CN104818120A - Cigarette black plum extract and preparation method thereof - Google Patents

Cigarette black plum extract and preparation method thereof Download PDF

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Publication number
CN104818120A
CN104818120A CN201510216631.1A CN201510216631A CN104818120A CN 104818120 A CN104818120 A CN 104818120A CN 201510216631 A CN201510216631 A CN 201510216631A CN 104818120 A CN104818120 A CN 104818120A
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China
Prior art keywords
enzymolysis
extraction
black cloth
cloth woods
cigarette
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CN201510216631.1A
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Chinese (zh)
Inventor
周湘
熊国玺
王娜
王珊
尹团章
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China Tobacco Hunan Industrial Co Ltd
Huanghelou Science and Technology Park Group Co Ltd
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China Tobacco Hunan Industrial Co Ltd
Huanghelou Science and Technology Park Group Co Ltd
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Application filed by China Tobacco Hunan Industrial Co Ltd, Huanghelou Science and Technology Park Group Co Ltd filed Critical China Tobacco Hunan Industrial Co Ltd
Priority to CN201510216631.1A priority Critical patent/CN104818120A/en
Publication of CN104818120A publication Critical patent/CN104818120A/en
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/025Recovery by solvent extraction
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/20Biochemical treatment

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Biochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention discloses a cigarette black plum extract and a preparation method thereof. A process of extracting black plum through cooperation of pectinase enzymolysis and microwave is adopted; the method has the advantages of mild treatment conditions, safety in operation, easy equipment, high extraction efficiency and the like; the prepared special black plum extract has the effects of enriching cigarette flavor, increasing sweetness and fragrance, softening smoke, reducing irritation, increasing mouth sweet aftertaste, improving mouth feeling and reducing residue in cigarette, and is a novel cigarette flavor which is easy and convenient to prepare, is economic and efficient and has a better application effect.

