweet strong | Perfume quantity increases, and enriches plentifully, and outer perfuming obviously and coordinate | Concentration increases, the soft exquisiteness of flue gas, and conglobation property is good | Sweet sense well, pungency reduces, pleasant impression is clean, aftertaste increases |
| ??2 | A little less than in the acid perfume (or spice) | Perfume quantity has increase slightly | Flue gas changes little | The sense of promoting the production of body fluid slightly increases |
| ??3 | ??- | Aroma change is little | The soft fine and smooth degree of flue gas has increase slightly | Change little |
| ??4 | Fragrant and sweet strong | Fragrance enriches plentiful, and concentration is big | Flue gas concentration increases, and conglobation property is good, exquisiteness | Sweet sense increases, and pungency reduces, and Tianjin sense slightly increases |
| ??5 | Fragrant and sweet strong | Perfume quantity increases, and outer perfuming is obviously coordinated | Flue gas concentration increases, and conglobation property is good, exquisiteness | Sweet sense increases, and pungency reduces, and pleasant impression is clean, aftertaste |
| Increase | ||||
| ??6 | ??- | Aroma change is little | Concentration has increase slightly | Change little |
| ??7 | A little less than the acid perfume (or spice) | Perfume quantity increases, and fragrance is coordinated | Flue gas concentration increases, soft exquisiteness | Stimulation reduces, and is residual less, slightly aftertaste |
Table 6,0.05% applied amount smoking result
| Embodiment | Smell perfume (or spice) | Odour characteristics | The flue gas feature | Inhale the flavor feature |
| ??1 | Fragrant and sweet strong | Perfume quantity increases, the obvious and coordination of outer perfuming | Concentration increases, and strength increases | Sweet sense increases, and stimulation reduces, but pleasant impression is not very clean |
| ??2 | In the acid perfume (or spice) | Perfume quantity increases, and outer perfuming is obvious | Flue gas strength increases, and flue gas looses | Excitement reduces, and the sense of promoting the production of body fluid increases, and pleasant impression changes little |
| ??3 | In the cream perfume (or spice) | Perfume quantity has increase slightly | Flue gas concentration increases, soft exquisiteness | Excitement reduces, the residual reduction in oral cavity |
| ??4 | Acid fragrant by | Perfume quantity increases, and outer perfuming is obvious | Concentration increases, and strength increases, and agglomerating sense well | Stimulate and reduce, Tianjin sense increases, and is slightly residual |
| ??5 | A little less than in fragrant and sweet | Perfume quantity increases, and fragrance matter is enriched plentiful, and outer perfuming is obviously coordinated | Concentration increases, and fine and smooth sense strengthens, and agglomerating sense well | Sweet sense stimulates for a short time well, and Tianjin is felt, and aftertaste increases, and is slightly residual |
| ??6 | Acid fragrant by | Perfume quantity increases | Concentration increases, and strength increases, and flue gas looses | Stimulation reduces, and pleasant impression improves |
| ??7 | A little less than in the acid perfume (or spice) | Perfume quantity increases, and fragrance is coordinated | Concentration increases, and agglomerating sense strengthens | Stimulation reduces, have residual, slightly aftertaste |
Table 7,0.1% applied amount smoking result
| Embodiment | Smell perfume (or spice) | Odour characteristics | The flue gas feature | Inhale the flavor feature |
| ??1 | Fragrant and sweet | Perfume quantity increases, outer perfuming | Concentration increases, and strength increases | Sweet sense increases, and thorn increases sharply |
| By force | Inharmonious | Greatly, but fine and smooth degree variation | Greatly, residual heavier | |
| 2 | Acid is fragrant strong | Fragrance is plentiful abundant | Flue gas concentration, strength are big, and flue gas looses | Excitement reduces, residual increase |
| 3 | Strong in the cream perfume (or spice) | Perfume quantity increases, and outer perfuming is obvious | Concentration increases, and conglobation property is good, soft exquisiteness | Excitement reduces, and the sense of promoting the production of body fluid increases, and the oral cavity has residual slightly, increases aftertaste |
| 4 | Strong in the acid perfume (or spice) | Perfume quantity increases, and outer perfuming is inharmonious | Concentration increases, and strength increases, and agglomerating sense well | Stimulate and reduce, Tianjin sense increases, and is residual heavy |
| 5 | Fragrant and sweet strong | Perfume quantity increases, and outer perfuming is inharmonious | Concentration increases, and fine and smooth sense strengthens, and agglomerating sense well | Sweet sense stimulates for a short time well, and Tianjin is felt, and pleasant impression is poor |
| 6 | Strong in the acid perfume (or spice) | Perfume quantity increases, and fragrance matter is enriched plentiful | Concentration increases, soft exquisiteness, and agglomerating sense is well | Stimulation reduces, and aftertaste is arranged |
| 7 | In the acid perfume (or spice) | Perfume quantity increases, and outer perfuming is coordinated | Concentration increases, agglomerating sense well, strength increases | Sweet sense strengthens, and stimulation reduces, residual reduction.The aftertaste sense strengthens |
Below be that three kinds of purple perilla substep extracts extract embodiment.
