CN101544991A - Natural antioxidant of perilla flavone for cigarette and method for preparing same - Google Patents
Natural antioxidant of perilla flavone for cigarette and method for preparing same Download PDFInfo
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- CN101544991A CN101544991A CN200810047174A CN200810047174A CN101544991A CN 101544991 A CN101544991 A CN 101544991A CN 200810047174 A CN200810047174 A CN 200810047174A CN 200810047174 A CN200810047174 A CN 200810047174A CN 101544991 A CN101544991 A CN 101544991A
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- perilla
- cigarette
- flavone
- antioxidant
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- 229930003944 flavone Natural products 0.000 title claims abstract description 60
- 235000011949 flavones Nutrition 0.000 title claims abstract description 60
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 title claims abstract description 49
- 150000002212 flavone derivatives Chemical class 0.000 title claims abstract description 49
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 235000004347 Perilla Nutrition 0.000 title claims abstract description 46
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000003963 antioxidant agent Substances 0.000 title claims abstract description 12
- 235000006708 antioxidants Nutrition 0.000 title claims abstract description 11
- 230000003078 antioxidant effect Effects 0.000 title claims abstract description 9
- 244000124853 Perilla frutescens Species 0.000 title description 2
- 241000229722 Perilla <angiosperm> Species 0.000 claims abstract description 46
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000605 extraction Methods 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 108090000790 Enzymes Proteins 0.000 claims abstract description 6
- 102000004190 Enzymes Human genes 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- 238000010992 reflux Methods 0.000 claims abstract description 5
- 238000007670 refining Methods 0.000 claims abstract description 4
- 238000000703 high-speed centrifugation Methods 0.000 claims abstract description 3
- 239000012528 membrane Substances 0.000 claims description 17
- 238000002360 preparation method Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 150000002213 flavones Chemical class 0.000 claims description 11
- 108010059892 Cellulase Proteins 0.000 claims description 8
- 102000035195 Peptidases Human genes 0.000 claims description 8
- 108091005804 Peptidases Proteins 0.000 claims description 8
- 108010059820 Polygalacturonase Proteins 0.000 claims description 8
- 229940106157 cellulase Drugs 0.000 claims description 8
- 239000000341 volatile oil Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 6
- 210000002421 cell wall Anatomy 0.000 claims description 5
- 229940088598 enzyme Drugs 0.000 claims description 5
- 235000012054 meals Nutrition 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 4
- 235000013305 food Nutrition 0.000 claims description 4
- 238000007654 immersion Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000012856 packing Methods 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- 239000000284 extract Substances 0.000 abstract description 14
- 241000208125 Nicotiana Species 0.000 abstract description 9
- 235000002637 Nicotiana tabacum Nutrition 0.000 abstract description 9
- 239000000654 additive Substances 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 238000002791 soaking Methods 0.000 abstract 2
- 238000006555 catalytic reaction Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 34
- -1 hydroxyl radical free radical Chemical class 0.000 description 11
- 239000000779 smoke Substances 0.000 description 10
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- 150000003254 radicals Chemical class 0.000 description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 230000031700 light absorption Effects 0.000 description 6
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 239000003546 flue gas Substances 0.000 description 5
- 239000007792 gaseous phase Substances 0.000 description 5
- 238000009413 insulation Methods 0.000 description 4
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 description 3
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 description 3
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 description 3
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 description 3
- 235000005493 rutin Nutrition 0.000 description 3
- 229960004555 rutoside Drugs 0.000 description 3
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 2
- 238000004435 EPR spectroscopy Methods 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002953 phosphate buffered saline Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000001953 sensory effect Effects 0.000 description 2
