CN105077552A - Application of eleutherococcus brachypus polysaccharide to cigarette as tobacco humectant - Google Patents
Application of eleutherococcus brachypus polysaccharide to cigarette as tobacco humectant Download PDFInfo
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- CN105077552A CN105077552A CN201510414991.2A CN201510414991A CN105077552A CN 105077552 A CN105077552 A CN 105077552A CN 201510414991 A CN201510414991 A CN 201510414991A CN 105077552 A CN105077552 A CN 105077552A
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- polysaccharide
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- eleutherococcus brachypus
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Abstract
The invention relates to a polysaccharide and an extraction and purification method thereof. The method concretely comprises the following steps: carrying out soxhlet extraction on crushed dry eleutherococcus brachypus fruits by using a diethyl ether, then extracting by using boiled water after drying residues; concentrating and centrifuging a boiling water extract solution; taking supernate to carry out alcohol precipitation and standing; centrifuging and collecting sediments; dissolving by using distilled water after washing, and then adding 0.1-0.2% of nematolyt to place in a water bath at 50+/-5 DEG C for 2-4 hours; removing protein by adopting a Sevage method, carrying out vacuum concentration after decoloring activated carbon, and carrying out water dialysis after cooling; carrying out alcohol precipitation and standing again after dialysis is ended, and drying the sediments at 60-70 DEG C to obtain crude polysaccharide for eleutherococcus brachypus. The test proves that the eleutherococcus brachypus polysaccharide has good physical and sensory embellishing effects on a cigarette, the thrill and an offensive odor of the cigarette can be reduced, the roundness and the comfort of cigarette smoke are improved, and the lycium barbarum polysaccharide can be applied to the cigarette as a tobacco humectant with excellent performance.
Description
Technical field
The invention belongs to humectant technical field, be specifically related to a kind of Eleutherococcus Brachypus polysaccharide as the application of tobacco humectant in cigarette.
Background technology
Current, mainly adopt the polyhydroxy substances such as glycerine, propane diols, sorbierite as humectant in China's cigarette industry, the main purpose of this type of humectant is used to be to maintain the moisture content of pipe tobacco in process, improve the resist processing of pipe tobacco, but above-mentioned humectant is to the maintenance of finished cigarettes moisture content with to suck the improvement effect of comfort level unsatisfactory.
Polysaccharide is polymerized by a large amount of monose, and its a large amount of hydroxyl and hydrone form hydrogen bond, can make it have stronger moisture holding capacity.At present, at home and abroad there is no the relevant report applied in cigarette as tobacco humectant by Eleutherococcus Brachypus polysaccharide.
Summary of the invention
The object of the invention is to provide a kind of Eleutherococcus Brachypus polysaccharide as the application of tobacco humectant in cigarette.
For achieving the above object, the present invention adopts following technical scheme:
A kind of method for extraction and purification of Eleutherococcus Brachypus polysaccharide, comprise the steps: after the dry Eleutherococcus Brachypus ether surname extraction pulverized (generally adding ether by solid-liquid ratio 1g:5-8ml), residue volatilizes and extracts with boiling water, extracting in boiling water liquid concentrates, centrifugal, get supernatant alcohol precipitation to leave standstill, centrifugal collecting precipitate again, dissolve with distilled water after sediment washing, the papain adding weight of precipitate 1-2 ‰ again places 2-4h in 50 ± 5 DEG C of water-baths, adopt Sevage method deproteination, reduced pressure concentration after activated carbon decolorizing, flowing water dialysis is carried out in order to remove small molecular weight impurity after cooling, after dialysis terminates, alcohol precipitation leaves standstill again, be deposited in 60-70 DEG C of dry Eleutherococcus Brachypus Thick many candies.
Further preferably, by Thick many candies chromatography purifying twice, obtain refined polysaccharide; Twice separation and purification eluent used is respectively 0.5mol/LNaCl solution and 0.05mol/LNH
4hCO
3solution.
Said extracted purification process is utilized to prepare the Eleutherococcus Brachypus polysaccharide of gained.
