CN1220460C - Application of emblic leafflower fruit extract as free radical scavenger of tobacco products and relevant tobacco products thereof - Google Patents
Application of emblic leafflower fruit extract as free radical scavenger of tobacco products and relevant tobacco products thereof Download PDFInfo
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- CN1220460C CN1220460C CN 200410022439 CN200410022439A CN1220460C CN 1220460 C CN1220460 C CN 1220460C CN 200410022439 CN200410022439 CN 200410022439 CN 200410022439 A CN200410022439 A CN 200410022439A CN 1220460 C CN1220460 C CN 1220460C
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Abstract
The present invention belongs to an application of a natural extract of plant in tobacco manufacturing. An extract of phyllanthi fructus is used as the free radical scavenger of smoking tobacco products, and the added extract can be prepared from a plurality of ingredients with a mixed state or be prepared from a mixture of one kind or more than one kinds of separated extracts. The tobacco products can be cigarettes and cigars or pipe tobacco shreds; if produce a cigarette, the extract of phyllanthi fructus can be added into the tobacco shreds or inside the filter tip; if the extract of phyllanthi fructus is added into the tobacco shreds, the procedure can be carried out during the process of tobacco shreds rolling, and the extract of phyllanthi fructus is from 0.02 to 0.06 wt% of the tobacco shreds. The invented product is manufactured by the invented application. The present invention has the advantage that a new health care function and a new field of application of phyllanthi fructus are developed. When used as a free radical scavenger, the extract of phyllanthi fructus has the advantages of obvious effect and good application prospect of the development of safety tobacco with low toxicity and low free radical.
Description
Affiliated technical field
The invention belongs to the natural plant extract in the tobacco product Application in Manufacturing Industry.
Background technology
People aspirate the flue gas that the tobacco product burning is produced, but have the free radical of cytotoxic molecule in the flue gas.These cytotoxic molecules bring out cancer in smoker's body, particularly lung cancer.The safety-type tobacco product of Development and Production low free radical is the important R﹠D direction of tobacco product industry in recent years.
Emblic is the dry mature fruit of euphorbia plant emblic Phyllanthus emblica L..Fresh fruit is sepia to blackish green, sphere or oblate spheroid, and nature and flavor are sweet, sour, puckery, cool, can be used as medicine.Present artificial cultivation and wild emblic fruit all are used as raw materials of food processing.The emblic extract composition is complicated, contains multiple bioactivators such as polysaccharide, Polyphenols, caffeine, SOD, vitamin C, can extract gallic acid and superoxide dismutase (SOD).Someone to its anti-oxidant, anti-anoxic, antifatigue, antitumor, reducing blood lipid, norcholesterol, fall blood viscosity and improve digestive functions etc. and carried out some exploitative experiments researchs, as seen the report of following document: " Yunnan hotwork science and technology ", 1999,2:23~25; " pharmacy progress ", 2001,4:12~13; " Wuhan University of Technology's journal ", 2000,2:13~15; " Guiyang College of Traditional Chinese Medicine's journal ", 2002,24 (2): 50~51.But emblic extract as the free radical scavenger in the tobacco product suction, is not seen bibliographical information so far.
Summary of the invention
The object of the present invention is to provide the new purposes of emblic and by product that this purposes obtained, purposes and the corresponding tobacco product of emblic extract as the tobacco product free radical scavenger promptly is provided, with the regional advantages of performance natural plant resource, satisfy pressing for of cigarette industry exploitation low free radical safety type cigarette.
Applicant is at first separated the emblic extract that obtains with regard to extraction and is carried out the Green Tea Extract performance evaluation, and its application in reducing the cigarette smoke free radical is studied.
The analysis of experiments situation that emblic extract carries out the Green Tea Extract performance is as follows.
Instrument and reagent:
Bruker-EMX6/1 EPR spectrometer ESR (German Bruker company).
752 type spectrophotometers (Shanghai Precision Scientific Apparatus Co., Ltd's analytical instrument head factory).
Free radical generating agent: DPPH (1.1-Diphenyl-2-picryl-hydrazyl), the Tokyo changes into Co., Ltd. and produces, A.R.
Emblic: available from market, Kunming.
One, emblic extract Green Tea Extract performance ESR analyzes
The acquisition of emblic extract: the fresh emblic that market is bought, stoning takes by weighing 100g after pulverizing, and adds industrial alcohol refluxing extraction 4h, filters while hot, extracts 3 times merging filtrate.The extract decompression and solvent recovery obtains emblic extract.With 50% ethanol is solvent, is mixed with the emblic extract sample liquid C of 0.1g/L
0
Free radical ESR analyzes experiment condition: EPR spectrometer test parameter: central magnetic field=3.385T, sweep wide=0.500T, microwave frequency=1.5GHz; Sweep time=2min, scanning times=1, multiplication factor=2.5 * 10
4, amount of samples=20 μ L.