Embodiment 1
(1) Perilla Leaf is ground into meal, in the Perilla Leaf meal, adds distilled water (Perilla Leaf: water=1: 12, weight ratio), soak at room temperature 16 hours.
(2) mixed liquor after will soaking carries out water vapour distillation volatile oil, and extracting temperature is 120 ℃, and the time is 6 hours, obtains faint yellow limpid transparent oily matter, and it is dissolved in 70% the ethanol of 100 times of weight, obtains extract A.
(3) the purple perilla mixed liquor that will extract behind the volatile oil filters, and obtains filtrate.Add the distilled water of 10 times of crude drug weight in the filter residue, under 120 ℃ temperature, carried out refluxing extraction 3 hours, filter, merge filtrate twice.
(4) getting half weight filtrate is 65 ℃ in temperature, and vacuum tightness is to be concentrated into the solution that is equivalent to crude drug 1.0g/ml under the 400psi.The dehydrated alcohol that adds weight in the solution and be 8 times carries out alcohol precipitation, leaves standstill after-filtration half an hour.Is 65 ℃ with filtrate in temperature, and vacuum tightness is the 0.4-1% that is concentrated into original volume under the 400psi, obtains medicinal extract, and it is dissolved in 70% the ethanol of 100 times of weight, obtains extract B.
(5) filtrate of second half weight is crossed the hollow-fibre membrane of one time 0.65 μ m earlier.To continue molecular weight cut-off be 3000 hollow-fibre membrane with crossing penetrating fluid behind the film, obtain penetrating fluid for the second time, penetrating fluid is 65 ℃ in temperature for the second time, vacuum tightness is the 0.5-1.5% that is concentrated into original volume under the 400psi, obtain medicinal extract, it is dissolved in 70% the ethanol of 100 times of weight, obtains extract C.
Embodiment 2
(1) Perilla Leaf is ground into meal, in the Perilla Leaf meal, adds distilled water (Perilla Leaf: water=1: 10, weight ratio), soak at room temperature 18 hours.
(2) mixed liquor after will soaking carries out water vapour distillation volatile oil, and extracting temperature is 120 ℃, and the time is 8 hours, obtains faint yellow limpid transparent oily matter, and it is dissolved in 70% the ethanol of 100 times of weight, obtains extract A.
(3) the purple perilla mixed liquor that will extract behind the volatile oil filters, and obtains filtrate.Add the distilled water of 8 times of crude drug weight in the filter residue, under 120 ℃ temperature, carried out refluxing extraction 3 hours, filter, merge filtrate twice.
(4) getting half weight filtrate is 65 ℃ in temperature, and vacuum tightness is to be concentrated into the solution that is equivalent to crude drug 1.0g/ml under the 420psi.The dehydrated alcohol that adds weight in the solution and be 8 times carries out alcohol precipitation, leaves standstill after-filtration half an hour.Is 65 ℃ with filtrate in temperature, and vacuum tightness is the 0.4-1% that is concentrated into original volume under the 420psi, obtains medicinal extract, and it is dissolved in 70% the ethanol of 100 times of weight, obtains extract B.
(5) filtrate of (4) being got half remaining weight of back is crossed the hollow-fibre membrane of one time 0.65 μ m earlier.To continue molecular weight cut-off be 3000 hollow-fibre membrane with crossing penetrating fluid behind the film, obtain penetrating fluid for the second time, penetrating fluid is 65 ℃ in temperature for the second time, vacuum tightness is the 0.5-1.5% that is concentrated into original volume under the 420psi, obtain medicinal extract, it is dissolved in 70% the ethanol of 100 times of weight, obtains extract C.
Embodiment 3
(1) Perilla Leaf is ground into meal, in the Perilla Leaf meal, adds distilled water (Perilla Leaf: water=1: 12, weight ratio), soak at room temperature 18 hours.
(2) mixed liquor after will soaking carries out water vapour distillation volatile oil, and extracting temperature is 120 ℃, and the time is 10 hours, obtains faint yellow limpid transparent oily matter, and it is dissolved in 70% the ethanol of 100 times of weight, obtains extract A.
(3) the purple perilla mixed liquor that will extract behind the volatile oil filters, and obtains filtrate.Add the distilled water of 10 times of crude drug weight in the filter residue, under 120 ℃ temperature, carried out refluxing extraction 3 hours, filter, merge filtrate twice.
