CN102715650B - Application of Dendrobium officinale polysaccharide to cigarette - Google Patents
Application of Dendrobium officinale polysaccharide to cigarette Download PDFInfo
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- CN102715650B CN102715650B CN201210209018.3A CN201210209018A CN102715650B CN 102715650 B CN102715650 B CN 102715650B CN 201210209018 A CN201210209018 A CN 201210209018A CN 102715650 B CN102715650 B CN 102715650B
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- dendrobium candidum
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Abstract
The invention discloses application of Dendrobium officinale polysaccharide to cigarettes. The amount of used Dendrobium officinale polysaccharide is 0.002-0.02 percent of weight of cut tobacco in the cigarettes. The preparation method of the Dendrobium officinale polysaccharide comprises the steps of: cleaning and drying Dendrobium officinale, crushing the dried Dendrobium officinale, extracting in water to obtain extract, cooling the extract, conducting centrifugal separation and vacuum suction filtration and vacuum-concentrating filtrate to obtain concentrated solution; and conducting ethanol precipitation to the concentrated solution, collecting sediment and freeze-drying the sediment to obtain the Dendrobium officinale polysaccharide. After the Dendrobium officinale polysaccharide is applied to the cigarettes, when the cigarettes are smoked, the smoke is mellow and full, the fineness and the softness are increased, the dry sensation is reduced and the quantity of aroma is increased.
Description
Technical field
The present invention relates to preparation and the application of plant polyose, be specifically related to the application of a kind of Dendrobium officinale polysaccharide in cigarette.
Background technology
Perfuming cigarette humectation technology always is the key point of outstanding tobacco product characteristic chicken flavor and personalized style, wherein humid keeping performance is the key factor that affects cigarette flavor, fragrance and suck comfort level, is important foundation and the guarantee of constructing Chinese-style cigarette core technology.At present domesticly mainly by adding the materials such as propane diols, glycerine, as humectant, improve the humid keeping performance of cigarette, but moistening effect is obvious not enough, still has the problems such as moisture loss is fast, flue gas moisture is on the low side, excitant is bigger than normal.China, as Zhejiang Province's Special plant aboundresources, containing a lot of active components, is applicable to the active components of plants of cigarette and extracts if find, and the performance being expected to cigarette is improved.
Dendrobium candidum Dendroblum officinale is seed plant, the orchid family, and stone Mongolian oak belongs to.Perennial nearly beautiful matter draft, 3~June of florescence.According to Chinese Plants will, produce Eastern Part of Zhejiang Province, China Yinxian County, balcony, fairy house, but do not see its sample according to zhejiang plants will, only explain copper sheet stone solution.Wild being difficult to gathers.All there is cultivation existing balcony, Yiwu, Linan, Hangzhou, various places, Wenzhou.Should pass through to gather the plant of nearly natural bionic cultivation.In 9~October, gather herb, clean and airing.All herbal medicine, tool tonifying-Yin and nourishing-stomach, antipyretic effect of promoting the production of body fluid.Main function chemical composition has alkaloid, polysaccharide, amino acid, luxuriant and rich with fragrance compounds compound etc.
Polysaccharide is the high molecular polymer being formed by connecting by glycosidic bond by 10 above monose, contains a large amount of hydroxyl isopolarity groups in its molecule, can slow down the lost speed of moisture by forming hydrogen bond with hydrone, thereby show certain moisture retention.At present some polysaccharide has been applied to tobacco business, has played good humectation effect, and as the application of disclosed a kind of cactus polyoses in cigarette in Chinese patent ZL200910172520.X etc., and the application of Dendrobium officinale polysaccharide in cigarette have not been reported.
The existing report about Dendrobium officinale polysaccharide and preparation thereof is also less, be mainly the preparation method of disclosed a kind of Dendrobium officinale polysaccharide in Chinese patent ZL200910101997.9, take dendrobium candidum as raw material, adopt water and microwave method to extract, extract is concentrated by alcohol precipitation and centrifugal, obtain the thick polysaccharide precipitation of dendrobium candidum, through macroporous resin purification, bag filter dialysis, remove albumen and the dry Dendrobium officinale polysaccharide that obtains of spraying again, wherein, during macroporous resin purification, take distilled water as eluent, and elution flow rate is 0.5-1.0ml/min; The recovery rate of the method Dendrobium officinale polysaccharide is higher.This Dendrobium officinale polysaccharide is for the preparation of dendrobium candidum polysaccharide buccal tablet.