- 239000008159 sesame oil Substances 0.000 description 2
- 235000011803 sesame oil Nutrition 0.000 description 2
- 230000000391 smoking effect Effects 0.000 description 2
- 235000010288 sodium nitrite Nutrition 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- CASFCVRUBIJLBN-UHFFFAOYSA-N 2-(1,10-phenanthrolin-2-yl)ethanol Chemical compound OCCc1ccc2ccc3cccnc3c2n1 CASFCVRUBIJLBN-UHFFFAOYSA-N 0.000 description 1
- HDPISCIDKUMRDI-UHFFFAOYSA-M N(=O)[O-].[Na+].[N+](=O)([O-])[O-].[Al+3] Chemical compound N(=O)[O-].[Na+].[N+](=O)([O-])[O-].[Al+3] HDPISCIDKUMRDI-UHFFFAOYSA-M 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- LOKCTEFSRHRXRJ-UHFFFAOYSA-I dipotassium trisodium dihydrogen phosphate hydrogen phosphate dichloride Chemical compound P(=O)(O)(O)[O-].[K+].P(=O)(O)([O-])[O-].[Na+].[Na+].[Cl-].[K+].[Cl-].[Na+] LOKCTEFSRHRXRJ-UHFFFAOYSA-I 0.000 description 1
- 239000008157 edible vegetable oil Substances 0.000 description 1
- 230000007760 free radical scavenging Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 235000014347 soups Nutrition 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000019505 tobacco product Nutrition 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Manufacture Of Tobacco Products (AREA)
- Pyrane Compounds (AREA)
Abstract
The invention discloses a natural antioxidant of perilla flavone for cigarette and a method for preparing the same, and relates to the technical field of additives for cigarettes. The natural antioxidant of perilla flavone for cigarette is prepared by the following steps that: the residue obtained after the naphtha is extracted from perilla leaves is dried, subjected to vacuum film breaking, soaking, compound enzyme-catalysis, namely ethanol refluxing extraction, pressure reduction suction filter and low-temperature high-speed centrifugation and refined to obtain an extracting solution of perilla flavone. The method for preparing the natural antioxidant of perilla flavone for cigarette comprises the following steps: (1) raw material processing, and vacuum film breaking; (2) soaking, and adding 0.1 to 1 percent compound enzyme; and (3) extraction and refining. When the extract of the invention is added to the cut tobacco, the quality of the cut tobacco is not changed. The raw material used by the invention is wide in source and low in cost and price; and the method has the advantages of simple technological process and simple equipment, and the extract can be used as a novel natural antioxidant for cigarette.
Description
Technical field
The present invention relates to the cigarette additive technical field, specifically a kind of natural cigarette extraction preparation method of antioxidant-perilla flavone.
Background technology
In tobacco product, should guarantee the flue gas quality, guarantee the low hazardness of cigarette again, in cigarette, add cigarette additive-antioxidant and more and more come into one's own.Extract natural antioxidants and carry out cigarette with being an important directions of lowering harm and decreasing coking, the applicant is exploring along this direction just.
Perilla Leaf is the leaf of labiate purple perilla Perilla frutescens (L.) Britt., claims Su Ye again, and tool is separated table function, is the annual herb plant.Originate in China, nowadays mainly be distributed in countries such as India, Burma, China, Japan, Korea, Korea S, Indonesia and Russia.All there are wild species and cultivar in China North China, Central China, south China, southwest and Taiwan Province.Purple perilla is used in China plantation nearly 2000 history approximately, is mainly used in medicinal, oil usefulness, spices, aspect such as edible, its leaf (Su Ye), obstruct (caulis perllae), really (perillaseed) all can be used as medicine, soup can be eaten, be done to tender leaf raw, cauline leaf can flood stain.In the last few years, purple perilla became a kind of multi-purpose plant of extremely World Focusing because of its distinctive active substance and nutritive ingredient, and economic worth is very high.States such as Russia, Japan, Korea S, the U.S., Canada have carried out a large amount of commerciality plantations to the Perilla plant, developed edible oil, medicine, flooded tens kinds of purple perilla products such as stain product, makeup.In the prior art, but Shang Weiyou extracts the precedent of cigarette additive from purple perilla, and, learn in the Perilla Leaf residue after aforementioned Perilla Leaf extracts sesame oil according to applicant research and to contain many useful components, all be used as waste disposal and fallen, do not obtain reasonable use as yet.
