CN104031162B - Radix Ophiopogonis polysaccharide, method for extraction and purification and the application as tobacco humectant thereof - Google Patents
Radix Ophiopogonis polysaccharide, method for extraction and purification and the application as tobacco humectant thereof Download PDFInfo
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Abstract
The present invention relates to a kind of Radix Ophiopogonis polysaccharide and method for extraction and purification thereof, particularly as follows: by dry Radix Ophiopogonis of pulverizing with after ether surname extraction, 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, use 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 is dried to obtain crude polysaccharides.Test proves: Radix Ophiopogonis polysaccharide of the present invention has good physics and sense organ humectation effect to Medicated cigarette, 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 Radix Ophiopogonis polysaccharide, method for extraction and purification and the application as tobacco humectant thereof.
Background technology
Currently, China's cigarette industry mainly use the polyhydroxy substances such as glycerol, propylene glycol, sorbitol as humectant, the main purpose using this type of humectant is 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, can make it have stronger moisture holding capacity.At present, at home and abroad there is no the relevant report applied in Medicated cigarette by Radix Ophiopogonis polysaccharide as tobacco humectant.
Summary of the invention
Present invention aim at providing a kind of Radix Ophiopogonis polysaccharide, 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 Radix Ophiopogonis polysaccharide, comprise the steps: the dry Radix Ophiopogonis pulverized with after ether surname extraction (typically adding ether by solid-liquid ratio 1g:5-8ml), 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, use 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 is dried to obtain khaki crude polysaccharides.
Further preferably, by crude polysaccharides chromatography purification twice, it is thus achieved that refined polysaccharide；Twice isolated and purified eluent used is respectively 0.5 mol/L NaCl solution and 0.05 mol/L NH4HCO3Solution.
Said extracted purification process is utilized to prepare the Radix Ophiopogonis polysaccharide of gained.
Said extracted purification process is utilized to prepare the application as tobacco humectant of the gained Radix Ophiopogonis polysaccharide.
The present invention obtains highly purified refined Radix Ophiopogonis 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 Medicated cigarette, 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) during the extraction of Radix Ophiopogonis polysaccharide, the method utilizing precipitate with ethanol, protease hydrolysis, Sevage removing protein and dialysis to combine except small molecular phase, significantly reduces the impurity in Radix Ophiopogonis polysaccharide, lays the foundation for the most isolated and purified.2) gel chromatography column chromatography for separation purification is used twice, it is thus achieved that highly purified refined Radix Ophiopogonis polysaccharide.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, Radix Ophiopogonis 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.
Main agents used by test and instrument:
Ether, ethanol, acetone (Suzhou chemical reagent company limited of China, analytical pure), DEAE-Celluose and Sephadex G200 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), TSKGEL G2000 PW high productivity computing post (Sigma Co., USA), Agilent LC1100 type efficient liquid phase instrument and differential pulse polarograpll instrument (Agilent company of the U.S.).
Embodiment
1
The method for extraction and purification of a kind of Radix Ophiopogonis polysaccharide, comprises the steps: the 300g pulverized to be dried Radix Ophiopogonis with 1800ml ether surname extraction 2h in order to remove oils and fats, and 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), and recentrifuge collects 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 and be placed in 70 DEG C of water-baths heating 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 be dried to obtain 8.1g khaki crude polysaccharides, yield is 2.70%.
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/L NaCl solution for flowing phase (i.e. eluent), flow velocity is 2.5ml/min, use Phenol-sulphate acid method that chromatographic solution is developed the color, collect main chromatographic peak, lyophilizing.Then by lyophilizing gained solid 0.05mol/L NH4HCO3Solution dissolves, with Sephadex G200 gel chromatographic columns chromatography again (5.0 × 50cm), with 0.05mol/L NH4HCO3Solution is flowing phase (i.e. eluent), and flow velocity is 2.0ml/min, uses Phenol-sulphate acid method to develop the color chromatographic solution, collects main chromatographic peak, and lyophilizing obtains the refined Radix Ophiopogonis polysaccharide solid of 392mg white, and yield 26.1%, LT1 sugar content is 96.6% after testing.
Embodiment
2
The method for extraction and purification of a kind of Radix Ophiopogonis polysaccharide, comprises the steps: the 300g pulverized to be dried Radix Ophiopogonis with 2000ml ether surname extraction 4h in order to remove oils and fats, and 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, and recentrifuge collects 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 and be placed in 70 DEG C of water-baths heating 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 be dried to obtain 7.5g khaki crude polysaccharides, yield is 2.50%.