Contrast blank and test specimens preparation: 0.000001mo/L DPPH solution is that solvent is made into the absolute ethyl alcohol, is the blank sample; Toward 0.000001mol/L DPPH solution, add emblic extract sample liquid C again
0, making emblic extract sample liquid mass concentration is 0.0001g/L, fully mixing is test specimens.
With EPR spectrometer analytical test Green Tea Extract performance, obtain paramagnetic resonance collection of illustrative plates (EPR).
Two, emblic extract Green Tea Extract performance DPPH spectrophotometric analysis
Experiment condition: through testing the maximum absorption wavelength of determining DPPH is 520nm, and the emblic extract sample liquid is almost colourless under this experiment condition, and the measurement peak 520nm of DPPH be can not form interference, and experiment selects for use 520nm as measuring wavelength.Experiment finds that in the pH6.88 buffer medium, DPPH free radical displaing amaranth changes the cushioning liquid consumption, and the DPPH solution absorbance does not change substantially, and the nearly neutral buffered solution of pH6.88 is selected in experiment for use.Because the reaction of extract sample and DPPH is exceedingly fast, and just can finish 85% degree of reaction in the 1min.Absorbance is constant substantially behind the reaction 5min.It is the reaction time that 10min is chosen in experiment.DPPH is to temperature-insensitive, and reaction is at room temperature selected in experiment for use.
The emblic extract sample solution of experimental technique: 100g/L: prepare with 50% ethanol.In the 10mL colorimetric cylinder, add 4mL pH6.88 standard PBS successively, 4mL 0.0001777mol/L DPPH solution, mixing, add a certain amount of emblic extract sample liquid again, distilled water replenishes volume to the 10.00mL scale, abundant mixing, behind the 10min in 520nm place survey absorbance.
The definition emblic is to the clearance rate K=[1-(A of DPPH free radical
i-A
j)/Ac * 100%,
In the formula: A
i-Jia emblic reaction back DPPH solution absorbance;
A
j-do not add DPPH, only add the solution absorbency of emblic and water;
Ac-does not add emblic, only adds the solution absorbency of DPPH and water.
The Green Tea Extract performance that can compare emblic extract according to K.
Three, experimental result and analysis
1, ESR method
Because DPPH can produce the long-life free radical, carry out the ESR detection as free radical generating agent and as the blank thing at this.Through adding emblic behind extract, the free radical quantity that DPPH is produced owing to its anti-radical action reduces.The free radical relative amount changes the Green Tea Extract performance that can reflect emblic extract.Contrast is carried out ESR and is detected the collection of illustrative plates obtain and see Fig. 1.
According to measuring collection of illustrative plates peak height (mm), can compare the clearance rate of the free radical of emblic extract sample liquid.
Ar=(H
Contrast-H
Test)/H
Contrast
(48.6-21.9)/48.6=0.549=54.9%
Electron paramagnetic resonance (EPR or ESR) is unique method that can directly detect the free radical signal.Be mainly used to study free radical, atom, molecule (comprising the triplet state molecule) with unpaired electron structure, its remolding sensitivity NMR high 230 times (theoretical values), and can be not the prefered method that present free radical detects to the free-radical generating destruction.This experiment with DPPH (1,1-diphenyl-2-picryl hydrazine free radical, C
18H
12N
5O
6) be free radical generation thing, under the sample condition, add the emblic matter sample, the signal after the DPPH free radical reduces after detecting the DPPH free radical signal of DPPH generation and adding the emblic extract sample.According to the relative variation of spectrum peak heights, can estimate the variation of free radical quantity, the radical scavenging activity of reflection emblic polyphenoils.
According to the EPR experimental data as can be seen, under above experiment condition, 54.9% DPPH free radical illustrates that owing to the effect of emblic extract reduces emblic extract has radicals scavenging effect preferably.
2, AAS
In existing antioxidant and free radical were analyzed, general way was manually to set up the generation system of active oxygen or free radical, detected the free radical that wherein produces then, and antioxidant or free radical scavenger are to the inhibition removing behavior of generation free radical.Experiment and studies show that, as the DPPH of long-life free radical (1,1-diphenyl-2-picryl hydrazine free radical, C
18H
12N
5O
6), itself also can be used as free radical the source takes place, and can reduce with the emblic extract effect or be eliminated.And, can produce bleach effect doing the time spent, thereby can utilize AAS that it is studied with emblic extract because DPPH has special purple.According to the variation of DPPH, can know the Green Tea Extract ability of emblic extract by inference in 520nm place characteristic absorption.