Description

A kind of cigarette black cloth woods extract and preparation method thereof
Technical field
The present invention relates to essence spice for cigarette and preparation method thereof, be specifically related to a kind of cigarette black cloth woods extract and preparation method thereof.
Background technology
Prunus salicina Lindl. Extract is perfume monomer conventional in tobacco, has been widely used in cigarette.Black cloth woods is exactly black plum in fact, belongs to the one of plum.The fruit of black cloth woods contains abundant sugar, VITAMIN, tartaric acid, the nutritive ingredients such as amino acid, and pulp contains total reducing sugar 10.4%, total acid 0.8%, sugar-acid ratio 11.3:1, soluble solid 11.5%.First of black cloth woods is listed in " five fruit ", medical circle is thought, black cloth woods have separate strongly fragrant poison, invigorate blood circulation promote the production of body fluid, effects such as drawing drink, cough-relieving apophlegmatic diuresis, ease constipation of quenching one's thirst.
The extraction to black cloth woods conventional at present mainly adopts traditional reflux extraction.The active substance extraction efficiency of reflux extraction black cloth woods is lower, the extraction efficiency of raw material and solvent can not be fully utilized, cause the wasting of resources, although and the black cloth woods extract obtained have in cigarette enrich cigarette perfume (or spice), increase fragrant and sweet, increase oral cavity and return the effect of sweet sense, also have simultaneously and increase residual, that flue gas is coarse counter productive.
Polygalacturonase can decompose in black cloth woods the most of pectin contained, and produces micromolecular acid, eliminates the pungency of extract to cigarette and the negative impact of mouthfeel, thus soft flue gas, reduce pungency, improve mouthfeel, reduce residual.
Microwave is the hertzian wave of frequency between 300MHZ to 300GHZ, and it has the large fundamental characteristics of fluctuation, high frequency, thermal property and non-thermal property four.Because microwave has penetrativity, thus can certain group effect directly optionally in fragrance matter molecule relevant to sample or molecule, make cell interior temperature increase rapidly, make its cell interior pressure exceed cell wall expansion ability to bear, cell rupture.By the molecule of microwave action or group, the surrounding environment on very fast and vegetable cell and whole sample matrices or its macromole is separated, thus velocity of separation is accelerated and improves extraction yield.Microwave extracting has that equipment is simple, applied widely, extraction efficiency is high, favorable reproducibility, save time, save reagent, pollute the features such as little.At present, except being mainly used in environmental sample pre-treatment, also for fields such as biochemistry, food, technical analysis and natural product extraction.At home, the research that microwave-assisted extraction technique extracts this respect for essence and flavoring agent in herbal medicine and plant is reported also fewer.In microwave extraction Effective Component of Chinese Medicine or plant, the Preliminary Study Results of essence and flavoring agent shows, extraction efficiency is high, and impurity is few, and solvent load is few.Microwave extraction can be widely used in extracts active ingredients: as alkaloids; Anthraquinones; Flavonoid; Saponins; Organic acid; Polyose; Volatile oil; Other: is as steroidal, terpenoid, vegetables oil, spices.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of collaborative technique by enzymolysis process and microwave extraction and prepare cigarette black cloth woods extract and preparation method thereof, improve the yield of black cloth woods total extractives, eliminate the negative impact in pungency and mouthfeel that black cloth woods extract that normal reflux extraction method obtains brings in cigarette simultaneously.
The present invention solves the problems of the technologies described above adopted technical scheme: the preparation method providing a kind of cigarette black cloth woods extract, described preparation method comprises the steps:
(1) black cloth woods is made thick paste solidliquid mixture;
(2) take solidliquid mixture and put into container, add pH value to 2.5 ~ 6.0 of regulator solution after distilled water immersion, the weight ratio of solidliquid mixture and distilled water is 1:5 ~ 1:15;
(3) in solution, polygalacturonase is added, container is placed on temperature be in 45 ~ 55 DEG C of waters bath with thermostatic control stir until enzymolysis complete after filtration, the filtrate obtained after the filter residue after enzymolysis and enzymolysis is for subsequent use, and the addition of polygalacturonase is 0.3 ~ 2% of solidliquid mixture weight;
(4) filter residue after enzymolysis is put into microwave extraction tank, and in extractor, add aqueous ethanolic solution extraction agent carry out microwave extraction;
(5) extracting liquid filtering after microwave extraction obtains the filtrate after extracting, and forms mixing filtrate the merging of the filtrate after extraction and the filtrate after enzymolysis, and mixing filtrate reduced in volume to relative density is 1.20 ~ 1.35 obtain black cloth woods extract.
Further, the stirring detailed process in described step (2) is: stirred once every 5 ~ 10 minutes, stir 4 ~ 6 minutes, enzymolysis 2 ~ 3h is until enzymolysis completes at every turn.
Further, adding the detailed process that aqueous ethanolic solution extraction agent carries out microwave extraction in described step (4) is: in microwave extraction tank, add the aqueous ethanolic solution extraction agent that mass percentage concentration is 70%, and the weight ratio of filter residue after aqueous ethanolic solution extraction agent and described enzymolysis is 1:5 ~ 1:12, carry out microwave extraction, extraction time is 0.25 ~ 1h, then repeat to extract once, extraction time is 0.25 ~ 1h.
Further, the extracting liquid filtering in described step (5) after microwave extraction is specially: by extracting solution filtering with microporous membrane.
Further, the addition of described polygalacturonase is 0.5 ~ 1.5% of solidliquid mixture weight.