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/L NaCl solution for flowing phase (i.e. eluent), flow velocity is 2.5ml/min, use Phenol-sulphate acid method that chromatographic solution is developed the color, collect main chromatographic peak, lyophilizing.Then by lyophilizing gained solid 0.05mol/L NH4HCO3Solution dissolves, with Sephadex G200 gel chromatographic columns chromatography again (5.0 × 50cm), with 0.05mol/L NH4HCO3Solution is flowing phase (i.e. eluent), and flow velocity is 2.0ml/min, uses Phenol-sulphate acid method to develop the color chromatographic solution, collects main chromatographic peak, and lyophilizing obtains the refined Radix Ophiopogonis polysaccharide solid of 383mg white, and yield 25.5%, LT1 sugar content is 96.6% after testing.
Application test: embodiment
1
Prepare gained and refine the Radix Ophiopogonis polysaccharide applied research as tobacco humectant
1, physics humid keeping performance test
For investigating the Radix Ophiopogonis polysaccharide physics humid keeping performance to Medicated cigarette, with Bright Yellow (great Jin circle) blank cigarette shreds as carrier, same for Radix Ophiopogonis polysaccharide glycerol, propylene glycol carry out together with sorbitol physics humid keeping performance contrast test research respectively, 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 balance 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 in the environment of relative humidity 40 ± 2% and solve wet process, and the change to instant moisture content is analyzed, investigate its physics humectation effect (after i.e. adding different sample, the moisture content of drying base in tobacco shred 72h changes), the results are shown in Table 1.
The physics humectation Contrast on effect of table 1 Radix Ophiopogonis polysaccharide, glycerol, propylene glycol and sorbitol
The result of the test of table 1 shows, add Radix Ophiopogonis 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 Radix Ophiopogonis 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, Radix Ophiopogonis polysaccharide is made into the solution that mass fraction is 1%.Take the above-mentioned solution containing Radix Ophiopogonis polysaccharide of 0.100g, 0.500g, 1.000g, 5.000g, 10.000g and 20.000g respectively, the most uniformly spray is added in five parts of 100g Bright Yellow blank cigarette shreds the most spiced, 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% balance 48h, smokes panel test.Control sample is Bright Yellow blank Medicated cigarette, and control sample balances 48h equally under mutually synthermal, damp condition.Smoking result is shown in Table 2.
The Radix Ophiopogonis polysaccharide smoking result of table 2 Different adding amount
By the smoking result of table 2 it can be seen that the Main Function of Medicated cigarette is shown as making flue gas substantially become mellow and full, soft by Radix Ophiopogonis polysaccharide, comfortable taste promotes, and miscellaneous QI and zest reduce.When Radix Ophiopogonis polysaccharide consumption is less, it is not clearly to the effect of Medicated cigarette；When its consumption reaches 1 ‰, occur that spine sense increases；When its consumption is more than 1 ‰, occurring that spine sense increases, concentration slightly reduces；When its consumption is 0.5 ‰, sucking quality is best.Therefore, when adding 0.05g Radix Ophiopogonis polysaccharide in 100g Medicated cigarette, best results, i.e. optimum consumption are 0.5 ‰.
Claims (2)
1. Radix Ophiopogonis polysaccharide is as the application of tobacco humectant, it is characterized in that, described Radix Ophiopogonis polysaccharide obtains through following step: by dry Radix Ophiopogonis of pulverizing with after ether surname extraction, 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, use 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 is dried to obtain crude polysaccharides；
During ether surname extraction, adding ether by solid-liquid ratio 1g:5-8ml, extraction time is 2-4h；
During boiling water extraction, 1g is dried and adds 2.5ml boiling water Radix Ophiopogonis.
2. as claimed in claim 1 Radix Ophiopogonis polysaccharide as the application of tobacco humectant, it is characterised in that by crude polysaccharides chromatography purification twice, it is thus achieved that refined polysaccharide；Twice isolated and purified eluent used is respectively 0.5 mol/L NaCl solution and 0.05 mol/L NH4HCO3Solution.
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| CN112830977B (en) * | 2021-02-26 | 2022-05-17 | 西南科技大学 | Method for extracting and purifying polysaccharide from fibrous root residues of radix ophiopogonis |
| CN115624514A (en) * | 2022-10-12 | 2023-01-20 | 杭州时光肌生物科技有限公司 | Preparation method of composite plant extract for improving facial redness |
| CN115746154A (en) * | 2022-11-22 | 2023-03-07 | 四川农业大学 | Extraction method and application of ophiopogon japonicus fibril polysaccharide with anti-infection effect |
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