The preparation method of disclosed a kind of dendrobium candidum polysaccharide extractive in Chinese patent ZL200610145677.X, comprise step: (1) degreasing: dendrobium candidum meal is refluxed with organic solvent, obtain the dregs of a decoction, (2) extract: boiling obtains decoction liquor, (3) concentrated: to obtain concentrate, (4) alcohol precipitation, (5) are dry, obtain the dendrobium candidum polysaccharide extractive that polyoses content is not less than 25% (weight); This dendrobium candidum polysaccharide extractive can be used for preparing the medicine of the disease that auxiliary curing hypoimmunity causes.
Summary of the invention
The invention provides the application of a kind of Dendrobium officinale polysaccharide in cigarette, Dendrobium officinale polysaccharide is applied in cigarette, can significantly improve fine and smooth soften and the perfume quantity of cigarette, improve flue gas form and dry sensation.
The application of Dendrobium officinale polysaccharide in cigarette, does not need to change the original processing technology of cigarette during application.
The consumption of described Dendrobium officinale polysaccharide is preferably 0.02 ‰-0.2 ‰ of cigarette shreds quality, can under the prerequisite economizing in raw materials, farthest improve saturation degree and the dry sensation of cigarette.
The application process of described Dendrobium officinale polysaccharide in cigarette, comprise: by described Dendrobium officinale polysaccharide through water-soluble solution, the solution spray that is mixed with 0.08mg/ml-0.8mg/ml is added on cigarette shreds, obtain the pipe tobacco containing Dendrobium officinale polysaccharide, adopt existing cigarette preparation method as after the operations such as mixed silk, balance, cigarette, with the pipe tobacco containing Dendrobium officinale polysaccharide, prepare cigarette.
The preparation method of described Dendrobium officinale polysaccharide, comprises the following steps:
A. dry after dendrobium candidum being cleaned, through pulverizing, obtain dendrobium candidum powder;
B. dendrobium candidum powder is extracted in water, obtain extract, wherein, the weight ratio of dendrobium candidum powder and water is 1: 20-50;
C. extract is cooling obtains filtrate by centrifugal and vacuum filtration, and filtrate Vacuum Concentration, to a thirtieth to 1/10th of extracting liquid volume, obtains concentrate;
D. to adding volume fraction in concentrate, be the ethanol of 95%-100%, make volume fraction of ethanol in system reach 75%-90%, stir, standing 8h-12h, centrifugal, collecting precipitation, obtains the thick polysaccharide of dendrobium candidum after freeze drying.
Described dendrobium candidum preferably adopts dendrobium candidum stem.
In step a, dry mode is varied, can naturally dry also and can pass through oven for drying, from saving time and avoiding destroying active component two aspects, considers, and dry temperature is preferably 30 ℃-50 ℃.
For the effect that further guarantees to extract, preferably:
The order number of described dendrobium candidum powder is 20 order-100 orders.
In step b, the condition of described extraction is: 70 ℃-100 ℃ are extracted 2h-4h; Or, adopting ultrasonic wave assisted extraction, ultrasonic power is 400w-500w, time 30min-50min.
Described volume fraction is that the ethanol of 95%-100% can adopt commercially available prod.
Compared with prior art, tool of the present invention has the following advantages:
The preparation method of Dendrobium officinale polysaccharide of the present invention, adopt dry, pulverizings → lixiviate → centrifugal, filter → concentrated → alcohol precipitation → freeze-drying → thick polysaccharide, simple to operate, be easy to control and cost low, pollution-free, processing technology without changing existing cigarette, is suitable for suitability for industrialized production.
Dendrobium officinale polysaccharide of the present invention may be used in cigarette, adds the cigarette of Dendrobium officinale polysaccharide of the present invention, and while burning and sucking cigarette, flue gas form is mellow and full, and fine and smooth soften has increase, and dry sensation declines, and perfume quantity increases.The shortcoming of having improved to a certain extent China's cigarette product humectation deficiency, has actual production meaning and value.
The specific embodiment
The present invention is described further below in conjunction with embodiment.
Embodiment 1
A, put into ovendry power at 45 ℃, baking oven after dendrobium candidum stem is cleaned and be broken to 40 orders, obtain dendrobium candidum powder;
B, dendrobium candidum powder is added as to water refluxing extraction 3h at 100 ℃ of 25 times of weight of dendrobium candidum powder, obtain extract;
C, extract are cooling by obtaining filtrate after 10000r/min high speed centrifugation and vacuum filtration, and filtrate Vacuum Concentration, to 1/15 of extracting liquid volume, obtains concentrate;
D, to adding volume fraction in concentrate, be 95% ethanol, make the volume fraction of ethanol in system reach 85%, stir, standing 10h, the centrifugal 20min of 4000r/min, collecting precipitation, obtains Dendrobium officinale polysaccharide after freeze drying.
