CN101828764B - Gynura bicolor extract and usage thereof in removing free radical in cigarette smoke - Google Patents
Gynura bicolor extract and usage thereof in removing free radical in cigarette smoke Download PDFInfo
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- CN101828764B CN101828764B CN2010101690769A CN201010169076A CN101828764B CN 101828764 B CN101828764 B CN 101828764B CN 2010101690769 A CN2010101690769 A CN 2010101690769A CN 201010169076 A CN201010169076 A CN 201010169076A CN 101828764 B CN101828764 B CN 101828764B
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Abstract
The invention relates to a gynura bicolor extract for removing free radical in cigarette smoke, which is obtained by the following steps of: soaking dry gynura bicolor with an extractant I and extracting at high pressure; extracting the obtained residue by using an extractant II under ultrasonic twice; combining the three filtrates and carrying out evaporation, condensation and short-path distillation sequentially; and taking the fraction at the light component outlet of a short-path distiller. The extract of the invention can be used as an addition material for removing the free radical in the cigarette smoke.
Description
Technical field
The present invention relates to contain preparation, be specifically related to remove the preparation of free radical in the cigarette smoke from the removing free radical of Gynura bicolor organic principle.
Background technology
Gynura bicolor (B egonia f im bristipula Hance) is a Begoniaceae Begonia plant; Another name is red dish, the dish of enriching blood (Taiwan), curled mallow, blood skin dish, water pseudo-ginseng; A blood dish, Gynura bicolor, red kind of amaranth, red hair kind, red three-coloured amaranth, red dish, Radix Angelicae Sinensis dish, carbuncle dish, gynura bicolor, Gynura Root, kwan-yin dish, leaf lower red, red back of the body dish, red winter maple, red wind dish and kwan-yin amaranth etc.Gynura bicolor is with cook half cultigen of usefulness of young stem and leaf; Perennial perennial root evergreen herbage; The tool peat-reek is rich in trace elements such as flavonoid glycoside, vitamin and iron, copper, manganese, has clearing heat and detoxicating, cooling blood and hemostasis, moisturizes, drug effects such as the stasis of blood, detumescence are loose in relieving cough and reducing sputum, anti-inflammatory.Zhaoqing Dinghu Hill, Guangdong Province special product Gynura bicolor, usefulness among the people its as for tea beverage, the heat extraction of relieving summer heat, aid digestion, be good for the stomach, relieve the effect of alcohol.Have the pass reported in literature, Gynura bicolor has free radical in the human body of removing in addition, and then realizes antidotal purpose except that above-mentioned food therapy health effect.Therefore, significant to the Gynura bicolor further investigation.
" extraction of general flavone and Study of Antioxidation thereof in the Gynura bicolor " literary composition of " Food Science " 2007 04 phases the 145th～148 page of publication; This article has disclosed the optimum extraction process condition of " utilize 70% ethanol; solid-liquid ratio 1: 25, the preheating lixiviate is 30 minutes under 50 ℃ of conditions, then through 600W microwave treatment 120s " and when sample concentration is 0.66mg/mL; Removing effect to DPPH is best, and inhibiting rate reaches 91.2%.But well-known, ethanol is the bigger organic solvent of a kind of polarity, and it is on the high side therefore in ethanol medium, to leach the big slightly alkaline matter of polarity, if it is added in the cigarette, just with producing a kind of astringent taste in the flue gas suction population.And the ethanol with 70% is more as the stripping of extractant macromolecular substances, adds water and can produce the gelatin phenomenon commercial Application and be difficult to realize.Moreover, contain a large amount of haematochrome in the Gynura bicolor, the redness that the resulting extract of simple organic solvent low-temperature prewarming lixiviate is inevitable, if add the impression that obviously can influence cigarette in the cigarette to, bring unnecessary mental burden to the smoker.On the other hand, because cigarette is a kind of specialities that vision and the sense of taste sense of taste are especially had relatively high expectations, so the Gynura bicolor extract that method for distilling obtains described in the above-mentioned article is inappropriate for adding to and is used for removing the flue gas free radical in the cigarette.
Summary of the invention
In view of there is above-mentioned deficiency in prior art, technical problem to be solved by this invention provides a kind of Gynura bicolor extract that is used for removing the flue gas free radical in the cigarette that is suitable for adding to.