Said extracted purification process is utilized to prepare gained Eleutherococcus Brachypus polysaccharide as the application of tobacco humectant in cigarette.Concrete, Eleutherococcus Brachypus polysaccharide adds before baking tabacco scrap, and its addition is the 0.01-2 ‰ of pipe tobacco weight.
The present invention obtains highly purified refining Eleutherococcus Brachypus polysaccharide by extraction purification, and carried out the test of physics humid keeping performance and inherent sensory quality assessment, find that it has good physics and sense organ humectation effect to cigarette, and the excitant of cigarette and assorted gas can be reduced, improve mellow and full sense and the comfortableness of cigarette smoke, can apply in cigarette as a kind of tobacco humectant of function admirable, and determine its Optimum in cigarette.Prove through test, Eleutherococcus Brachypus polysaccharide of the present invention, to the humectation successful of tobacco product, therefore has significant industrial application value and wide popularizing application prospect.
Detailed description of the invention
The present invention is described further by the following examples, but protection scope of the present invention is not limited thereto.
test main agents used and instrument:
Ether, ethanol, acetone (Chinese Suzhou chemical reagent Co., Ltd, analyzes pure), DEAE-Celluose and SephadexG200 gel (sigma company of the U.S.), experimental water is distilled water.
BS200SWE1 type electronic balance (sensibility reciprocal: 0.0001g, Beijing match Doris balance Co., Ltd); R-215 type Rotary Evaporators (BUCHI company of Switzerland); V-700 vavuum pump (BUCHI company of Switzerland); DLSB-20/60 DEG C of sub-cooled circulating pump (Shanghai Mei Qiang instrument and equipment Co., Ltd); KDM type regulating temp. electrothermal cover (Shandong Hua Lu electric heating Instrument Ltd.); 85-2 type constant temperature blender with magnetic force (Shanghai Si Le instrument plant), ZK-82B type electric vacunm drying case (Shanghai Shen Guang instrument and meter Co., Ltd), CHRIST freeze dryer (BUCHI company of Switzerland), TSKGELG2000PW high productivity computing post (Sigma Co., USA), the efficient liquid phase instrument of AgilentLC1100 type and differential pulse polarograpll instrument (Agilent company of the U.S.).
embodiment 1
A method for extraction and purification for Eleutherococcus Brachypus polysaccharide, comprises the steps: that residue volatilizes by the 300g that pulverized dry Eleutherococcus Brachypus 1800ml ether surname extraction 2h in order to except degrease.Residue after volatilizing uses 2L extracting in boiling water 3 times again, merges the extracting in boiling water liquid of 3 gained, and concentrated, centrifugal, get supernatant, the absolute ethyl alcohol with supernatant 3 times of volumes carries out alcohol precipitation, hold over night (12h), centrifugal collecting precipitate again.Dissolve with distilled water after sediment washs 3 times with ethanol, acetone successively, then the papain adding weight of precipitate 1 ‰ places 2h in 50 DEG C of water-baths, adopt Sevage method deproteination.Add 8g active carbon to be placed in 70 DEG C of water-baths and to heat 3h, cross and filter active carbon, reduced pressure concentration, naturally load flowing water in bag filter after cooling and dialyse 48h in order to remove small molecular weight impurity, after dialysis terminates, after again adding dialysis, the absolute ethyl alcohol of polysaccharide solution volume 3 times amount carries out alcohol precipitation, hold over night (12h), be deposited in 70 DEG C of dry 11.79g Thick many candies, yield is 3.93%.
After getting the dissolving of 2.0g Thick many candies distilled water, by DEAE-Celluose gel chromatography column chromatography for separation (5.0 × 50cm), with 0.5mol/LNaCl solution for mobile phase (i.e. eluent), flow velocity is 2.5ml/min, adopt Phenol-sulphate acid method to develop the color to chromatographic solution, collect main chromatographic peak, freeze-drying.Then by freeze-drying gained solid 0.05mol/LNH
4hCO
3solubilize, by SephadexG200 gel chromatographic columns chromatography (5.0 × 50cm) again, with 0.05mol/LNH
4hCO
3solution is mobile phase (i.e. eluent), and flow velocity is 2.0ml/min, adopts Phenol-sulphate acid method to develop the color to chromatographic solution, collects main chromatographic peak, freeze-drying, obtain 486mg and refine Eleutherococcus Brachypus polysaccharide solid, yield 24.3%, and LT1 sugar content is 95.3% after testing.
