CN105077552B - Acanthopanax brachypus polysaccharide is as tobacco humectant application in Medicated cigarette - Google Patents
Acanthopanax brachypus polysaccharide is as tobacco humectant application in Medicated cigarette Download PDFInfo
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Abstract
The present invention relates to a kind of Acanthopanax brachypus polysaccharide and method for extraction and purification thereof, particularly as follows: by after the dry Acanthopanax brachypus fruit ether surname extraction pulverized, residue volatilizes and extracts with boiling water, boiling water extraction liquid concentrates, centrifugal, take supernatant precipitate with ethanol to stand, recentrifuge collects precipitate, dissolve with distilled water after washing, the papain adding 1-2 ‰ places 2-4h in 50 ± 5 DEG C of water-baths, adopt Sevage method deproteination, concentrating under reduced pressure after activated carbon decolorizing, flowing water dialysis is carried out after cooling, dialysis terminate after again precipitate with ethanol stand, it is deposited in 60-70 DEG C and dries to obtain Acanthopanax brachypus crude polysaccharides.It has been experienced that: Medicated cigarette is had good physics and sense organ humectation effect by Acanthopanax brachypus polysaccharide of the present invention, and zest and the miscellaneous QI of Medicated cigarette can be reduced, improve mellow and full sense and the comfortableness of cigarette smoke, can apply in Medicated cigarette as the tobacco humectant of a kind of function admirable.
Description
Technical field
The invention belongs to humectant technical field, be specifically related to a kind of Acanthopanax brachypus polysaccharide as tobacco humectant application in Medicated cigarette.
Background technology
Currently, China's cigarette industry mainly adopt the polyhydroxy substances such as glycerol, propylene glycol, sorbitol as humectant, the main purpose using this type of humectant is in that to maintain the moisture content of tobacco shred in the course of processing, improve the resist processing of tobacco shred, but above-mentioned humectant to the maintenance of finished cigarettes moisture content and to suck the improvement effect of comfort level unsatisfactory.
Polysaccharide is to be polymerized by a large amount of monosaccharide, and its substantial amounts of hydroxyl forms hydrogen bond with hydrone, it is possible to make it have stronger moisture holding capacity.At present, at home and abroad there is no the relevant report applied in Medicated cigarette by Acanthopanax brachypus polysaccharide as tobacco humectant.
Summary of the invention
Present invention aim at providing a kind of Acanthopanax brachypus polysaccharide as tobacco humectant application in Medicated cigarette.
For achieving the above object, the present invention adopts the following technical scheme that
A kind of method for extraction and purification of Acanthopanax brachypus polysaccharide, comprise the steps: after the dry Acanthopanax brachypus ether surname extraction (general by solid-liquid ratio 1g:5-8ml interpolation ether) pulverized, residue volatilizes and extracts with boiling water, boiling water extraction liquid concentrates, centrifugal, take supernatant precipitate with ethanol to stand, recentrifuge collects precipitate, dissolve with distilled water after precipitate washing, the papain adding weight of precipitate 1-2 ‰ places 2-4h in 50 ± 5 DEG C of water-baths, adopt Sevage method deproteination, concentrating under reduced pressure after activated carbon decolorizing, carry out flowing water after cooling to dialyse in order to remove small molecular weight impurity, dialysis terminate after again precipitate with ethanol stand, it is deposited in 60-70 DEG C and dries to obtain Acanthopanax brachypus crude polysaccharides.
It is preferred that, by crude polysaccharides chromatography purification twice, it is thus achieved that refined polysaccharide；Separate eluent respectively 0.5mol/LNaCl solution and 0.05mol/LNH used by purification twice4HCO3Solution.
Said extracted purification process is utilized to prepare the Acanthopanax brachypus polysaccharide of gained.
Said extracted purification process is utilized to prepare gained Acanthopanax brachypus polysaccharide as tobacco humectant application in Medicated cigarette.Concrete, Acanthopanax brachypus polysaccharide adds before baking tabacco scrap, and its addition is the 0.01-2 ‰ of tobacco shred weight.
The present invention obtains highly purified refining Acanthopanax brachypus polysaccharide by extraction purification, and carried out the test of physics humid keeping performance and inherent sensory quality assessment, find that Medicated cigarette is had good physics and sense organ humectation effect by it, and zest and the miscellaneous QI of Medicated cigarette can be reduced, improve mellow and full sense and the comfortableness of cigarette smoke, can apply in Medicated cigarette as the tobacco humectant of a kind of function admirable, and determine its Optimum in Medicated cigarette.Tests prove that, Acanthopanax brachypus polysaccharide of the present invention is obvious to the humectation effect 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 to this.