According to 0.1 ‰ of tobacco quality, take Dendrobium officinale polysaccharide, the spray solution that is made into 0.4mg/ml with pure water, to rolling cigarette cigarette on pipe tobacco, carries out sensory evaluating smoking after constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) balance 48h; Sensory evaluating smoking's result is: with the Cigarette comparison of not adding Dendrobium officinale polysaccharide, flue gas form is mellow and full, and fine and smooth soften has increase, and dry sensation declines, and perfume quantity increases.
Embodiment 2
A, put into after dendrobium candidum stem is cleaned at 30 ℃, baking oven and dry, the sample of getting after oven dry is crushed to 20 orders, obtains dendrobium candidum powder;
B, the water that dendrobium candidum powder is added as to 20 times of weight of dendrobium candidum powder extract 2h at 90 ℃, obtain extract;
C, extract is cooled to room temperature, 8000r/min high speed centrifugation 15min, supernatant is after vacuum filtration, and filtrate Vacuum Concentration, to 1/30 of extracting liquid volume, obtains concentrate;
D, in concentrate, add absolute alcohol (being that volume fraction is 100% ethanol), constantly stir, make volume fraction of ethanol in system reach 90%, standing 8h, the centrifugal 15min of 4000r/min, collecting precipitation, obtains the thick polysaccharide of dendrobium candidum after freeze drying.
By 0.02 ‰ of tobacco quality, take the thick polysaccharide of dendrobium candidum of gained, after water-soluble solution, be mixed with the spray solution of 0.08mg/ml to pipe tobacco, roll into after Cigarette and carry out sensory evaluating smoking after constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) balance 48h; Sensory evaluating smoking's result is: with the Cigarette comparison of not adding Dendrobium officinale polysaccharide, flue gas form is mellow and full, and fine and smooth soften has increase, and dry sensation declines, and perfume quantity increases.
Embodiment 3
A, put into ovendry power at 50 ℃, baking oven after dendrobium candidum stem is cleaned and be broken to 100 orders, obtain dendrobium candidum powder;
B, the water that dendrobium candidum powder is added as to 50 times of weight of dendrobium candidum powder extract 4h at 70 ℃, obtain extract;
C, extract are cooling by obtaining filtrate after 10000r/min high speed centrifugation and vacuum filtration, and filtrate Vacuum Concentration, to 1/10 of extracting liquid volume, obtains concentrate;
D, to adding volume fraction in concentrate, be 98% ethanol, make the volume fraction of ethanol in system reach 75%, stir, standing 12h, the centrifugal 15min of 4000r/min, collecting precipitation, obtains Dendrobium officinale polysaccharide after freeze drying.
According to 0.2 ‰ of tobacco quality, take Dendrobium officinale polysaccharide, the spray solution that is made into 0.8mg/ml with pure water rolls into Cigarette to pipe tobacco, after constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) balance 48h, carries out sensory evaluating smoking; Sensory evaluating smoking's result is: with the Cigarette comparison of not adding Dendrobium officinale polysaccharide, flue gas form is mellow and full, and fine and smooth soften has increase, and dry sensation declines, and perfume quantity increases.
Embodiment 4
A, put into ovendry power at 35 ℃, baking oven after dendrobium candidum stem is cleaned and be broken to 60 orders, obtain dendrobium candidum powder;
B, dendrobium candidum powder is added as to water refluxing extraction 3h at 80 ℃ of 40 times of weight of dendrobium candidum powder, obtain extract;
C, extract are cooling by obtaining filtrate after 10000r/min high speed centrifugation and vacuum filtration, and filtrate Vacuum Concentration, to 1/20 of extracting liquid volume, obtains concentrate;
D, to adding volume fraction in concentrate, be 96% ethanol, make the volume fraction of ethanol in system reach 88%, stir, standing 10h, the centrifugal 20min of 4000r/min, collecting precipitation, obtains Dendrobium officinale polysaccharide after freeze drying.
According to 0.08 ‰ of tobacco quality, take Dendrobium officinale polysaccharide, the spray solution that is made into 0.15mg/ml with pure water, to rolling cigarette cigarette on pipe tobacco, carries out sensory evaluating smoking after constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) balance 48h; Sensory evaluating smoking's result is: with the Cigarette comparison of not adding Dendrobium officinale polysaccharide, flue gas form is mellow and full, and fine and smooth soften has increase, and dry sensation declines, and perfume quantity increases.