Press the emblic extract sample liquid of experimental technique adding different volumes, measure A
i, A
j, Ac, calculate its corresponding free radical scavenging activity K in view of the above again, the results are shown in Figure 2.
As can be seen from Figure 2, emblic extract possesses the ability of removing the DPPH free radical, and its ability and extract consumption of removing the DPPH free radical all is dose-effect relationship: along with the increase of emblic extract consumption, the DPPH free radical of its reduction is also many more.
Emblic extract has tangible radicals scavenging effect.Under the same conditions, emblic extract is proportionate to the clearance rate of free radical and the concentration of its use.Reach one regularly but work as its concentration, its effect increase is promptly no longer obvious.Under above experimental technique, the free radical scavenging activity of emblic extract is different between 30%-80%.
According to the experimental study result, it is as follows to obtain the present invention:
The technical scheme of purposes invention is among the present invention: the extract of emblic is used as free radical scavenger in the tobacco product suction.Said tobacco product can be a cigarette, also can be cigar or tobacco pipe pipe tobacco.If cigarette, then the extract of emblic can add in the pipe tobacco of cigarette, also can add in the filter tip of cigarette.
The emblic extract that is added can be the extract under the multiple composition admixture, also can be the mixture of isolated a kind of extract or more than one extracts the extract under multiple composition admixture.
The approach that obtains emblic extract has multiple, for example can obtain by polar solvent such as alcohol or aqueous alcohols solvent extraction.The alcohol that is used as solvent especially can be ethanol.This extract also can obtain by supercritical carbon dioxide extracting.Certainly also can carry out supercritical carbon dioxide extracting more earlier after polar solvent extracts obtains.
The method of the one-tenth branch of extraction and separation emblic extract is a prior art, and it reports visible many public publications.
If emblic extract is added in the pipe tobacco of cigarette, can roll in the process at the pipe tobacco of production of cigarettes and implement.Be added into the emblic extract in the pipe tobacco, can account for 0.02%~0.06% of pipe tobacco weight, be preferably and account for 0.03%~0.05% of pipe tobacco weight.Emblic extract can be dissolved in the solvent, the solvent that is dissolved with emblic extract is sprayed on the pipe tobacco, evaporate said solvent subsequently.
Product of the present invention, the tobacco product that is obtained by above-mentioned emblic extract purposes invention exactly.
The anti-oxidant behavior of antioxidant has certain selectivity.The main component of the free radical in the smoking gas phase is alkanes and alcoxyl type free base.Will effectively remove the free radical in the flue gas, selected antioxidant should have versatility, promptly has the ability of removing multiple free radical.Patent applicant's series of experimental research result shows that the emblic extract of adding can be removed the free radical in the flue gas effectively when tobacco product aspirates, and promptly emblic extract meets the requirement of removing free radical in the tobacco.Add the tobacco product of emblic extract and comparing of not adding, no matter the molecule of cytotoxin free radical in the former flue gas is a gas phase or a phase, can both significantly be reduced.
The invention has the beneficial effects as follows, excavated new health purpose, opened up a new application for emblic.Emblic extract is as the tobacco product free radical scavenger, and effect is obvious, and exploitation low toxicity safety-type tobacco product harmful, low free radical is had good application prospects.
Description of drawings
What Fig. 1 was an emblic extract to tester DPPH free radical influences the ESR collection of illustrative plates.
Fig. 2 is the spectrophotometric analysis result of emblic extract Green Tea Extract.
The present invention is described further by embodiment below, but scope of invention is not subjected to the limitation of illustrated embodiment.
The specific embodiment
See following embodiment.
(1) preparation of extract
The fresh emblic that market is bought, stoning are pulverized the back and are added industrial alcohol refluxing extraction 4h, filter while hot, extract 3 times merging filtrate.The extract decompression and solvent recovery obtains emblic extract.
(2) in the pipe tobacco of cigarette, add emblic extract
Extract rolled in the pipe tobacco of production of cigarettes add pipe tobacco in the process.Be added into the emblic extract in the pipe tobacco, account for 0.04% of pipe tobacco weight.Concrete grammar is earlier the said extracted thing of emblic to be dissolved in the ethanol, and the ethanol that is dissolved with emblic extract evenly is sprayed on the pipe tobacco, and ethanol is evaporated subsequently.Pipe tobacco rolls into test sample cigarette through cigarette machine.