Summary of the invention
At the above-mentioned deficiency of prior art, the technical problem to be solved in the present invention provides a kind of natural cigarette antioxidant-perilla flavone and preparation method thereof, and perilla flavone is applied to obtain in the cigarette better antioxidation; The inventive method makes as the Perilla Leaf residue after the Perilla Leaf extraction sesame oil of waste material and obtains reasonable use, and it is higher to extract yield.
Technical scheme of the present invention is: natural cigarette with antioxidant-perilla flavone by the preparation of following method and get: after Perilla Leaf extracted residue drying behind the volatile oil, the perilla flavone extracting solution that must extract with vacuum rupture of membranes, immersion, compound enzymatic-alcohol reflux, decompress filter, centrifugal afterwards the making with extra care of low-temperature and high-speed.
Described prozyme is the combination enzyme of food grade solid powdery cellulase, polygalacturonase, proteolytic enzyme.
Described prozyme is made up of following component and umber: cellulase: polygalacturonase: proteolytic enzyme=0.5～2:0.5～2:0.5～2.
Described vacuum rupture of membranes is meant that the residue that Perilla Leaf is extracted behind the volatile oil places vacuum tightness 98% time, vacuumizes 2min, and all standing makes purple perilla cell walls rupture of membranes.
The preparation method of natural antioxidant of perilla flavone for cigarette carries out according to the following steps:
(1) raw material is handled: after will extracting Perilla Leaf residue behind the volatile oil and carrying out drying, the vacuum extractor of packing into vacuum tightness 98% time, vacuumizes 2min, and all standing carries out the vacuum rupture of membranes, makes purple perilla cell walls rupture of membranes, and pulverizing obtains Perilla Leaf residue meal then;
(2) immersion and enzyme are handled: get Perilla Leaf residue meal and put into container, add 0.1～1% prozyme, 5～10 times of water mixings, adjust pHs soak 1h～2h for 4.0～6.0,40 ℃-50 ℃;
(3) extraction is refining: add 3～5 times of 95% ethanol, 80 ℃～90 ℃ constant temperature water bath refluxing extraction 1～2h, water pump vacuumizes decompress filter, be concentrated to original volume 1/4～1/5 after, separate with 8000～11000rpm high speed centrifugation, the gained supernatant liquor is the perilla flavone extracting solution.
Described prozyme is food grade solid powdery cellulase, polygalacturonase, proteolytic enzyme.
Described prozyme is made up of following component and umber: cellulase: polygalacturonase: proteolytic enzyme=0.5～2:0.5～2:0.5～2.
The present invention has the following advantages compared with the prior art: pre-treatment of the present invention has adopted vacuum rupture of membranes and prozyme to handle, destroyed cell wall structure to a greater degree, effective constituent is come out more, reduce the water holdup of filter residue, improve productive rate and reduce extraction cost, and the vacuum rupture of membranes is that physical method, prozyme are treated to biological method, and is all safe, easy.Extract of the present invention does not change the flue gas quality after adding pipe tobacco.Its raw material source of the present invention is extensive, and cost is low, is worth cheap; Method technological process of the present invention is simple, and equipment is simple, and extract can be used as new type natural cigarette antioxidant.
Embodiment
Below relevant technologies problem of the present invention is described in further detail.The perilla flavone extracting solution that the applicant extracts the inventive method compares with the yield of handling directly the perilla flavone extracting solution that extracts with alcohol solvent without rupture of membranes, and the content of flavones is taked determined by ultraviolet spectrophotometry.