Embodiment 5
A, put into after dendrobium candidum stem is cleaned at 45 ℃, baking oven and dry, the sample of getting after oven dry is crushed to 80 orders, obtains dendrobium candidum powder;
B, dendrobium candidum powder is added as to the distilled water of 30 times of weight of dendrobium candidum powder, put into ultrasonic extractor, ultrasonic power 480w, ultrasonic extraction 35min, obtains extract;
C, extract is cooled to room temperature, 10000r/min high speed centrifugation 10min, supernatant is after vacuum filtration, and filtrate Vacuum Concentration, to 1/20 of extracting liquid volume, obtains concentrate;
D, in concentrate, add absolute alcohol (being that volume fraction is 100% ethanol), constantly stir, make volume fraction of ethanol in system reach 90%, standing 8h, the centrifugal 15min of 4000r/min, collecting precipitation, obtains Dendrobium officinale polysaccharide after freeze drying.
By 0.2 ‰ of tobacco quality, take the Dendrobium officinale polysaccharide of gained, after water-soluble solution, be mixed with the spray solution of 0.8mg/ml to pipe tobacco, roll into after Cigarette and carry out sensory evaluating smoking after constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) balance 48h; Sensory evaluating smoking's result is: with the Cigarette comparison of not adding Dendrobium officinale polysaccharide, flue gas form is mellow and full, and fine and smooth soften has increase, and dry sensation declines, and perfume quantity increases.
Embodiment 6
A, put into after dendrobium candidum stem is cleaned at 50 ℃, baking oven and dry, the sample of getting after oven dry is crushed to 60 orders, obtains dendrobium candidum powder;
B, dendrobium candidum powder is added as to the distilled water of 35 times of weight of dendrobium candidum powder, put into ultrasonic extractor, ultrasonic power 400w, ultrasonic extraction 50min, obtains extract;
C, extract is cooled to room temperature, 10000r/min high speed centrifugation 10min, supernatant is after vacuum filtration, and filtrate Vacuum Concentration, to 1/10 of extracting liquid volume, obtains concentrate;
D, to adding volume fraction in concentrate, be 95% ethanol, constantly stir, make volume fraction of ethanol in system reach 85%, standing 8h, the centrifugal 15min of 4000r/min, collecting precipitation, obtains Dendrobium officinale polysaccharide after freeze drying.
By 0.02 ‰ of tobacco quality, take the Dendrobium officinale polysaccharide of gained, after water-soluble solution, be mixed with the spray solution of 0.08mg/ml to pipe tobacco, roll into after Cigarette and carry out sensory evaluating smoking after constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) balance 48h; Sensory evaluating smoking's result is: with the Cigarette comparison of not adding Dendrobium officinale polysaccharide, flue gas form is mellow and full, and fine and smooth soften has increase, and dry sensation declines, and perfume quantity increases.
Embodiment 7
A, put into after dendrobium candidum stem is cleaned at 30 ℃, baking oven and dry, the sample of getting after oven dry is crushed to 100 orders, obtains dendrobium candidum powder;
B, dendrobium candidum powder is added as to the distilled water of 20 times of weight of dendrobium candidum powder, put into ultrasonic extractor, ultrasonic power 500w, ultrasonic extraction 30min, obtains extract;
C, extract is cooled to room temperature, 10000r/min high speed centrifugation 10min, supernatant is after vacuum filtration, and filtrate Vacuum Concentration, to 1/30 of extracting liquid volume, obtains concentrate;
D, to adding volume fraction in concentrate, be 97% ethanol, constantly stir, make volume fraction of ethanol in system reach 75%, standing 12h, the centrifugal 15min of 4000r/min, collecting precipitation, obtains Dendrobium officinale polysaccharide after freeze drying.
By 0.12 ‰ of tobacco quality, take the Dendrobium officinale polysaccharide of gained, after water-soluble solution, be mixed with the spray solution of 0.4mg/ml to pipe tobacco, roll into after Cigarette and carry out sensory evaluating smoking after constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) balance 48h; Sensory evaluating smoking's result is: with the Cigarette comparison of not adding Dendrobium officinale polysaccharide, flue gas form is mellow and full, and fine and smooth soften has increase, and dry sensation declines, and perfume quantity increases.
Embodiment 8
A, put into after dendrobium candidum stem is cleaned at 35 ℃, baking oven and dry, the sample of getting after oven dry is crushed to 80 orders, obtains dendrobium candidum powder;
B, dendrobium candidum powder is added as to the distilled water of 50 times of weight of dendrobium candidum powder, put into ultrasonic extractor, ultrasonic power 500w, ultrasonic extraction 50min, obtains extract;
C, extract is cooled to room temperature, 10000r/min high speed centrifugation 10min, supernatant is after vacuum filtration, and filtrate Vacuum Concentration, to 1/25 of extracting liquid volume, obtains concentrate;
D, to adding volume fraction in concentrate, be 98% ethanol, constantly stir, make volume fraction of ethanol in system reach 80%, standing 12h, the centrifugal 15min of 4000r/min, collecting precipitation, obtains Dendrobium officinale polysaccharide after freeze drying.