embodiment 2
A method for extraction and purification for Eleutherococcus Brachypus polysaccharide, comprises the steps: that residue volatilizes by the 300g that pulverized dry Eleutherococcus Brachypus 2000ml ether surname extraction 4h in order to except degrease.Residue after volatilizing uses 2L extracting in boiling water 3 times again, merges the extracting in boiling water liquid of 3 gained, and concentrated, centrifugal, get supernatant, the absolute ethyl alcohol with supernatant 3 times of volumes carries out alcohol precipitation, leaves standstill 12h, again centrifugal collecting precipitate.Dissolve with distilled water after sediment washs 3 times with ethanol, acetone successively, then the papain adding weight of precipitate 2 ‰ places 4h in 50 DEG C of water-baths, adopt Sevage method deproteination.Add 8g active carbon to be placed in 70 DEG C of water-baths and to heat 4h, cross and filter active carbon, reduced pressure concentration, naturally load flowing water in bag filter after cooling and dialyse 48h in order to remove small molecular weight impurity, after dialysis terminates, after again adding dialysis, the absolute ethyl alcohol of polysaccharide solution volume 3 times amount carries out alcohol precipitation, hold over night, be deposited in 70 DEG C of dry 12.66g Thick many candies, yield is 4.22%.
After getting the dissolving of 2.0g Thick many candies distilled water, by DEAE-Celluose gel chromatography column chromatography for separation (5.0 × 50cm), with 0.5mol/LNaCl solution for mobile phase (i.e. eluent), flow velocity is 2.5ml/min, adopt Phenol-sulphate acid method to develop the color to chromatographic solution, collect main chromatographic peak, freeze-drying.Then by freeze-drying gained solid 0.05mol/LNH
4hCO
3solubilize, by SephadexG200 gel chromatographic columns chromatography (5.0 × 50cm) again, with 0.05mol/LNH
4hCO
3solution is mobile phase (i.e. eluent), and flow velocity is 2.0ml/min, adopts Phenol-sulphate acid method to develop the color to chromatographic solution, collects main chromatographic peak, freeze-drying, obtain 476mg and refine Eleutherococcus Brachypus polysaccharide solid, yield 23.8%, and LT1 sugar content is 96.3% after testing.
application test: Eleutherococcus Brachypus polysaccharide is as the application study of tobacco humectant
1, physics humid keeping performance test
For investigating Eleutherococcus Brachypus polysaccharide to the physics humid keeping performance of cigarette, with Bright Yellow (Jin Mantang) blank cigarette shreds for carrier, prepared by embodiment 1 gained refine the same glycerine of Eleutherococcus Brachypus polysaccharide, propane diols carry out respectively together with sorbierite physics humid keeping performance contrast test research, respectively prepare mass fraction be 5% the above-claimed cpd aqueous solution.First by 1500g mix blank cigarette shreds is placed in temperature 22 ± 1 DEG C, relative humidity 60 ± 2% environment balances 48h.Then equivalent takes five parts of pipe tobaccos, every part of 100g, and evenly apply the 4g above-claimed cpd aqueous solution respectively in pipe tobacco, contrasting blank sample is that pipe tobacco evenly applies 4g water.Then five parts of pipe tobaccos are placed in respectively 22 ± 1 DEG C, investigate it under the environment of relative humidity 40 ± 2% and separate wet process, and the change of instant moisture content is analyzed, investigate its physics humectation effect, the results are shown in Table 1.
Table 1 physics humectation Contrast on effect table
Result of the test shows, the pipe tobacco of interpolation Eleutherococcus Brachypus polysaccharide, glycerine, propane diols and sorbierite four kinds of compounds is compared with blank pipe tobacco, moisture loss speed is slower, this is that hydrophilic radical hydroxyl contained by polyol can form hydrogen bond with water and be fettered by water, delay scattering and disappearing of moisture, improve the physics humid keeping performance of pipe tobacco; Wherein the physics humid keeping performance of Eleutherococcus Brachypus polysaccharide is best, is secondly propane diols and glycerine, is finally sorbierite.
