CN104031165B - Grifolan, method for extraction and purification and the application as tobacco humectant thereof - Google Patents
Grifolan, method for extraction and purification and the application as tobacco humectant thereof Download PDFInfo
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- CN104031165B CN104031165B CN201410292982.6A CN201410292982A CN104031165B CN 104031165 B CN104031165 B CN 104031165B CN 201410292982 A CN201410292982 A CN 201410292982A CN 104031165 B CN104031165 B CN 104031165B
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Abstract
The present invention relates to a kind of grifolan and method for extraction and purification thereof, particularly as follows: by after the dry Grifola frondosa 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 crude polysaccharides.It has been experienced that: Medicated cigarette is had good physics and sense organ humectation effect by grifolan 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 grifolan, method for extraction and purification and the application as tobacco humectant thereof.
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 grifolan as tobacco humectant.
Summary of the invention
Present invention aim at providing a kind of grifolan, method for extraction and purification and the application as tobacco humectant thereof.
For achieving the above object, the present invention adopts the following technical scheme that
A kind of method for extraction and purification of grifolan, comprise the steps: after the dry Grifola frondosa 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 brown 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 grifolan of gained.
Said extracted purification process is utilized to prepare the application as tobacco humectant of the gained grifolan.
Grifola frondosa is food, medicine dual-purpose mushroom fungus, and between the autumn in summer, Chang Yesheng is around chesnut.Sporophore endoplasm, handle is short is overlapped into clump in coralliform branch, its outward appearance, and graceful, stacking is like chrysanthemum；Its abnormal smells from the patient, delicate fragrance overflow, refreshing；Its meat is tender and crisp tasty and refreshing, and hundred eat and do not mind；Its nutrition has good health-care effect and significantly high medical value.In recent years as a kind of high-class healthy food, it is in fashion the markets such as Japan, Singapore.The present invention obtains highly purified refining grifolan 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.
Compared to the prior art, beneficial effects of the present invention: 1) in the extraction process of grifolan, the method utilizing precipitate with ethanol, protease hydrolysis, Sevage removing protein and dialysis to combine except small molecular phase, significantly reduces the impurity in grifolan, lays the foundation for further separating purification.2) gel chromatography column chromatography for separation purification is adopted twice, it is thus achieved that highly purified refining grifolan.Whole extraction purification process operation is easy, and raw material and the reagent of use are cheap and easy to get.3) tests prove that, grifolan 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 grifolan, comprises the steps: dry for the 300g pulverized Grifola frondosa 1800ml ether surname extraction 2h in order to remove oils and fats, residue volatilizes.Residue after volatilizing uses 750ml 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 after respectively washing 3 times with 300ml ethanol, 300ml acetone successively, and the papain adding weight of precipitate 1 ‰ places 2h in 50 DEG C of water-baths, adopts Sevage method deproteination.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 14.4g crude polysaccharides, yield is 4.8%.
After taking the dissolving of 1.5g 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 grifolan solid of 365mg, and yield 24.3%, LT1 sugar content is 96% after testing.
Embodiment 2
The method for extraction and purification of a kind of grifolan, comprises the steps: dry for the 300g pulverized Grifola frondosa 2000ml ether surname extraction 4h in order to remove oils and fats, residue volatilizes.Residue after volatilizing uses 750ml 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 after respectively washing 3 times with 300ml ethanol, 300ml acetone successively, and the papain adding weight of precipitate 2 ‰ places 4h in 50 DEG C of water-baths, adopts Sevage method deproteination.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 15.6g crude polysaccharides, yield is 5.2%.
After taking the dissolving of 1.5g 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 grifolan solid of 349mg, and yield 23.3%, LT1 sugar content is 96.2% after testing.
Application test: embodiment 1 prepares the gained refining grifolan applied research as tobacco humectant
1, physics humid keeping performance test
For investigating the grifolan physics humid keeping performance to Medicated cigarette, with Bright Yellow (great Jin circle) blank cigarette shreds for carrier, same for grifolan glycerol, propylene glycol carry out respectively the research of physics humid keeping performance contrast test together with sorbitol, and preparation mass fraction is the above-claimed cpd aqueous solution of 5% respectively.First the blank cigarette shreds that 1000g 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 are respectively placed in 22 ± 1 DEG C, investigate it under the environment of relative humidity 40 ± 2% and solve wet process, and the change of instant moisture content is analyzed, investigating its physics humectation effect (after namely adding different sample, the moisture content of drying base in tobacco shred 72h changes), result is in Table 1.
The physics humectation Contrast on effect of table 1, grifolan, glycerol, propylene glycol and sorbitol
The result of the test of table 1 shows: add grifolan, 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 grifolan 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, grifolan is made into the solution that mass fraction is 1%.Take 0.100g, 0.500g, 1.000g, the above-mentioned solution containing grifolan of 5.000g, 10.000g and 20.000g respectively, then uniformly spray is added in five 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.
The grifolan smoking result of table 2 Different adding amount
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 grifolan, comfortable taste promotes, and miscellaneous QI and zest reduce.When grifolan consumption is less, the effect of Medicated cigarette is not as obvious by it；When its consumption is more than 1 ‰, the phenomenon that spine sense increase, concentration reduce occurs；When its consumption is 1 ‰, sucking quality is best.Therefore, adding best results during 0.1g grifolan in 100g Medicated cigarette, namely optimum consumption is 1 ‰.
Claims (2)
1. grifolan is as the application of tobacco humectant, it is characterized in that, described grifolan obtains through following step: by after the dry Grifola frondosa 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, 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 crude polysaccharides.
2. as claimed in claim 1 grifolan as the application of tobacco humectant, it is characterised in 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.
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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. |