CN102389162A - Method for preparing cornus officinalis extract, application in cigarettes and cigarette - Google Patents
Method for preparing cornus officinalis extract, application in cigarettes and cigarette Download PDFInfo
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- CN102389162A CN102389162A CN2011102225909A CN201110222590A CN102389162A CN 102389162 A CN102389162 A CN 102389162A CN 2011102225909 A CN2011102225909 A CN 2011102225909A CN 201110222590 A CN201110222590 A CN 201110222590A CN 102389162 A CN102389162 A CN 102389162A
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Abstract
The invention discloses a method for preparing cornus officinalis extract, an application in cigarettes and the cigarette. The method for preparing the cornus officinalis extract comprises the following steps: preparing the cornus officinalis; using the ultrasonic wave to extract collaborated with microwaves; extracting the liquid and concentrating; centrifuging and separating; separating by column chromatography; and concentrating to obtain the cornus officinalis extract. The cornus officinalis extract prepared by the invention is applied to the cigarettes, the use is convenient, the quality and level of the cigarette are improved, the smoke is rich and sweet, and the palate aftertaste is improved. The method combines the advantages of the ultrasonic wave with the homogenization of the microwave vibration, so the stress of each point in the sample medium is the same, the range of the target extract is large, the combination force of the target object and the sample substrate is reduced, the process that the target object enters the liquid from the solid phase is accelerated, and the sample process quantity is large. The cornus officinalis extract is obtained after extracting and refining by column chromatography with gentle conditions, which provides a new perfume material for natural tobaccos.
Description
Technical field
The present invention relates to plant extract and application thereof, the cigarette that particularly relates to a kind of preparation method of cornel extractive and the application in cigarette thereof and comprise this cornel extractive.
Background technology
Fructus Corni is the drying and ripening pulp that Cornaceae plant Fructus Corni (Comus officinalis Sieb.Ct Zucc.) removes removal core, has another name called another name for Sichuan Province jujube, medicine jujube, dogwood fruit, fructus corni, meat jujube etc." book on Chinese herbal medicine is newly organized " record: sour-puckery flavor, gas is flat, tepor, and is nontoxic.Go into kidney, liver two warps.Classify middle article as, have tonifying the liver and kidney, restrain, be used for diseases such as dizzy tinnitus, liver cold of insufficiency type heat with puckery effect." each edition of Chinese pharmacopoeia all recorded.
Modern medicine analysis and research proof: Fructus Corni mainly contains compositions such as volatile ingredient, iridoid are sweet, organic acid, tannin, and wherein volatile ingredient has comprised 9 kinds of monoterpene, 6 kinds of sesquiterpenes, 7 kinds of monoterpene alcohol, 6 kinds of fatty alcohols, 4 kinds of monoterpene aldehyde and ketone, 3 kinds of fatty aldehydes and alcohol, 4 kinds of organic acids, 8 kinds of Esters and l5 kind aromatic.Have antibiotic, regulate functions such as immune, hypoglycemic, reducing blood lipid, anti-oxidant, anticancer, anti-AIDS, cardiac stimulant, the medical value height has been listed among the big list of national health food dietotherapeutic at present.
In recent years, for the extracts active ingredients in the Fructus Corni, new and high technologies such as enzymolysis and extraction, Extraction by Ultrasound, Microwave Extraction have appearred at present; The result shows that microwave, the ultrasonic enzyme process that involves can both obviously shorten extraction time, improves effective component yield; Extraction effect is superior to conventional reflux extraction; But microwave method is not suitable for heat-sensitive substance to be extracted, and Extraction by Ultrasound receives the ultrasonic attenuation factor easily, forms the ultrasonic air white area.Simultaneously refining for the active ingredient in the Fructus Corni is main with water extract-alcohol precipitation mainly in the traditional handicraft, but this method length consuming time, uses quantity of solvent big, and the cornel extractive active constituent content that obtains is low.How extraction process being improved, with the cornel extractive content of effective that raising obtains, is the direction that people make great efforts.On the other hand, present stage, because the pharmacological action of Fructus Corni, the application study of domestic relevant Fructus Corni mainly concentrates on the medicines and health protection field, and is less in the application of other field, and relevant report is not seen in the application in cigarette.