The scheme that the present invention solves the problems of the technologies described above is following:
A kind of Gynura bicolor extract, this extract is prepared by following method:
(1) get dry Gynura bicolor and pulverize, adds after 4～12 times of extractant I soaked 4-15 hour, extraction is 10-20 minute super-pressure extractor (UHP) in, centrifugal filtration, filtrate and filter residue subsequent use;
(2) get filter residue and add 3-10 extractant II doubly, add lactic acid again pH is transferred to 5～5.5, Extraction by Ultrasound is 10 minutes～60 minutes under 20～70 ℃ of conditions, centrifugal filtration, and it is subsequent use with filter residue to filtrate;
(3) filter residue of getting step (2) adds 3～10 times extractant II, adds lactic acid again pH is transferred to 5～5.5, and Extraction by Ultrasound is 10 minutes～60 minutes under 20～70 ℃ of conditions, centrifugal filtration, and reserved filtrate is subsequent use;
(4) filtrating of combining step (1), step (2) and step (3), 50～80 ℃ of following evaporation and concentration promptly are equivalent to contain in every milliliter of concentrate 120-180mg Gynura bicolor raw material to 120-180mg Gynura bicolor raw material/ml;
(5) filtrating after step (4) is concentrated is heated to 60 ℃～150 ℃ and sends in the scraped film type short-distance distiller; Be 1.0 * 101Pa～4.5 * 102Pa with temperature at pressure be to carry out short-path distillation under-25 ℃～10 ℃ the condition to separate; Get the cut of light component outlet, promptly get;
Wherein, described extractant I is made up of water 5～15 weight portions, ethanol 10～40 weight portions, propane diols 10～40 weight portions, third ethanol, 10～20 weight portions, ethyl acetate 10～20 weight portions and benzyl cinnamate 10～15 weight portions described extractant I; Described extractant II is made up of water 5～15 weight portions, ethanol 15～45 weight portions, propane diols 15～40 weight portions and 10～20 glycerine weight portions.
Gynura bicolor extract of the present invention, evaporating concentration process is preferably in the thin film evaporator and carries out described in the step of wherein said method for preparing extractive (4), takes off the flavor effect with further raising.
Extract of the present invention can be used for removing free radical in the flue gas; Concrete grammar can be before rolling cigarette, described extract to be sprayed onto in the pipe tobacco; Also with described extract attached on the carrier, add the filter tip of processing cigarette in the material of preparation filter stick then to.
Gynura bicolor extract according to the invention has following useful effect than prior art:
1, adopting extractant I according to the invention and extractant II all is the combination extractant; Adopt 70% single alcohol extract agent to compare with prior art; Except can the bioactive ingredients of Gynura bicolor being extracted, also avoided material strippings such as wax, pectin, starch, tannin and protein simultaneously.Materials such as wax, pectin, tannin and protein can influences greatly the sucking quality of cigarette, the fragrance of destruction cigarette, cause bad effect such as oral stimulation.And the ethanol with 70% is more as the stripping of extractant macromolecular substances, and thin up can produce the gelatin phenomenon commercial Application to be difficult to realize.So the ratio of water is one of key factor that influences this type content of material in the solution that extracts in the extractant.Adopt combination extractant of the present invention, can avoid these materials are extracted in the lump, add its style is maintained and promotes to.
The extract elder generation evaporation and concentration that 2, will adopt the organic solvent extraction to obtain; Short-path distillation (also claiming molecular clock) again; Extract stoste is pressed molecular weight separates; Removed the original smell of the haematochrome in the Gynura bicolor, macromolecular substances and Gynura bicolor, making the extract that obtains is a kind of transparency liquid of colorless and odorless.
Description of drawings
Fig. 1 is the extraction process flow chart of Gynura bicolor extract of the present invention.
The specific embodiment
One, preparation example
Example 1
1, preparation extractant
(1) respectively by weight ratio, 15 weight portions of fetching water, ethanol 25 weight portions, propane diols 40 weight portions, third ethanol, 15 weight portions, ethyl acetate 10 weight portions, benzyl cinnamate 12.5 weight portions mix and obtain the extractant I.
(2) respectively by weight ratio, 5 weight portions of fetching water, ethanol 30 weight portions, propane diols 40 weight portions, glycerine 15 weight portions mix and obtain the extractant II.