(3) the removing effect of free radical in the cigarette smoke
The detection of free radical has multiple known method to adopt, electron spin resonance (ESR) for example, chromatography, chemoluminescence method, XRF, AAS etc.One of the device people such as visible Pryor that are used for holding back cigarette smoke gas phase and grain phase free radical publication " Environmengtal Health Perspectives " (1976, vol.16, report pp161-175).
The main electron paramagnetic resonance method that adopts is tested in the process of the present invention, also uses additive method, particularly AAS simultaneously, test result has been done contrast reflected card, and the result conforms to.Used EPR spectrometer is the BKER-EMX6/1 of German BRUKER company.
1, blank test
Is the concentration adjustment of the gaseous phase free radical trapping agent DMPO in the organic solvent-benzene 20 mMs, and use 5 cigarette that are not added with emblic extract (brand is " cloud and mist ") to carry out in its flue gas gas phase and grain catching of free radical mutually, carry out free radical mensuration with ESR then.ESR instrument parameter: CF:3385G, SW:200G, MA:1G, SP:20MV.Location parameter: scan multiplication factor: 5 * 10 5 times
5How many visual sample free-radical contents of multiplication factor is adjusted.5 times mean value is calculated in parallel determination 5 times.
2, clearance test
Use 5 cigarette that are added with emblic extract (brand is " cloud and mist ") to carry out in its flue gas gas phase and grain catching of free radical mutually, repetition aforesaid operations.
Blank test and clearance test are all carried out record with automatic recording instrument to sample free radical signal peak height, and its peak height is directly proportional with free-radical contents, carries out the comparison of free-radical contents relative size with this.
Reduction effect to grain phase free-radical contents in the flue gas sees the following form:
Numbering | 1 | 2 | 3 | 4 | 5 |
Blank sample ESR peak height/cm | 6.6 | 7.0 | 9.0 | 7.8 | 7.6 |
Sample survey ESR peak height/cm | 5.5 | 6.3 | 6.4 | 7.0 | 6.3 |
Peak height reduced rate/% | 16.7 | 10.0 | 28.9 | 10.3 | 16.5 |
As can be seen from the above table, because the inhomogeneities that sample cigarette rolls, emblic extract reduces the ratio of grain phase free radical in the cigarette smoke between 10.0~28.9%, and mean value is 16.5%.
Result of the test shows that also the ratio mean value that emblic extract reduces gaseous phase free radical in the cigarette smoke is 20.8%.
Claims (6)
1, emblic extract is as the purposes of tobacco product free radical scavenger.
2, purposes as claimed in claim 1 is characterized in that wherein said emblic extract obtains for extracting by polar solvent.
3, as the purposes of claim 1 or 2, it is characterized in that emblic extract is added in the pipe tobacco of cigarette, and roll in the process at the pipe tobacco of production of cigarettes and to implement, the emblic extract that is added in the pipe tobacco accounts for 0.02%~0.06% of pipe tobacco weight.
4, purposes as claimed in claim 3, the emblic extract that it is characterized in that being added in the pipe tobacco accounts for 0.03%~0.05% of pipe tobacco weight.
5, purposes as claimed in claim 4 is characterized in that emblic extract is dissolved in the solvent, and the solvent that is dissolved with emblic extract is sprayed on the pipe tobacco, evaporates said solvent subsequently.
6, be added with the tobacco product of emblic extract as free radical scavenger.
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Families Citing this family (6)
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CN101787329B (en) * | 2010-03-10 | 2012-02-08 | 广东中烟工业有限责任公司 | Tobacco flavor as well as preparation method and application thereof |
CN104232309A (en) * | 2014-09-30 | 2014-12-24 | 云南中烟工业有限责任公司 | Tobacco flavor prepared from phyllanthus emblica, plum, broadleaf holly leaf and tobacco and application of tobacco flavor |
CN105595421B (en) * | 2015-10-23 | 2019-03-12 | 云南中烟工业有限责任公司 | A kind of cigarette filter rod plant compound granular and preparation method thereof |
CN110184121A (en) * | 2019-04-29 | 2019-08-30 | 深圳市永沣香料有限公司 | Cigarette quick-fried pearl essential oil and the preparation method and application thereof |
CN111575113A (en) * | 2020-05-21 | 2020-08-25 | 云南中烟再造烟叶有限责任公司 | Cigarette containing emblic leafflower fruit extract and application thereof |
CN111772227B (en) * | 2020-08-10 | 2022-05-03 | 四川中烟工业有限责任公司 | Phyllanthus emblica targeted refined substance, preparation method and application thereof in cigarettes |
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