Further, described pH value is adjusted to 3.0 ~ 4.0, can ensure that the activity of polygalacturonase is higher.
Also provide a kind of cigarette black cloth woods extract, described cigarette black cloth woods extract is cigarette black cloth woods extract prepared by preparation method described above.
The present invention has following characteristics: pectinase enzymatic hydrolysis provided by the invention works in coordination with the technique of microwave extraction black cloth woods, has that treatment condition gentleness, operational safety, equipment are simple, extraction efficiency advantages of higher; Eliminate the negative impact in pungency and mouthfeel that black cloth woods extract that normal reflux extraction method obtains brings in cigarette simultaneously, the black cloth woods extract prepared its have in cigarette and enrich cigarette perfume (or spice), increase fragrant and sweet, soft flue gas, reduce pungency, increase oral cavity and return sweet sense, improve mouthfeel, reduce residual effect, be that one prepares easy, the good Novel tobacco perfume material of economical and efficient, effect.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
Embodiment 1
Black cloth woods is shredded, is squeezed into thick paste solidliquid mixture with juice extractor.Take solidliquid mixture 1kg, add 10kg distilled water, after soaking 60 min, add acid-base buffer, regulate the pH value of the aqueous solution, pH value is adjusted to 2.5, then the polygalacturonase that weight is solidliquid mixture 0.3% is added, be placed in water bath with thermostatic control and carry out enzymolysis, the temperature of water-bath is set as 45 DEG C, and in enzymolysis process, every 8min stirs once, each stirring 6min, ensure that polygalacturonase can fully be distributed in solidliquid mixture, by the continuous enzymolysis of pectin in black cloth woods pulp, enzymolysis time is that 2.5h is until enzymolysis completes.After enzymolysis completes, suction filtration obtains the filtrate after enzymolysis and the filter residue after enzymolysis, in order to follow-up use.
Filter residue after enzymolysis is put into microwave extraction tank, add the aqueous ethanolic solution extraction agent that mass percentage concentration is 70%, the weight ratio of the filter residue after aqueous ethanolic solution extraction agent and enzymolysis is 1:5, and select power to be that 30KW, for the first time extraction electric machine frequency are 12HZ, second time extraction electric machine frequency is 15HZ, carry out microwave extraction, extract twice each 0.25h.
Extracting solution after microwave extraction 0.8 μm of filtering with microporous membrane, forms mixing filtrate the merging of the filtrate after extraction and the filtrate after enzymolysis, and mixing filtrate reduced in volume to relative density is 1.20 obtain black cloth woods extract.
After enzymolysis, the black cloth woods extract of microwave extraction comparatively only improves 30% by the efficiency of the aqueous ethanolic solution extraction of 70%.
Embodiment 2
Black cloth woods is shredded, is squeezed into thick paste solidliquid mixture with juice extractor.Take solidliquid mixture 1kg, add 10kg distilled water, after soaking 60 min, add acid-base buffer, regulate the pH value of the aqueous solution, pH value is adjusted to 3.5, then the polygalacturonase that weight is solidliquid mixture 0.5% is added, be placed in water bath with thermostatic control and carry out enzymolysis, the temperature of water-bath is set as 45 DEG C, and in enzymolysis process, every 10min stirs once, each stirring 5min, ensure that polygalacturonase can fully be distributed in solidliquid mixture, by the continuous enzymolysis of pectin in black cloth woods pulp, enzymolysis time is that 2h is until enzymolysis completes.After enzymolysis completes, suction filtration obtains the filtrate after enzymolysis and the filter residue after enzymolysis, in order to follow-up use.
Filter residue after enzymolysis is put into microwave extraction tank, add the aqueous ethanolic solution extraction agent that mass percentage concentration is 70%, the weight ratio of the filter residue after aqueous ethanolic solution extraction agent and enzymolysis is 1:8, and select power to be that 30KW, for the first time extraction electric machine frequency are 12HZ, second time extraction electric machine frequency is 15HZ, carry out microwave extraction, extract twice each 0.5h.
Extracting solution after microwave extraction 0.8 μm of filtering with microporous membrane, forms mixing filtrate the merging of the filtrate after extraction and the filtrate after enzymolysis, and mixing filtrate reduced in volume to relative density is 1.20 obtain black cloth woods extract.
After enzymolysis, the black cloth woods extract of microwave extraction comparatively only improves 30% by the efficiency of the aqueous ethanolic solution extraction of 70%.
Embodiment 3
Black cloth woods is shredded, is squeezed into thick paste solidliquid mixture with juice extractor.Take solidliquid mixture 1kg, add 10kg distilled water, after soaking 60 min, add acid-base buffer, regulate the pH value of the aqueous solution, pH value is adjusted to 4.0, then the polygalacturonase that weight is solidliquid mixture 1.5% is added, be placed in water bath with thermostatic control and carry out enzymolysis, the temperature of water-bath is set as 50 DEG C, and in enzymolysis process, every 10min stirs once, each stirring 4min, ensure that polygalacturonase can fully be distributed in black cloth woods solidliquid mixture, by the continuous enzymolysis of pectin in black cloth woods pulp, enzymolysis time is that 3h is until enzymolysis completes.After enzymolysis completes, suction filtration obtains the filtrate after enzymolysis and the filter residue after enzymolysis, in order to follow-up use.
Filter residue after enzymolysis is put into microwave extraction tank, add the aqueous ethanolic solution extraction agent of mass percentage concentration 70%, the weight ratio of the filter residue after aqueous ethanolic solution extraction agent and enzymolysis is 1:10, and select power to be that 30KW, for the first time extraction electric machine frequency are 12HZ, second time extraction electric machine frequency is 15HZ, carry out microwave extraction, extract twice each 0.5h.