Test main agents used and instrument:
Ether, ethanol, acetone (Suzhou chemical reagent company limited of China, analytical 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 company limited)；R-215 type Rotary Evaporators (BUCHI company of Switzerland)；V-700 vacuum pump (BUCHI company of Switzerland)；DLSB-20/60 DEG C of sub-cooled circulating pump (Shanghai Mei Qiang instrument and equipment company limited)；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 company limited), 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
The method for extraction and purification of a kind of Acanthopanax brachypus polysaccharide, comprises the steps: dry for the 300g pulverized Acanthopanax brachypus 1800ml ether surname extraction 2h in order to remove oils and fats, residue volatilizes.Residue after volatilizing uses 2L boiling water extraction 3 times again, merges the boiling water extraction liquid of 3 gained, concentrates, is centrifuged, takes supernatant, and the dehydrated alcohol adding 3 times of volumes of supernatant carries out precipitate with ethanol, stands overnight (12h), recentrifuge collection precipitate.Precipitate dissolves with distilled water with after ethanol, washing with acetone 3 times successively, and the papain adding weight of precipitate 1 ‰ places 2h, employing Sevage method deproteination in 50 DEG C of water-baths.Add 8g activated carbon to be placed in 70 DEG C of water-baths and heat 3h, it is filtered to remove activated carbon, concentrating under reduced pressure, load flowing water in bag filter after natural cooling and dialyse 48h in order to remove small molecular weight impurity, after dialysis terminates, after again adding dialysis, the dehydrated alcohol of polysaccharide solution volume 3 times amount carries out precipitate with ethanol, stands overnight (12h), being deposited in 70 DEG C and dry to obtain 11.79g crude polysaccharides, yield is 3.93%.
After taking the dissolving of 2.0g crude polysaccharides distilled water, with 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 that chromatographic solution is developed the color, collect main chromatographic peak, lyophilizing.Then by lyophilizing gained solid 0.05mol/LNH4HCO3Solution dissolves, with SephadexG200 gel chromatographic columns chromatography again (5.0 × 50cm), with 0.05mol/LNH4HCO3Solution is mobile phase (i.e. eluent), and flow velocity is 2.0ml/min, adopts Phenol-sulphate acid method that chromatographic solution is developed the color, collects main chromatographic peak, lyophilizing, obtains the refining Acanthopanax brachypus polysaccharide solid of 486mg, and yield 24.3%, LT1 sugar content is 95.3% after testing.
Embodiment 2
The method for extraction and purification of a kind of Acanthopanax brachypus polysaccharide, comprises the steps: dry for the 300g pulverized Acanthopanax brachypus 2000ml ether surname extraction 4h in order to remove oils and fats, residue volatilizes.Residue after volatilizing uses 2L boiling water extraction 3 times again, merges the boiling water extraction liquid of 3 gained, concentrates, is centrifuged, takes supernatant, and the dehydrated alcohol adding 3 times of volumes of supernatant carries out precipitate with ethanol, stands 12h, recentrifuge collection precipitate.Precipitate dissolves with distilled water with after ethanol, washing with acetone 3 times successively, and the papain adding weight of precipitate 2 ‰ places 4h, employing Sevage method deproteination in 50 DEG C of water-baths.Add 8g activated carbon to be placed in 70 DEG C of water-baths and heat 4h, it is filtered to remove activated carbon, concentrating under reduced pressure, load flowing water in bag filter after natural cooling and dialyse 48h in order to remove small molecular weight impurity, after dialysis terminates, after again adding dialysis, the dehydrated alcohol of polysaccharide solution volume 3 times amount carries out precipitate with ethanol, stands overnight, being deposited in 70 DEG C and dry to obtain 12.66g crude polysaccharides, yield is 4.22%.
After taking the dissolving of 2.0g crude polysaccharides distilled water, with 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 that chromatographic solution is developed the color, collect main chromatographic peak, lyophilizing.Then by lyophilizing gained solid 0.05mol/LNH4HCO3Solution dissolves, with SephadexG200 gel chromatographic columns chromatography again (5.0 × 50cm), with 0.05mol/LNH4HCO3Solution is mobile phase (i.e. eluent), and flow velocity is 2.0ml/min, adopts Phenol-sulphate acid method that chromatographic solution is developed the color, collects main chromatographic peak, lyophilizing, obtains the refining Acanthopanax brachypus polysaccharide solid of 476mg, and yield 23.8%, LT1 sugar content is 96.3% after testing.