1, the preparation of typical curve
Accurately take by weighing rutin standard substance 0.0501g, use 30% dissolve with ethanol, and move into fully in the 500ml volumetric flask, with 30% ethanol constant volume.Get rutin standardized solution 0,1,2,4,6,8,10ml respectively in 7 25ml volumetric flasks, be supplemented to 15ml with 30% ethanol, the Sodium Nitrite 0.7ml of adding 5%, shake up, add 10% aluminum nitrate 0.7ml behind the placement 5min, add 4% sodium hydroxide 5ml behind the 6min again, mixing, to scale, in wavelength 510nm place's colorimetric estimation, blank is a rutin 0ml reference liquid behind the 10min with 30% alcohol dilution.The typical curve regression equation that records absorbance A and concentration C mg/ml is: C=0.10016A, R2=0.99951.
2, the mensuration of flavones content
Spectrophotometry: adopt Sodium Nitrite-aluminum nitrate colorimetry.
Get each 0.2ml of extracting solution respectively in 5 25ml volumetric flasks, be supplemented to 15ml with 30% ethanol, the Sodium Nitrite 0.7ml of adding 5%, shake up, add 10% aluminum nitrate 0.7ml behind the placement 5min, add 4% sodium hydroxide 5ml behind the 6min again, mixing, to scale, in wavelength 510nm place's colorimetric estimation, the record light absorption value is effective 0-1.0 with in behind the 10min with 30% alcohol dilution.
3, test-results
Record perilla flavone extracting solution through vacuum rupture of membranes of the present invention, compound enzymatic-solvent extraction, extract the perilla flavone extracting solution light absorption value of (contrast) with direct solvent after, promptly be the content of flavones by institute's value after the regression equation calculation.Raw material is the Perilla Leaf residue meal 10g behind the extraction volatile oil, and the extracting solution constant volume is to 500ml, and two kinds of method gained flavones contents relatively see Table 1.
The flavones content contrast of table 1 extracting solution
| Sample | Concentration (mg/ml) | Quality (g) | Yield (%) |
| Through vacuum rupture of membranes, compound enzymatic-solvent extraction liquid | 2.0052 | 1.0026 | 10.026％ |
| The direct solvent extracting solution | 1.1521 | 0.5761 | 5.761％ |
Raw material of the present invention is the residue after Perilla Leaf extracts volatile oil, and is cheap.Extracting method of the present invention is than without vacuum rupture of membranes, not enzyme-added direct solvent extracting method, and the yield of the perilla flavone of gained obviously improves, and has improved extraction efficiency, has reduced production cost, and the vacuum rupture of membranes, to add composite enzyme method easy, easy to operate.
The applicant has also carried out the oxidation-resistance of perilla flavone extracting solution and has measured, and measures and takes phenanthroline system hydroxyl radical free radical to remove experiment.
1, gets 1ml 0.75mmol/L phenanthroline ethanol solution adds 2ml, 0.15mol/L successively in test tube phosphate buffered saline buffer (PBS, pH=7.2) and 1ml distilled water, abundant mixing, the 0.75mmol/L copperas solution that adds the new preparation of 1ml, behind the mixing, add 0.01% hydrogen peroxide of the new preparation of 1ml, behind 37 ℃ of heating in water bath 1h, survey light absorption value at 536nm, measured data are light absorption value A0.Replace 1ml 0.01% hydrogen peroxide with 1ml distilled water, working method is same as described above, and the light absorption value A1 in the time of can recording 536nm is blank with A0.Replace 1ml 0.01% hydrogen peroxide with the 1ml sample, working method is same as described above, and the light absorption value A2 in the time of can recording 536nm is blank with A0.
Clearance rate (%)=A2/A1 * 100%
2, perilla flavone extracting solution and xitix (Vc) solution of preparation 0.1,0.125,0.15,0.175,0.20mg/ml, adding phenanthroline hydroxy radical qiao master gives birth in the system, efficient to hydroxyl radical free radical in the perilla flavone extracting solution of different concns and xitix (Vc) the removing system detects, to the clearance rate of hydroxyl radical free radical relatively as table 2.