By 0.08 ‰ of tobacco quality, take the Dendrobium officinale polysaccharide of gained, after water-soluble solution, be mixed with the spray solution of 0.6mg/ml to pipe tobacco, roll into after Cigarette and carry out sensory evaluating smoking after constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) balance 48h; Sensory evaluating smoking's result is: with the Cigarette comparison of not adding Dendrobium officinale polysaccharide, flue gas form is mellow and full, and fine and smooth soften has increase, and dry sensation declines, and perfume quantity increases.
The requirement of smokeing panel test: the smokeing panel test of each sample needs seven and the above persons to participate in, two judging panels of cigarette country, five and above provincial judging panel; These qualifications all need to pass qualification examinations.
Smoke panel test with reference to State Standard of the People's Republic of China (GB 5606.4-2005) < < cigarette the 4th part: sense organ specification requirement > > (Cigarettes-Part 4:Technical requirements for sense-evaluation), 2005-6-17 issue, 2006-1-1 implement, and by General Administration of Quality Supervision, Inspection and Quarantine o of the People's Republic of China and Standardization Administration of China, are issued.
Claims (1)
1. the application of Dendrobium officinale polysaccharide in cigarette, is characterized in that, the consumption of described Dendrobium officinale polysaccharide be in cigarette tobacco quality 0.02 ‰-0.2 ‰;
The preparation method of described Dendrobium officinale polysaccharide, comprises the following steps:
A. dry after dendrobium candidum being cleaned, through pulverizing, obtain dendrobium candidum powder;
Described dendrobium candidum is dendrobium candidum stem;
Dry temperature is 30 ℃-50 ℃;
The order number of described dendrobium candidum powder is 20 order-100 orders;
B. dendrobium candidum powder is extracted in water, obtain extract, wherein, the weight ratio of dendrobium candidum powder and water is 1:20-50;
The condition of described extraction is: 70 ℃-100 ℃ are extracted 2h-4h, adopt ultrasonic wave assisted extraction, and ultrasonic power is 400w-500w, time 30min-50min;
C. extract is cooling obtains filtrate by centrifugal and vacuum filtration, and filtrate Vacuum Concentration, to a thirtieth to 1/10th of extracting liquid volume, obtains concentrate;
D. to adding volume fraction in concentrate, be the ethanol of 95%-100%, make volume fraction of ethanol in system reach 75%-90%, stir, standing 8h-12h, centrifugal, collecting precipitation, obtains the thick polysaccharide of dendrobium candidum after freeze drying;
Described application process comprises: by described Dendrobium officinale polysaccharide, through water-soluble solution, the solution spray that is mixed with 0.08mg/ml-0.8mg/ml is added on cigarette shreds, prepares cigarette.
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CN103211298A (en) * | 2013-04-23 | 2013-07-24 | 广州中医药大学 | Application of dendrobium officinale polysaccharides in preparation of harm-reducing cigarettes |
WO2016019548A1 (en) * | 2014-08-07 | 2016-02-11 | 香港大学 | Pharmaceutical use of polysaccharide of dendrobium officinale |
CN104926956A (en) * | 2015-06-26 | 2015-09-23 | 广西健宝石斛有限责任公司 | Method of extracting Dendrobium candidum polysaccharides via ultrasonic optimization |
CN105733994B (en) * | 2016-04-18 | 2019-01-15 | 云南中烟工业有限责任公司 | A kind of trichoderma aureoviride bacterial strain and the method for preparing dendrobium candidum tobacco aromaticss with it |
CN106148007A (en) * | 2016-08-11 | 2016-11-23 | 江西中烟工业有限责任公司 | A kind of method preparing cigarette Herba Dendrobii spice for Extraction solvent with jowar wine |
CN110037335A (en) * | 2019-03-20 | 2019-07-23 | 福建绿色黄金生物科技有限公司 | A kind of processing method and its application of dendrobium candidum |
CN113308301A (en) * | 2021-06-04 | 2021-08-27 | 安徽中烟工业有限责任公司 | Dendrobium polysaccharide Amadori latent aroma spice, preparation method thereof and application thereof in cigarettes |
CN114276470A (en) * | 2021-12-28 | 2022-04-05 | 亿利耐雀生物科技有限公司 | Dendrobium polysaccharide and preparation method and application thereof |
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