2, preparation Gynura bicolor
Referring to Fig. 1, the Gynura bicolor extract method for distilling described in this example is following:
(1) get dry Gynura bicolor and pulverize, adds after 8 times of extractant I soaked 9 hours, extraction is 15 minutes super-pressure extractor (UHP) in, centrifugal filtration, filtrate and filter residue subsequent use;
(2) get filter residue and add 6 times extractant II, add lactic acid again pH is transferred to 5, Extraction by Ultrasound is 35 minutes under 45 ℃ of conditions, centrifugal filtration, and it is subsequent use with filter residue to filtrate;
(3) filter residue of getting step (2) adds 6 times extractant II, adds lactic acid again pH is transferred to 5, and Extraction by Ultrasound is 35 minutes under 45 ℃ of conditions, centrifugal filtration, and reserved filtrate is subsequent use;
(4) filtrating of combining step (1), step (2) and step (3), 80 ℃ of following evaporation and concentration are to being equivalent to contain 150mg Gynura bicolor raw material in every milliliter of concentrate;
(5) filtrating after step (4) is concentrated is heated to 110 ℃ and sends in the scraped film type short-distance distiller; At pressure is that 3 * 102Pa separates for carrying out short-path distillation under-15 ℃ the condition with temperature; Get the cut of light component outlet, obtain colorless and odorless and transparent Gynura bicolor extract.
Example 2
1, preparation extractant
(1) respectively by weight ratio, 10 weight portions of fetching water, ethanol 40 weight portions, propane diols 25 weight portions, third ethanol, 10 weight portions, ethyl acetate 15 weight portions, benzyl cinnamate 15 weight portions mix and obtain the extractant I.
(2) respectively by weight ratio, 10 weight portions of fetching water, ethanol 45 weight portions, propane diols 27.5 weight portions, glycerine 10 weight portions mix and obtain the extractant II.
2, preparation Gynura bicolor
Referring to Fig. 1, the Gynura bicolor extract method for distilling described in this example is following:
(1) get dry Gynura bicolor and pulverize, adds after 5 times of extractant I soaked 15 hours, extraction is 20 minutes super-pressure extractor (UHP) in, centrifugal filtration, filtrate and filter residue subsequent use;
(2) get filter residue and add 4 times extractant II, add lactic acid again pH is transferred to 5.5, Extraction by Ultrasound is 60 minutes under 20 ℃ of conditions, centrifugal filtration, and it is subsequent use with filter residue to filtrate;
(3) filter residue of getting step (2) adds 4 times extractant II, adds lactic acid again pH is transferred to 5.2, and Extraction by Ultrasound is 60 minutes under 20 ℃ of conditions, centrifugal filtration, and reserved filtrate is subsequent use;
(4) filtrating of step (1), step (2) and step (3) merges and to be placed in the thin film evaporator, 60 ℃ of following evaporation and concentration to being equivalent to contain 120mg Gynura bicolor raw material in every milliliter of concentrate;
(5) filtrating after step (4) is concentrated is heated to 60 ℃ and sends in the scraped film type short-distance distiller; At pressure is that 4.5 * 101Pa separates for carrying out short-path distillation under-25 ℃ the condition with temperature; Get the cut of light component outlet, obtain colorless and odorless and transparent Gynura bicolor extract.
Example 3
1, preparation extractant
(1) respectively by weight ratio, 5 weight portions of fetching water, ethanol 25 weight portions, propane diols 10 weight portions, third ethanol, 15 weight portions, ethyl acetate 20 weight portions, benzyl cinnamate 10 weight portions mix and obtain the extractant I.
(2) respectively by weight ratio, 15 weight portions of fetching water, ethanol 30 weight portions, propane diols 15 weight portions, glycerine 20 weight portions mix and obtain the extractant II.