Application test: Acanthopanax brachypus polysaccharide is as the applied research of tobacco humectant
1, physics humid keeping performance test
For investigating the Acanthopanax brachypus polysaccharide physics humid keeping performance to Medicated cigarette, with the blank cigarette shreds of Bright Yellow (Jin Mantang) for carrier, embodiment 1 being prepared the gained refining same glycerol of Acanthopanax brachypus polysaccharide, propylene glycol and carries out the research of physics humid keeping performance contrast test together with sorbitol respectively, preparation mass fraction is the above-claimed cpd aqueous solution of 5% respectively.First the blank cigarette shreds that 1500g mixes is placed in temperature 22 ± 1 DEG C, relative humidity 60 ± 2% environment and balances 48h.Then equivalent weighs five parts of tobacco shreds, every part of 100g, uniformly applies 4g above-claimed cpd aqueous solution respectively in tobacco shred, and the blank sample of comparison is that tobacco shred uniformly applies 4g water.Then five parts of tobacco shreds being respectively placed in 22 ± 1 DEG C, investigates it under the environment of relative humidity 40 ± 2% and solve wet process, and the change of instant moisture content is analyzed, investigate its physics humectation effect, result is in Table 1.
Table 1 physics humectation Contrast on effect table
Result of the test shows, add Acanthopanax brachypus polysaccharide, glycerol, four kinds of compounds of propylene glycol and sorbitol tobacco shred compared with blank tobacco shred, moisture loss speed is slower, this is that the hydrophilic group 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 tobacco shred；Wherein the physics humid keeping performance of Acanthopanax brachypus polysaccharide is best, next to that propylene glycol and glycerol, be finally sorbitol.
2, sense organ humid keeping performance test
Make solvent with 20v% ethanol water, the refining Acanthopanax brachypus polysaccharide of gained is prepared by embodiment 1 and is made into the solution that mass fraction is 1%.Take 0.100g, 0.500g, 1.000g, 5.000g, the above-mentioned solution containing Acanthopanax brachypus polysaccharide of 10.000g, 15.000g and 20.000g respectively, then uniformly spray is added in seven parts of not spiced 100g Bright Yellow blank cigarette shreds respectively, roll, respectively pick out 100 same weight Medicated cigarette, it is placed in the climatic chamber of temperature 22 DEG C ± 1 DEG C, humidity 60% ± 2% and balances 48h, smoke panel test.Control sample is Bright Yellow blank Medicated cigarette, and control sample balances 48h equally under identical temperature, damp condition.Smoking result is in Table 2.
Being made flue gas substantially become mellow and full, soft by the smoking result of table 2 it can be seen that the Main Function of Medicated cigarette is shown as by Acanthopanax brachypus polysaccharide, comfortable taste promotes, and miscellaneous QI and zest reduce.When Acanthopanax brachypus polysaccharide consumption is less, the effect of Medicated cigarette is not as obvious by it；When its consumption reaches 2.0 ‰, the phenomenon that spine sense increase, concentration reduce occurs；When its consumption is 1.5 ‰, sucking quality is best.Therefore, adding best results during 0.15g Acanthopanax brachypus polysaccharide in 100g Medicated cigarette, namely optimum consumption is 1.5 ‰.
The Acanthopanax brachypus polysaccharide smoking result of table 2 Different adding amount
Claims (2)
1. Acanthopanax brachypus polysaccharide is as tobacco humectant application in Medicated cigarette, it is characterised in that described Acanthopanax brachypus polysaccharide obtains through following step extraction purification:
By after the dry Acanthopanax brachypus ether surname extraction pulverized, residue volatilizes and extracts with boiling water, boiling water extraction liquid concentrates, centrifugal, take supernatant precipitate with ethanol to stand, recentrifuge collects precipitate, dissolve with distilled water after precipitate washing, the papain adding weight of precipitate 1-2 ‰ places 2-4h in 50 ± 5 DEG C of water-baths, adopt Sevage method deproteination, concentrating under reduced pressure after activated carbon decolorizing, carry out flowing water after cooling to dialyse in order to remove small molecular weight impurity, dialysis terminate after again precipitate with ethanol stand, it is deposited in 60-70 DEG C and dries to obtain Acanthopanax brachypus crude polysaccharides；
By crude polysaccharides chromatography purification twice, it is thus achieved that refined polysaccharide；Separate eluent respectively 0.5mol/LNaCl solution and 0.05mol/LNH used by purification twice4HCO3Solution.
2. as claimed in claim 1 Acanthopanax brachypus polysaccharide as tobacco humectant application in Medicated cigarette, it is characterised in that: Acanthopanax brachypus polysaccharide adds before baking tabacco scrap, and its addition is the 0.01-2 ‰ of tobacco shred weight.
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| 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 |
| 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 |
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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. |