Table 2 different concns perilla flavone extracting solution and Vc contrast the free radical scavenging of phenanthroline system
The perilla flavone extracting solution that the inventive method obtains with the Perilla Leaf residue, the hydroxyl radical free radical that the phenanthroline system is produced has certain scavenging(action), and when 0.175mg/ml, clearance rate reaches 58.87%; Under same concentrations, perilla flavone extracting solution removing ability of the present invention is 5～10 times of natural antioxidants xitix (Vc), and within the specific limits, along with concentration increases, the removing ability also progressively strengthens.
With perilla flavone extracting solution of the present invention, join in the pipe tobacco by 1%, 0.5%, 0.1% (mass percent), dry and roll into cigarette and (smoke panel test by relevant regulations of the prior art, with Wuhan tobacco Group Co.,Ltd, red certain two class cigarette of gold dragon are contrast, carry out sensory evaluating smoking and smoke gaseous phase free radical and measure.
1, sensory evaluating smoking
Smoke panel test through the military cigarette expert group of smokeing panel test, compare with blank, add Perilla Leaf residue flavone extractive in the pipe tobacco after, do not change the flue gas quality.
2, smoke gaseous phase free radical is measured
Each 20 of cigarette that are averaged Dan Zhichong 0.920g ± 0.02g and average resistance to suction 1.065kPa ± 0.05kPa are as test sample.The test cigarette of preparation is all put into the environment equilibrium water content 48h of climatic chamber in 22 ℃ ± 2 ℃ of temperature and relative humidity 60% ± 2%.Adopt electron spin resonance (ESR) to carry out smoke gaseous phase free radical and detect, the results are shown in Table 3.
The experiment of flue gas free radical is removed in the smoke adding of table 3 Perilla Leaf residue flavone extractive
| Perilla flavone extracting solution consumption (%) | Strength of signal (cm) | Clearance rate (%) |
| 0 | 21.8±3.2 | / |
| 0.1％ | 18.4±2.8 | 15.6％ |
| 0.5％ | 16.9±2.6 | 22.5％ |
| 1％ | 14.3±2.7 | 34.4％ |
Measurement result shows that compared with the control, the cigarette smoke number of free radical that adds the perilla flavone extracting solution has certain reduction; And within the specific limits, along with the increase of perilla flavone extract concentration, clearance rate improves.
The applicant tests the stability of the perilla flavone extracting solution of the inventive method preparation.The experiment of first temperature stability.With content is perilla flavone extracting solution insulation 12h under 90 ℃ of 0.175mg/ml, or behind insulation 24h under 60 ℃, measures its flavones content and phenanthroline system hydroxyl radical free radical clearance rate, the results are shown in Table 4.
Table 4, temperature stability are measured
As seen from the above table, the perilla flavone extracting solution is better through 60 ℃ of insulation 24h rear stabilities, and compares flavones content before the heating and has only slightly reduced 0.02mg/ml, and its phenanthroline system hydroxyl radical free radical clearance rate has reduced by 12.66%; And that the sample result of 90 ℃ of insulation 12h is presented under this temperature thermostability is relatively poor, and flavones content has reduced half, and phenanthroline system hydroxyl radical free radical clearance rate only has an appointment 5%.But in cigarette processing, after flavone extractive added pipe tobacco, the high temperature that runs into only may be in weather, room temperature influence scope, and so also high temperature for a long time when the technology for making tobacco threds perfuming is the cigarette good thermal stability of Perilla Leaf residue flavone extractive.It two is to have carried out pH value of solution gradient stability experiment.The perilla flavone extracting solution that with concentration is 0.175mg/ml is measured flavones content, phenanthroline system hydroxyl radical free radical clearance rate pH2,4,6,8, at 10 o'clock, the results are shown in Table 5.
Table 5, pH value of solution gradient stability
As seen from the above table, the perilla flavone extracting solution, good at pH4～6 scope internal stabilities, its flavones content is constant substantially, and phenanthroline system hydroxyl radical free radical clearance rate is constant substantially.And also slant acidity of the pH value of pipe tobacco, about pH5～6, so the active pH value of perilla flavone extracting solution is fit to cigarette and uses.