2, preparation Gynura bicolor
Referring to Fig. 1, the Gynura bicolor extract method for distilling described in this example is following:
(1) get dry Gynura bicolor and pulverize, adds after 12 times of extractant I soaked 5 hours, extraction is 10 minutes super-pressure extractor (UHP) in, centrifugal filtration, filtrate and filter residue subsequent use;
(2) get filter residue and add 10 times extractant II, add lactic acid again pH is transferred to 5.5, Extraction by Ultrasound is 10 minutes under 70 ℃ of conditions, centrifugal filtration, and it is subsequent use with filter residue to filtrate;
(3) filter residue of getting step (2) adds 10 times extractant II, adds lactic acid again pH is transferred to 5, and Extraction by Ultrasound is 10 minutes under 70 ℃ of conditions, centrifugal filtration, and reserved filtrate is subsequent use;
(4) merging of the filtrating of step (1), step (2) and step (3) is placed in the thin film evaporator, 70 ℃ of following evaporation and concentration to being equivalent to contain 150mg Gynura bicolor raw material in every milliliter of concentrate;
(5) filtrating after step (4) is concentrated is heated to 150 ℃ and sends in the scraped film type short-distance distiller; Be 1.0 * 101Pa with temperature at pressure be to carry out short-path distillation under 10 ℃ the condition to separate; Get the cut of light component outlet, obtain colorless and odorless and transparent Gynura bicolor extract.
Two, application examples
Example 1
The Gynura bicolor extract adding volume ratio of getting the foregoing description 1 is that 10 volumes concentration doubly is 70% ethanol; Mixing the back is sprayed onto on the pipe tobacco by 0.05% of pipe tobacco weight uniformly; Sealing was deposited 2-3 hour at ambient temperature then; Let itself and pipe tobacco fully absorb, being dried to moisture content again is 12.5%, processes cigarette by common process.
Example 2
The Gynura bicolor extract adding volume ratio of getting the foregoing description 1 is that 10 volumes concentration doubly is 70% ethanol; Mixing the back is sprayed onto on the pipe tobacco by 0.1% of pipe tobacco weight uniformly; Sealing was deposited 2-3 hour at ambient temperature then; Let itself and pipe tobacco fully absorb, being dried to moisture content again is 12.5%, processes cigarette by common process.
Example 3
The Gynura bicolor extract adding volume ratio of getting the foregoing description 1 is that 20 volumes concentration doubly is 70% ethanol; Mixing the back is sprayed onto on the pipe tobacco by 0.08% of pipe tobacco weight uniformly; Sealing was deposited 2-3 hour at ambient temperature then; Let itself and pipe tobacco fully absorb, being dried to moisture content again is 12.5%, processes cigarette by common process.
Example 4
Earlier active carbon is fully immersed in the Gynura bicolor extract of embodiment 1 in the preparation example, obtains composite activated carbon after the drying; Then the gained composite activated carbon is added on the intrafascicular cellulose acetate filter rod that obtains feeding in raw material that rolls of loose acetate fibres at filter-stick forming device, at last with described reinforced cellulose acetate filter rod and common cellulose acetate filter rod by 2: 1～1: 2 length compound promptly get can remove free radical in the cigarette smoke filter tip.
Three, effect experimental example
1, the preparation of sample and reference substance
Sample and reference substance are circumference 24.5mm, total length 84mm, and filter length 25mm adopts same pipe tobacco, and the filter stick material is acetate silk.Totally 4 groups in sample, wherein, 3 groups cigarette part is pressed the example 1 of above-mentioned application examples respectively, and example 2 is prepared from example 3 said methods, and filter tip is the filter tip that common cellulose acetate filter rod is made, and difference called after sample 1, sample 2 and sample 3; 1 group cigarette part is prepared from by the example 1 said method of above-mentioned application examples respectively, and filter tip adopts the example 4 said methods of above-mentioned application examples to be prepared from called after sample 4.1 group of reference substance, its pipe tobacco is processed by conventional method with the filter stick material raw material identical with sample.
2, experimental technique
2.1 above-mentioned sample and reference substance are placed climatic chamber; In temperature is 22 ± 1 ℃; Balance 48h under the condition of relative humidity 60% ± 2%, from every group of sample and reference substance, select respectively then the average weight deviation for ± 0.02g and average resistance to suction deviation for the cigarette the in ± 49Pa scope as laboratory sample.
2.2 hexichol is processed 1.5 * 10 for bitter taste diazanyl free radical (being DPPH) by conventional method
15Spin, 3.0 * 10
15Spin and 6.0 * 10
15The series standard sample of Spin is proofreaied and correct and the confirming of concentration benchmark electron spin resonance spectrometer.