Summary of the invention
Technical problem to be solved by this invention is: the deficiency that remedies above-mentioned prior art; A kind of preparation method of cornel extractive and application in cigarette and cigarette are proposed; Can improve content of effective in the cornel extractive that obtains by a relatively large margin; The cornel extractive that obtains is applied in the cigarette preparation, can greatly improves the interior quality of cigarette.
Technical problem of the present invention solves through following technical scheme:
A kind of preparation method of cornel extractive may further comprise the steps:
1) ultrasonic-microwave is collaborative extracts: be that the ethanolic solution of 50 wt %～80 wt % of 6～12 times of Asiatic Cornelian Cherry Fruit and the said Asiatic Cornelian Cherry Fruit quality of 150～420 μ m drops in the lump in the ultrasonic-microwave synergic solvent extraction equipment cavity and extracts with the granularity of drying; Cool off after extracting completion, use 150～200 purpose screen filtration extracts to obtain filtrating, said filtrating is concentrated, get concentrate;
2) centrifugation: with water-soluble separate of said concentrate, centrifugalize, obtain supernatant with 2～3 times of said concentrate quality;
3) column chromatography is separated: with said supernatant through chromatographic column, earlier with the 10wt%～30 wt % ethanol or the water elution impurity of 2～6 times of column volumes, again with the 50 wt %～70 wt % ethanol elutions of 2～6 times of column volumes and collect eluent;
4) concentrate: the eluent that obtains in the step 3) is concentrated, and the thick solution that obtains after concentrating is cornel extractive.
Preferably, condition was when ultrasonic-microwave described in the said step 1) was worked in coordination with extraction: ultrasonic power is 40～350W, and microwave power is 10～500W, and extracting temperature is 40～80 ℃, and extraction time is 15min～40min.
Preferably, said step 2) in during centrifugation centrifugation rate be 2000～8000rpm, the time is 10～30min.
Preferably; Filler in the said step 3) in the chromatographic column is polyamide or macroporous absorbent resin, and consumption is 1～5 times of said supernatant quality, the blade diameter length ratio 1:4～1:10 of said filler; The absorption flow velocity is 0.5～4.0BV/h, and elution flow rate is 0.5～4.0BV/h; The granularity of said polyamide is 60～80 orders, and the type of said macroporous absorbent resin is AB-8, DM-301, DM-130, a kind of among the DS-401.
Preferably, adopt decompression to concentrate in the said step 1), relative density was 1.12～1.16 when said filtrating was concentrated into 25 ℃; Adopt decompression to concentrate in the said step 4), relative density was 1.20～1.40 when said eluent was concentrated into 25 ℃.Through concentrating of step 1), the concentrate that obtains has been removed most of solvent, but still has bigger flowability, is convenient to step 2) in water can better dissolve; Decompression through step 4) concentrates control; The extract product that obtains can reach certain viscosity; And still has certain fluidity; Generally need not add anticorrisive agent under this state in the extract product and just can preserve the long period, promptly make the cornel extractive after concentrating that better stability is arranged.
A kind of cornel extractive adopts above-mentioned any described method to prepare.
A kind of application of cornel extractive in cigarette that obtains according to the above-mentioned any described method of claim is sprayed on the independent wiring solution-forming of said cornel extractive or allocate in the conventional tobacco spice in the tobacco with perfuming or reinforced mode.
Preferably, said cornel extractive is diluted with the nontoxic organic solvent that has no irritating odor, extension rate be 10-15 doubly, be sprayed in the tobacco by the 0.1%-1% of tobacco quality.
Preferably, said organic solvent is a kind of in propane diols, sorbierite, xylitol and the glycerine, perhaps two or more mixed liquor arbitrarily wherein.
A kind of cigarette is added with in the said cigarette according to above-mentioned any cornel extractive that described method obtains.
The beneficial effect of the present invention and prior art contrast is: ultrasonic wave and Microwave Extraction are organically combined; Make full use of the high energy effect of cavitation effect of ultrasonic waves and microwave, under the low-temperature atmosphere-pressure condition, carry out the collaborative Fructus Corni that extracts of ultrasonic-microwave, make that the active ingredient in the Fructus Corni can be extracted comparatively fully; Before separating, centrifugation step is set through column chromatography; Make extract have higher clarity and stability, can avoid when upper prop, stopping up filler, reduce the situation of chromatography efficient; Adopt column chromatography to separate simultaneously, utilize the specific adsorption effect of filler resin, through gradient elution, alternative is removed and is most ofly influenced the macromolecular substances such as tannin of tobacco flavoring effect in the back extended meeting, guarantees content of effective in the cornel extractive; The method for distilling of Fructus Corni of the present invention except that making water and ethanol, does not add any harmful chemical reagent and carries out assisted extraction, and is free from environmental pollution, extraction process is simple, the operating time is short, makes in the whole process of production efficiently, is suitable for industrializing implementation.On the other hand, the resulting cornel extractive of preparation method of the present invention is applied in the cigarette, easy to use, the quality and the class sense that can improve cigarette smoke, make flue gas abundant, sweet, improve the mouthfeel pleasant impression.