Extracting solution after microwave extraction 0.8 μm of filtering with microporous membrane, forms mixing filtrate the merging of the filtrate after extraction and the filtrate after enzymolysis, is 1.20 obtain black cloth woods extract to relative density after mixing filtrate reduced in volume.
After enzymolysis, the black cloth woods extract of microwave extraction comparatively only improves 40% by the efficiency of the aqueous ethanolic solution extraction of 70%.
Embodiment 4
Black cloth woods is shredded, is squeezed into thick paste solidliquid mixture with juice extractor.Take solidliquid mixture 1kg, add 10kg distilled water, after soaking 60 min, add acid-base buffer, regulate the pH value of the aqueous solution, pH value is adjusted to 3.0, then the polygalacturonase that weight is solidliquid mixture 1.0% is added, be placed in water bath with thermostatic control and carry out enzymolysis, the temperature of water-bath is set as 50 DEG C, and in enzymolysis process, every 10min stirs once, each stirring 5min, ensure that polygalacturonase can fully be distributed in black cloth woods solidliquid mixture, by the continuous enzymolysis of pectin in black cloth woods pulp, enzymolysis time is that 2h is until enzymolysis completes.After enzymolysis completes, suction filtration obtains the filtrate after enzymolysis and the filter residue after enzymolysis, in order to follow-up use.
Filter residue after enzymolysis is put into microwave extraction tank, add the aqueous ethanolic solution extraction agent of mass percentage concentration 70%, the weight ratio of the filter residue after aqueous ethanolic solution extraction agent and enzymolysis is 1:8, and select power to be that 30KW, for the first time extraction electric machine frequency are 12HZ, second time extraction electric machine frequency is 15HZ, carry out microwave extraction, extract twice each 0.5h.
Extracting solution after microwave extraction 0.8 μm of filtering with microporous membrane, forms mixing filtrate the merging of the filtrate after extraction and the filtrate after enzymolysis, is 1.20 obtain black cloth woods extract to relative density after mixing filtrate reduced in volume.
After enzymolysis, the black cloth woods extract of microwave extraction comparatively only improves 40% by the efficiency of the aqueous ethanolic solution extraction of 70%.
Embodiment 5
Black cloth woods is shredded, is squeezed into thick paste solidliquid mixture with juice extractor.Take solidliquid mixture 1kg, add 10kg distilled water, after soaking 60 min, add acid-base buffer, regulate the pH value of the aqueous solution, pH value is adjusted to 6.0, then the polygalacturonase that weight is solidliquid mixture 2.0% is added, be placed in water bath with thermostatic control and carry out enzymolysis, the temperature of water-bath is set as 55 DEG C, and in enzymolysis process, every 5min stirs once, each stirring 6min, ensure that polygalacturonase can fully be distributed in black cloth woods solidliquid mixture, by the continuous enzymolysis of pectin in black cloth woods pulp, enzymolysis time is that 3h is until enzymolysis completes.After enzymolysis completes, suction filtration obtains the filtrate after enzymolysis and the filter residue after enzymolysis, in order to follow-up use.
Filter residue after enzymolysis is put into microwave extraction tank, add the aqueous ethanolic solution of mass percentage concentration 70%, the weight ratio of the filter residue after aqueous ethanolic solution extraction agent and enzymolysis is 1:12, and select power to be that 30KW, for the first time extraction electric machine frequency are 12HZ, second time extraction electric machine frequency is 15HZ, carry out microwave extraction, extract twice each 1.0h.
Extracting solution after microwave extraction 0.8 μm of filtering with microporous membrane, forms mixing filtrate the merging of the filtrate after extraction and the filtrate after enzymolysis, is 1.25 obtain black cloth woods extract to relative density after mixing filtrate reduced in volume.
After enzymolysis, the black cloth woods extract of microwave extraction comparatively only improves 45% by the efficiency of the aqueous ethanolic solution extraction of 70%.
Embodiment 6
Black cloth woods is shredded, is squeezed into thick paste solidliquid mixture with juice extractor.Take solidliquid mixture 1kg, add 10kg distilled water, after soaking 60 min, add acid-base buffer, regulate the pH value of the aqueous solution, pH value is adjusted to 4.0, then the polygalacturonase that weight is solidliquid mixture 1.5% is added, be placed in water bath with thermostatic control and carry out enzymolysis, the temperature of water-bath is set as 55 DEG C, and in enzymolysis process, every 10min stirs once, each stirring 5min, ensure that polygalacturonase can fully be distributed in black cloth woods solidliquid mixture, by the continuous enzymolysis of pectin in black cloth woods pulp, enzymolysis time is that 2h is until enzymolysis completes.After enzymolysis completes, suction filtration obtains the filtrate after enzymolysis and the filter residue after enzymolysis, in order to follow-up use.
Filter residue after enzymolysis is put into microwave extraction tank, add the aqueous ethanolic solution of mass percentage concentration 70%, the weight ratio of the filter residue after aqueous ethanolic solution extraction agent and enzymolysis is 1:8, and select power to be that 30KW, for the first time extraction electric machine frequency are 12HZ, second time extraction electric machine frequency is 15HZ, carry out microwave extraction, extract twice each 1.0h.
Extracting solution after microwave extraction 0.8 μm of filtering with microporous membrane, forms mixing filtrate the merging of the filtrate after extraction and the filtrate after enzymolysis, is 1.25 obtain black cloth woods extract to relative density after mixing filtrate reduced in volume.
After enzymolysis, the black cloth woods extract of microwave extraction comparatively only improves 45% by the efficiency of the aqueous ethanolic solution extraction of 70%.
The above; be only the specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, anyly belongs to those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.