The applicant has carried out smoke gaseous phase free radical mensuration
Each 20 of cigarette that are averaged Dan Zhichong 0.920g ± 0.02g and average resistance to suction 1.065kPa ± 0.05kPa are as test sample.The test cigarette of preparation is all put into the environment equilibrium water content 48h of climatic chamber in 22 ℃ ± 2 ℃ of temperature and relative humidity 60% ± 2%.Adopt electron spin resonance (ESR) to carry out smoke gaseous phase free radical and detect, the results are shown in Table 6.
Table 6 adds perilla flavone extracting solution cigarette and removes the experiment of flue gas free radical
| Perilla flavone extracting solution consumption (%) | Strength of signal (cm) | Clearance rate (%) |
| 0 | 21.8+3.2 | / |
| 0.05％ | 20.9+3.0 | 4.1 |
| 0.1％ | 18.4+2.8 | 15.6 |
| 0.5％ | 16.9+2.6 | 22.5 |
Last table measurement result shows, and to compare in the same old way, the cigarette smoke number of free radical that adds the perilla flavone extracting solution has certain reduction; And within the specific limits, along with the increase of extract concentration, clearance rate improves.
Claims (7)
1, a kind of natural cigarette antioxidant-perilla flavone, it is characterized in that by the preparation of following method and get: after Perilla Leaf is extracted residue drying behind the volatile oil, with vacuum rupture of membranes, immersion, compound enzymatic-alcohol reflux, decompress filter, the centrifugal back of low-temperature and high-speed is refining and get the perilla flavone extracting solution.
2, natural cigarette antioxidant-perilla flavone according to claim 1, it is characterized in that: described prozyme is the combination enzyme of food grade solid powdery cellulase, polygalacturonase, proteolytic enzyme.
3, natural cigarette according to claim 1 and 2 is with antioxidant-perilla flavone, it is characterized in that described prozyme is made up of following component and umber: cellulase: polygalacturonase: proteolytic enzyme=0.5～2:0.5～2:0.5～2.
4, natural cigarette according to claim 1 is characterized in that with antioxidant-perilla flavone: described vacuum rupture of membranes is meant that the residue that Perilla Leaf is extracted behind the volatile oil places vacuum tightness 98% time, vacuumizes 2min, and all standing makes purple perilla cell walls rupture of membranes.
5, a kind of preparation method of natural antioxidant of perilla flavone for cigarette is characterized in that described method carries out according to the following steps:
(1) raw material is handled: after will extracting Perilla Leaf residue behind the volatile oil and carrying out drying, the vacuum extractor of packing into vacuum tightness 98% time, vacuumizes 2min, and all standing carries out the vacuum rupture of membranes, makes purple perilla cell walls rupture of membranes, and pulverizing obtains Perilla Leaf residue meal then;
(2) immersion and enzyme are handled: get Perilla Leaf residue meal and put into container, add 0.1～1% prozyme, 5～10 times of water mixings, adjust pHs soak 1h～2h for 4.0～6.0,40 ℃-50 ℃;
(3) extraction is refining: add 3～5 times of 95% ethanol, 80 ℃～90 ℃ constant temperature water bath refluxing extraction 1～2h, water pump vacuumizes decompress filter, be concentrated to original volume 1/4～1/5 after, separate with 8000～11000rpm high speed centrifugation, the gained supernatant liquor is the perilla flavone solution of extraction.
6, the natural cigarette according to claim 5 preparation method of antioxidant-perilla flavone, it is characterized in that: described prozyme is food grade solid powdery cellulase, polygalacturonase, proteolytic enzyme.
7,, it is characterized in that described prozyme is made up of following component and umber: cellulase: polygalacturonase: proteolytic enzyme=0.5～2:0.5～2:0.5～2 according to claim 5 or 6 described natural cigarettes preparation method with antioxidant-perilla flavones.
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