The specific embodiment
Below in conjunction with the specific embodiment the present invention is explained further details.
In one embodiment; The preparation method of cornel extractive may further comprise the steps: 1) ultrasonic-microwave is collaborative extracts: be that the ethanolic solution of 50 wt %～80 wt % of 6～12 times of Asiatic Cornelian Cherry Fruit and the said Asiatic Cornelian Cherry Fruit quality of 150～420 μ m drops in the lump in the ultrasonic-microwave synergic solvent extraction equipment cavity and extracts with the granularity of drying; Cool off after extracting completion, use 150～200 purpose screen filtration extracts to obtain filtrating, said filtrating is concentrated, get concentrate; 2) centrifugation: with water-soluble separate of said concentrate, centrifugalize, obtain supernatant with 2～3 times of said concentrate quality; 3) column chromatography is separated: with said supernatant through chromatographic column, earlier with the 10wt%～30 wt % ethanol or the water elution impurity of 2～6 times of column volumes, again with the 50 wt %～70 wt % ethanol elutions of 2～6 times of column volumes and collect eluent; 4) concentrate: the eluent that obtains in the step 3) is concentrated, and the thick solution that obtains after concentrating is cornel extractive.
In further embodiments, can adopt in the following optimum condition one or more:
Condition was when ultrasonic-microwave was worked in coordination with extraction in the step 1): ultrasonic power is 40～350W, and microwave power is 10～500W, and extracting temperature is 40～80 ℃, and extraction time is 15min～40min.
Centrifugation rate is 2000～8000rpm when centrifugalizing step 2), and the time is 10～30min.
Filler in the step 3) in the chromatographic column is polyamide or macroporous absorbent resin, and consumption is 1～5 times of said supernatant quality, the blade diameter length ratio 1:4～1:10 of said filler, and the absorption flow velocity is 0.5～4.0BV/h, elution flow rate is 0.5～4.0BV/h; The granularity of said polyamide is 60～80 orders, and the type of said macroporous absorbent resin is AB-8, DM-301, DM-130, a kind of among the DS-401.
Adopt decompression to concentrate in the step 1), relative density was 1.12～1.16 when said filtrating was concentrated into 25 ℃;
Adopt decompression to concentrate in the step 4), relative density was 1.20～1.40 when said eluent was concentrated into 25 ℃.
The processing of raw material: Fructus Corni raw material to be extracted is dried under 40～70 ℃ of conditions, and be crushed to the meal that granularity is 150～420 μ m.With raw material pulverizing is meal, makes Fructus Corni that higher recovery rate arranged in subsequent extracted.
Below through preferred embodiment the present invention is elaborated.
Embodiment 1
Accurately take by weighing the 200g Fructus Corni,, and be crushed to the meal that granularity is 250 μ m 45 ℃ of oven dry; Adding 1.6kg concentration is the ethanolic solution of 70 %, ultrasonic-microwave synergic solvent extraction 15min, ultrasonic power 50W; Microwave power 300W, 55 ℃ of constant temperature, extract filters through 200 eye mesh screens; Relative density is 1.12 when being evaporated to 25 ℃, gets concentrate; With the water-soluble concentrate of separating of 2 times of concentrate quality, be centrifugation 20min under the 4000rpm at centrifugation rate, get supernatant; Supernatant dynamically adsorbs through polyamide, and the absorption separation of flow is 1BV/h, after application of sample is accomplished; Earlier with 20% ethanol elution impurity of 5 times of column volumes, use 70% ethanol elution of 4 times of column volumes again, the eluent that collection obtains with the ethanol elution of 70wt%; Wherein the consumption of polyamide is 1.5 times of supernatant quality; Granularity is 60～80 orders, and the blade diameter length ratio of filler is 1:8, and elution flow rate is 1BV/h; Relative density was 1.25 when the eluent process was evaporated to 25 ℃, was the cornel extractive I.