2.3 sample and reference substance are placed on respectively on the 5 duct smoking machines by the suction of ISO4387 method, and directly collect the flue gas of cigarette with cambridge filter.After taking off cambridge filter; It is 22 ± 2 ℃ in temperature earlier; Relative humidity is 60% ± 5% time balance 30～60min; Pack into then and use electron spin resonance spectrometer to carry out EPR in the high-precision quartz pipe of 3mm diameter to detect, write down the free radical mean concentration of pairing sample of each cambridge filter and reference substance simultaneously.
2.4 after obtaining the free radical mean concentration of sample and reference substance, the percentage of free radical mean concentration ratio of difference and reference substance that the free radical mean concentration that calculates reference substance deducts the free radical mean concentration of sample promptly gets free radical scavenging activity.Concrete outcome is as shown in the table.
Gynura bicolor extract reduces the effect of free-radical contents in the cigarette smoke
Claims (3)
1. Gynura bicolor extract, this extract is prepared by following method:
(1) get dry Gynura bicolor and pulverize, adds after 4～12 times of extractant I soaked 4-15 hour, in the super-pressure extractor, extracted 10-20 minute, centrifugal filtration, filtrate and filter residue subsequent use;
(2) get filter residue and add 3-10 extractant II doubly, add lactic acid again pH is transferred to 5～5.5, Extraction by Ultrasound is 10 minutes～60 minutes under 20～70 ℃ of conditions, centrifugal filtration, and it is subsequent use with filter residue to filtrate;
(3) filter residue of getting step (2) adds 3～10 times extractant II, adds lactic acid again pH is transferred to 5～5.5, and Extraction by Ultrasound is 10 minutes～60 minutes under 20～70 ℃ of conditions, centrifugal filtration, and reserved filtrate is subsequent use;
(4) filtrating of combining step (1), step (2) and step (3), 50～80 ℃ of following evaporation and concentration are to 120-180mg Gynura bicolor raw material/ml;
(5) filtrating after step (4) is concentrated is heated to 60 ℃～150 ℃ and sends in the scraped film type short-distance distiller; Be 1.0 * 101Pa～4.5 * 102Pa with temperature at pressure be to carry out short-path distillation under-25 ℃～10 ℃ the condition to separate; Get the cut of light component outlet, promptly get;
Wherein, described extractant I is made up of water 5～15 weight portions, ethanol 10～40 weight portions, propane diols 10～40 weight portions, third ethanol, 10～20 weight portions, ethyl acetate 10～20 weight portions and benzyl cinnamate 10～15 weight portions; Described extractant II is made up of water 5～15 weight portions, ethanol 15～45 weight portions, propane diols 15～40 weight portions and glycerine 10～20 weight portions.
2. a kind of Gynura bicolor extract according to claim 1 is characterized in that, the evaporating concentration process step (4) of extract is carried out in thin film evaporator.
3. claim 1 or 2 described Gynura bicolor extracts are as the application of removing the additive of free radical in the cigarette smoke.
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| CN2010101690769A CN101828764B (en) | 2010-05-12 | 2010-05-12 | Gynura bicolor extract and usage thereof in removing free radical in cigarette smoke |
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| CN2010101690769A CN101828764B (en) | 2010-05-12 | 2010-05-12 | Gynura bicolor extract and usage thereof in removing free radical in cigarette smoke |
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| CN101828764B true CN101828764B (en) | 2012-05-23 |
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| CN104970445B (en) * | 2015-07-21 | 2017-11-07 | 中国烟草总公司广东省公司 | A kind of spacetabs type aerosol mouth cigarette |
| CN105920065A (en) * | 2016-04-21 | 2016-09-07 | 肇庆医学高等专科学校 | Separation and purification method of begonia fimbritipula saponin and application of begonia fimbritipula saponin |
| CN106189349A (en) * | 2016-07-15 | 2016-12-07 | 广西顺帆投资有限公司 | A kind of method extracting dyestuff based on Radix seu Folium Alchorneae trewioidis |
| TWI642632B (en) * | 2017-04-06 | 2018-12-01 | 國立宜蘭大學 | Gynura decolorized metabolite, the composition and the use for decolorization of dye thereof |
| CN109527641B (en) * | 2017-09-22 | 2021-04-27 | 江西中烟工业有限责任公司 | Tobacco extract and preparation method thereof |
| CN111122764B (en) * | 2020-01-18 | 2022-03-11 | 河北中医学院 | Rapid multi-information thin-layer identification method for muskroot-like semiaquilegia root granules and target decoction dry powder |
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