(4) getting half weight filtrate is 68 ℃ in temperature, and vacuum tightness is to be concentrated into the solution that is equivalent to crude drug 1.0g/ml under the 450psi.The dehydrated alcohol that adds weight in the solution and be 8 times carries out alcohol precipitation, leaves standstill after-filtration half an hour.Is 68 ℃ with filtrate in temperature, and vacuum tightness is the 0.4-1% that is concentrated into original volume under the 450psi, obtains medicinal extract, and it is dissolved in 70% the ethanol of 100 times of weight, obtains extract B.
(5) filtrate of (4) being got half remaining weight of back is crossed the hollow-fibre membrane of one time 0.65 μ m earlier.To continue molecular weight cut-off be 3000 hollow-fibre membrane with crossing penetrating fluid behind the film, obtain penetrating fluid for the second time, penetrating fluid is 68 ℃ in temperature for the second time, vacuum tightness is the 0.5-1.5% that is concentrated into original volume under the 450psi, obtain medicinal extract, it is dissolved in 70% the ethanol of 100 times of weight, obtains extract C.
Claims (5)
1, the step-by-step extracting method of purple perilla is characterized in that the step-by-step extracting method of purple perilla carries out according to the following steps:
(1) Perilla Leaf is ground into meal; In the Perilla Leaf meal, add Perilla Leaf meal weight 10-14 water doubly, soak at room temperature 14-18 hour;
(2) the purple perilla mixed liquor after will soaking carries out water vapour distillation volatile oil, extracting temperature is 110-130 ℃, time is 6-10 hour, the volatile oil that obtains is faint yellow limpid transparence, with 70% the dissolve with ethanol that accounts for 100 times of amounts of its weight, the ethanolic soln of gained volatile oil is an extract A with volatile oil;
(3) the purple perilla mixed liquor that will extract behind the volatile oil filters, and keeps filtrate; Add former purple perilla weight 8-10 distilled water doubly in the filter residue, under 110-130 ℃ temperature, carried out refluxing extraction 2-4 hour, filter, with gained filtrate with last time kept the filtrate merging;
(4) getting in the above-mentioned merging filtrate half, is 60-68 ℃ in temperature, and vacuum tightness is to be concentrated into the concentration that contains raw material purple perilla 1.0g in every ml soln under the 380-450psi; Add concentrated solution weight 6-8 dehydrated alcohol doubly and carry out alcohol precipitation, leave standstill after-filtration half an hour, is 60-68 ℃ with filtrate in temperature, vacuum tightness is the 0.4-1% that is concentrated into original volume under the 380-450psi, obtain medicinal extract, medicinal extract is dissolved in 70% the ethanol of 100 times of weight, the ethanolic soln that obtains is an extract B;
(5) get second half of above-mentioned merging filtrate, cross the hollow-fibre membrane of one time 0.65 μ m earlier, to continue molecular weight cut-off be 3000 hollow-fibre membrane with crossing penetrating fluid behind the film, obtain penetrating fluid for the second time, penetrating fluid is 60-68 ℃ in temperature for the second time, and vacuum tightness is the 0.5-1.5% that is concentrated into original volume under the 380-450psi, obtains medicinal extract, medicinal extract is dissolved in 70% the ethanol of 100 times of weight, the gained ethanolic soln is an extract C.
2, the application of the resulting extract of the step-by-step extracting method of purple perilla as claimed in claim 1 in cigarette, it is characterized in that: with extract A, or extract B, or extract C, or the mixture of extract A, B, C, ratio with 0.01%～0.1% adds in the cigarette shreds, can make cigarette have the peculiar fragrance of purple perilla, or have and coordinate to enrich fragrance, soft convergence flue gas, reducing stimulates, increase the effect of aftertaste, or have antioxygenation, or have the effect that reduces the flue gas free radical, or have the comprehensive action of above effect.
3, the application of the resulting extract of the step-by-step extracting method of purple perilla according to claim 2 in cigarette, it is characterized in that: extract A is applied in the cigarette shreds separately, or when containing extract A in the extract mixing liquid, make cigarette have the peculiar fragrance of purple perilla after the adding, and have and coordinate to enrich fragrance, soft convergence flue gas, reducing stimulates, and increases the effect of aftertaste.
4, the application of the resulting extract of the step-by-step extracting method of purple perilla according to claim 2 in cigarette, it is characterized in that: extract B is applied in the cigarette shreds separately, or be applied to when containing extract B in the extract mixing liquid in the cigarette shreds, can make cigarette have antioxygenation.
5, the application of the resulting extract of the step-by-step extracting method of purple perilla according to claim 2 in cigarette, it is characterized in that: extract C is applied in the cigarette shreds separately, or be applied to when containing extract C in the extract mixing liquid in the cigarette shreds, can make cigarette have antioxygenation and reduce the effect of flue gas free radical.
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| CN115232673A (en) * | 2022-07-06 | 2022-10-25 | 玉溪农业职业技术学院(云南省玉溪烟草栽培学校) | Aromatic perilla extract composition with antibacterial function and preparation method thereof |
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