Embodiment 2
Accurately take by weighing the 200g Fructus Corni,, and be crushed to the meal that granularity is 420 μ m 50 ℃ of oven dry; Adding 1.2kg concentration is 50% ethanolic solution, ultrasonic-microwave synergic solvent extraction 25min, ultrasonic power 50W; Microwave power 250W, 60 ℃ of constant temperature, extract filters through 200 eye mesh screens; Relative density is 1.15 when being evaporated to 25 ℃, gets concentrate; With the water-soluble concentrate of separating of 2 times of concentrate quality, be centrifugation 10min under the 6000rpm at centrifugation rate, get supernatant; Supernatant dynamically adsorbs through the AB-8 macroporous absorbent resin, and the absorption flow velocity is 0.5BV/h, after last appearance is accomplished; Elder generation is with 20% ethanol elution impurity of 5 times of column volumes; Use 80% ethanol elution of 4 times of column volumes again, collect eluent, wherein the consumption of AB-8 macroporous absorbent resin is 2 times of supernatant; The blade diameter length ratio of filler is 1:4, and elution flow rate is 0.5BV/h; Relative density was 1.31 when the eluent process was evaporated to 25 ℃, was the cornel extractive II.
Embodiment 3
Accurately take by weighing the 200g Fructus Corni,, and be crushed to the meal that granularity is 250 μ m 65 ℃ of oven dry; Add 1.2 kg concentration and be 75% ethanolic solution, ultrasonic-microwave synergic solvent extraction 30min, ultrasonic power 50W; Microwave power 400W, 60 ℃ of constant temperature, extract filters through 200 eye mesh screens; Relative density is 1.12 when being evaporated to 25 ℃, gets concentrate; With the water-soluble concentrate of separating of 2 times of concentrate quality, be centrifugation 15min under the 5000rpm at centrifugation rate, obtain supernatant; Supernatant dynamically adsorbs through the DM-130 macroporous absorbent resin, and the absorption flow velocity is 2.5BV/h BV/h, after last appearance is accomplished; With the water elution impurity of 5 times of column volumes, use 60% ethanol elution of 5 times of column volumes more earlier, collect eluent; Wherein the consumption of DM-130 macroporous absorbent resin is 3 times of total extract; Granularity is 60～80 orders, and the blade diameter length ratio of filler is 1:10, and elution flow rate is 2.5BV/h; Relative density was 1.33 when the eluent process was evaporated to 25 ℃, was the cornel extractive III.
Embodiment 4
A kind of cornel extractive adopts the method for above-mentioned any embodiment to prepare.
Embodiment 5
The application of a kind of cornel extractive in cigarette, the independent wiring solution-forming of cornel extractive that the method that adopts above-mentioned any embodiment is prepared or allocate in the conventional tobacco spice is sprayed in the tobacco with perfuming or reinforced mode.
Cornel extractive is diluted with the nontoxic organic solvent that has no irritating odor, and extension rate is 10-15 times, wherein; Organic solvent can be propane diols, sorbierite, xylitol or glycerine; Perhaps wherein any mixed liquor more than 2 kinds before the preparation cigarette, is sprayed at the cured tobacco leaf surface with the cornel extractive dilution by the 0.1%-1% of tobacco quality; Cigarette process by routine is handled; Promptly after spraying the dilution of cornel extractive,, process cigarette finished product through chopping, baking silk, perfuming, storage silk, cigarette and packaging process again with flue-cured tobacco tobacco storage 4 hours.
Embodiment 6
Experimental test: the cornel extractive I that makes in the foregoing description 1,2 and 3, II, III all are diluted to 10 times with 50% propylene glycol solution; Be sprayed at then with a kind of blank (not flavoring and casing) flue-cured tobacco pipe tobacco surface, addition is respectively 0.1%, 0.2%, 0.5%, 1.0% of pipe tobacco weight.Be control samples with the flue-cured tobacco pipe tobacco that does not spray cornel extractive simultaneously; Subsequent treatment is undertaken by the cigarette process of routine; Promptly after spraying the dilution of cornel extractive,, process cigarette finished product through chopping, baking silk, perfuming, storage silk, cigarette and packaging process again with flue-cured tobacco tobacco storage 4 hours; The group of smokeing panel test that is made up of 8 people is respectively to the contrast of smokeing panel test of above-mentioned sample, result such as following table:
Can know that from last table the tobacco leaf flue gas that adds the proper ratio cornel extractive is abundant, the raising of sweet property, pleasant impression improves, and the quality of exhaust gas volumn, sweet property and mouthfeel three aspects all is improved, and has totally given the fresh and sweet style of cigarette.