Claims (7)

1. a cigarette preparation method for black cloth woods extract, is characterized in that: described preparation method comprises the steps:
(1) black cloth woods is made thick paste solidliquid mixture;
(2) take solidliquid mixture and put into container, add pH value to 2.5 ~ 6.0 of regulator solution after distilled water immersion, the weight ratio of solidliquid mixture and distilled water is 1:5 ~ 1:15;
(3) in solution, polygalacturonase is added, container is placed on temperature be in 45 ~ 55 DEG C of waters bath with thermostatic control stir until enzymolysis complete after filtration, the filtrate obtained after the filter residue after enzymolysis and enzymolysis is for subsequent use, and the addition of polygalacturonase is 0.3 ~ 2% of solidliquid mixture weight;
(4) filter residue after enzymolysis is put into microwave extraction tank, and in extractor, add aqueous ethanolic solution extraction agent carry out microwave extraction;
(5) extracting liquid filtering after microwave extraction obtains the filtrate after extracting, and forms mixing filtrate the merging of the filtrate after extraction and the filtrate after enzymolysis, and mixing filtrate reduced in volume to relative density is 1.20 ~ 1.35 obtain black cloth woods extract.
2. the preparation method of cigarette black cloth woods extract according to claim 1, it is characterized in that: the stirring detailed process in described step (2) is: stirred once every 5 ~ 10 minutes, each stirring 4 ~ 6 minutes, enzymolysis 2 ~ 3h is until enzymolysis completes.
3. the preparation method of cigarette black cloth woods extract according to claim 1, it is characterized in that: adding the detailed process that aqueous ethanolic solution extraction agent carries out microwave extraction in described step (4) is: in microwave extraction tank, add the aqueous ethanolic solution extraction agent that mass percentage concentration is 70%, and the weight ratio of filter residue after aqueous ethanolic solution extraction agent and described enzymolysis is 1:5 ~ 1:12, carry out microwave extraction, extraction time is 0.25 ~ 1h, then repeat to extract once, extraction time is 0.25 ~ 1h.
4. the preparation method of cigarette black cloth woods extract according to claim 1, is characterized in that: the extracting liquid filtering in described step (5) after microwave extraction is specially: by extracting solution filtering with microporous membrane.
5. the preparation method of cigarette black cloth woods extract according to claim 1, is characterized in that: the addition of described polygalacturonase is 0.5 ~ 1.5% of solidliquid mixture weight.
6. the preparation method of cigarette black cloth woods extract according to claim 1, is characterized in that: described pH value is adjusted to 3.0 ~ 4.0.
7. a cigarette black cloth woods extract, is characterized in that: the cigarette black cloth woods extract that described cigarette black cloth woods extract is prepared for the preparation method as described in as arbitrary in claim 1 ~ 6 one.
CN201510216631.1A 2015-04-29 2015-04-29 Cigarette black plum extract and preparation method thereof Pending CN104818120A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105146741A (en) * 2015-08-26 2015-12-16 江西中烟工业有限责任公司 Natural herbal enzymatic hydrolyte liquid, preparation method thereof and application thereof in cigarettes
CN106701325A (en) * 2017-03-08 2017-05-24 湖北中烟工业有限责任公司 Apricot extract for tobaccos and preparation method of apricot extract
CN108004023A (en) * 2017-12-14 2018-05-08 江西中烟工业有限责任公司 Iris extract and its application in cigarette

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105146741A (en) * 2015-08-26 2015-12-16 江西中烟工业有限责任公司 Natural herbal enzymatic hydrolyte liquid, preparation method thereof and application thereof in cigarettes
CN106701325A (en) * 2017-03-08 2017-05-24 湖北中烟工业有限责任公司 Apricot extract for tobaccos and preparation method of apricot extract
CN108004023A (en) * 2017-12-14 2018-05-08 江西中烟工业有限责任公司 Iris extract and its application in cigarette
CN108004023B (en) * 2017-12-14 2021-04-16 江西中烟工业有限责任公司 Iris extract and application thereof in cigarettes

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Application publication date: 20150805