2, sense organ humid keeping performance test
Make solvent with 20v% ethanol water, gained prepared by embodiment 1 and refine Eleutherococcus Brachypus polysaccharide and be made into the solution that mass fraction is 1%.Get the above-mentioned solution containing Eleutherococcus Brachypus polysaccharide of 0.100g, 0.500g, 1.000g, 5.000g, 10.000g, 15.000g and 20.000g respectively, then evenly spray is added in seven parts of blank cigarette shreds of not spiced 100g Bright Yellow respectively, roll, respectively pick out 100 same weight cigarette, be placed in temperature 22 DEG C ± 1 DEG C, the climatic chamber of humidity 60% ± 2% balances 48h, smoke panel test.Control sample is the blank cigarette of Bright Yellow, and control sample balances 48h equally under identical temperature, damp condition.Smoking result is in table 2.
As can be seen from the smoking result of table 2, the Main Function of Eleutherococcus Brachypus polysaccharide to cigarette shows as and makes flue gas obviously become mellow and full, soft, and comfortable taste promotes, and assorted gas and excitant reduce.When Eleutherococcus Brachypus polysaccharide consumption is less, it is not clearly to the effect of cigarette; When its consumption reaches 2.0 ‰, there is the phenomenon of spine sense increase, concentration reduction; When its consumption is 1.5 ‰, sucking quality is best.Therefore, best results when adding 0.15g Eleutherococcus Brachypus polysaccharide in 100g cigarette, namely optimum consumption is 1.5 ‰.
The Eleutherococcus Brachypus polysaccharide smoking result of table 2 Different adding amount
Claims (2)
1. Eleutherococcus Brachypus polysaccharide is as the application of tobacco humectant in cigarette.
2. Eleutherococcus Brachypus polysaccharide, as the application of tobacco humectant in cigarette, is characterized in that as claimed in claim 1: Eleutherococcus Brachypus polysaccharide adds before baking tabacco scrap, and its addition is the 0.01-2 ‰ of pipe tobacco weight.
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|---|---|---|---|
| CN201510414991.2A CN105077552B (en) | 2015-07-15 | 2015-07-15 | Acanthopanax brachypus polysaccharide is as tobacco humectant application in Medicated cigarette |
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| CN201510414991.2A CN105077552B (en) | 2015-07-15 | 2015-07-15 | Acanthopanax brachypus polysaccharide is as tobacco humectant application in Medicated cigarette |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110269273A (en) * | 2019-06-28 | 2019-09-24 | 云南中烟工业有限责任公司 | A kind of preparation method and application of the tobacco humectant based on super-pressure induction |
| CN110283660A (en) * | 2019-06-28 | 2019-09-27 | 云南中烟工业有限责任公司 | A kind of preparation method and application of microwave-assisted tobacco humectant |
| CN110301669A (en) * | 2019-06-28 | 2019-10-08 | 云南中烟工业有限责任公司 | A kind of preparation method and application of ultrasonically-modified tobacco humectant |
-
2015
- 2015-07-15 CN CN201510414991.2A patent/CN105077552B/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110269273A (en) * | 2019-06-28 | 2019-09-24 | 云南中烟工业有限责任公司 | A kind of preparation method and application of the tobacco humectant based on super-pressure induction |
| CN110283660A (en) * | 2019-06-28 | 2019-09-27 | 云南中烟工业有限责任公司 | A kind of preparation method and application of microwave-assisted tobacco humectant |
| CN110301669A (en) * | 2019-06-28 | 2019-10-08 | 云南中烟工业有限责任公司 | A kind of preparation method and application of ultrasonically-modified tobacco humectant |
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Address after: 450000 Yulin South Road, Henan, Zheng Dong, No. 16 South Road, Zhengzhou Patentee after: China Tobacco Henan Industrial Co., Ltd. Address before: 450000 Zhengzhou agricultural road, Henan, No. 29 Patentee before: China Tobacco Henan Industrial Co., Ltd. |