Above content is to combine concrete preferred implementation to the further explain that the present invention did, and can not assert that practical implementation of the present invention is confined to these explanations.For the those of ordinary skill of technical field under the present invention, make some substituting or obvious modification under the prerequisite of the present invention design not breaking away from, and performance or purposes are identical, all should be regarded as belonging to protection scope of the present invention.
Claims (10)
1. the preparation method of a cornel extractive is characterized in that: may further comprise the steps:
1) ultrasonic-microwave is collaborative extracts: be that the ethanolic solution of 50 wt %～80 wt % of 6～12 times of Asiatic Cornelian Cherry Fruit and the said Asiatic Cornelian Cherry Fruit quality of 150～420 μ m drops in the lump in the ultrasonic-microwave synergic solvent extraction equipment cavity and extracts with the granularity of drying; Cool off after extracting completion, use 150～200 purpose screen filtration extracts to obtain filtrating, said filtrating is concentrated, get concentrate;
2) centrifugation: with water-soluble separate of said concentrate, centrifugalize, obtain supernatant with 2～3 times of said concentrate quality;
3) column chromatography is separated: with said supernatant through chromatographic column, earlier with the 10wt%～30 wt % ethanol or the water elution impurity of 2～6 times of column volumes, again with the 50 wt %～70 wt % ethanol elutions of 2～6 times of column volumes and collect eluent;
4) concentrate: the eluent that obtains in the step 3) is concentrated, and the thick solution that obtains after concentrating is cornel extractive.
2. the preparation method of cornel extractive according to claim 1; It is characterized in that: condition was when ultrasonic-microwave described in the said step 1) was worked in coordination with extraction: ultrasonic power is 40～350W; Microwave power is 10～500W; Extracting temperature is 40～80 ℃, and extraction time is 15min～40min.
3. the preparation method of cornel extractive according to claim 1 is characterized in that: said step 2) during centrifugation centrifugation rate be 2000～8000rpm, the time is 10～30min.
4. the preparation method of cornel extractive according to claim 1; It is characterized in that: the filler in the said step 3) in the chromatographic column is polyamide or macroporous absorbent resin; Consumption is 1～5 times of said supernatant quality; Blade diameter length ratio 1:4～the 1:10 of said filler, the absorption flow velocity is 0.5～4.0BV/h, elution flow rate is 0.5～4.0BV/h; The granularity of said polyamide is 60～80 orders, and the type of said macroporous absorbent resin is AB-8, DM-301, DM-130, a kind of among the DS-401.
5. the preparation method of cornel extractive according to claim 1 is characterized in that: adopt decompression to concentrate in the said step 1), relative density was 1.12～1.16 when said filtrating was concentrated into 25 ℃; Adopt decompression to concentrate in the said step 4), relative density was 1.20～1.40 when said eluent was concentrated into 25 ℃.
6. a cornel extractive is characterized in that: adopt any described method of claim 1-5 to prepare.
7. the application of cornel extractive in cigarette that obtains according to any described method of claim 1-5 is characterized in that: the independent wiring solution-forming of said cornel extractive or allocate in the conventional tobacco spice is sprayed in the tobacco with perfuming or reinforced mode.
8. the application of cornel extractive according to claim 7 in cigarette; It is characterized in that: said cornel extractive is diluted with the nontoxic organic solvent that has no irritating odor; Extension rate be 10-15 doubly, be sprayed in the tobacco by the 0.1%-1% of tobacco quality.
9. the application of cornel extractive according to claim 8 in cigarette is characterized in that: said organic solvent is a kind of in propane diols, sorbierite, xylitol and the glycerine, perhaps two or more mixed liquor arbitrarily wherein.
10. a cigarette is characterized in that: be added with any cornel extractive that described method obtains according to claim 1-5 in the said cigarette.
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| CN102614243A (en) * | 2012-04-26 | 2012-08-01 | 西北大学 | Method for extracting common macrocarpium fruit total glycoside and application of common macrocarpium fruit total glycoside to preparation of hypoxia tolerant medicines |
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