CN106167739A - A kind of containing doing the microcapsule of extract of Folium Camelliae sinensis, Preparation Method And The Use - Google Patents
A kind of containing doing the microcapsule of extract of Folium Camelliae sinensis, Preparation Method And The Use Download PDFInfo
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- CN106167739A CN106167739A CN201610608937.6A CN201610608937A CN106167739A CN 106167739 A CN106167739 A CN 106167739A CN 201610608937 A CN201610608937 A CN 201610608937A CN 106167739 A CN106167739 A CN 106167739A
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- CN
- China
- Prior art keywords
- folium camelliae
- camelliae sinensis
- microcapsule
- extract
- sinensis
- Prior art date
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, 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
- C11B9/00—Essential oils; Perfumes
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/281—Treatment of tobacco products or tobacco substitutes by chemical substances the action of the chemical substances being delayed
- A24B15/283—Treatment of tobacco products or tobacco substitutes by chemical substances the action of the chemical substances being delayed by encapsulation of the chemical substances
- A24B15/284—Treatment of tobacco products or tobacco substitutes by chemical substances the action of the chemical substances being delayed by encapsulation of the chemical substances the additive being bound to a host by chemical, electrical or like forces, e.g. use of precursors, inclusion complexes
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
- A24B15/302—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
- A24B15/303—Plant extracts other than tobacco
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/06—Use of materials for tobacco smoke filters
- A24D3/061—Use of materials for tobacco smoke filters containing additives entrapped within capsules, sponge-like material or the like, for further release upon smoking
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/06—Use of materials for tobacco smoke filters
- A24D3/08—Use of materials for tobacco smoke filters of organic materials as carrier or major constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
- B01J13/043—Drying and spraying
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, 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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, 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
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, 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
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
Abstract
The present invention relates to Nicotiana tabacum L. and essence field, relate to a kind of containing doing the microcapsule of extract of Folium Camelliae sinensis, Preparation Method And The Use.The invention still further relates to the filter stick containing described microcapsule and tobacco product, such as Medicated cigarette and chewing tobacco.The invention still further relates to the extract doing Folium Camelliae sinensis for preparing the purposes of microcapsule, such as, described microcapsule is used for preparing tobacco product.
Description
Technical field
The present invention relates to Nicotiana tabacum L. and essence field, in particular it relates to containing the microcapsule of the extract doing Folium Camelliae sinensis, system
The method of standby described microcapsule, and contain filter stick and the tobacco product, such as Medicated cigarette and chewing tobacco of described microcapsule；The present invention is also
Relate to the extract doing Folium Camelliae sinensis for preparing the purposes of microcapsule, it is preferable that described microcapsule is used for preparing filter stick and Nicotiana tabacum L. system
Product.
Background technology
In the making of oolong tea, including doing this technique blue or green.Doing the blue or green stage, Folium Camelliae sinensis blade is acted on by mechanical force,
Leaf margin cell sustains damage, and promotes polyphenol compound to aoxidize, is polymerized, and produces coloring matter, and promotes aroma substance
Formed.Doing young worker's skill and generally include rocking of green leaf and airing, rocking of green leaf refers to by hand or machine, makes Folium Camelliae sinensis carry out circumference in a reservoir
Moving and stir up and down, airing refers to stand the Folium Camelliae sinensis through rocking of green leaf.Doing in young worker's skill, rocking of green leaf and airing generally replace
Carry out.Do the intermediate product that young worker's skill obtains to be referred to as doing Folium Camelliae sinensis.
In prior art, had the essence made with finished product tea extract for raw material, but, this area need nonetheless remain for
The tea extract essence that the aromatic style of above-mentioned essence is different.
Additionally, similar to the characteristic of other natural plant extracts, tea extract there is also that volatility is relatively strong, hold fragrant ability
Shortcoming more weak, the most easily-storied, these shortcomings make the application of tea extract be restricted.
Summary of the invention
The present inventor passes through in-depth study and performing creative labour, it has surprisingly been found that do the extract of Folium Camelliae sinensis relative to
Finished product tea extract, not only the yield of aroma substance is higher, and aromatic style has tea perfume and the fragrance of a flower concurrently, and odor type is pleasant especially.
Do the extract of Folium Camelliae sinensis and there is elegant sweet, feature that breath is pleasant, close with the product feature that high-grade cigarette is pursued.
The present inventor utilizes the extract doing Folium Camelliae sinensis to make microcapsule, and described microcapsule is put on tobacco product (example
Such as Medicated cigarette) in.Surprisingly, it was found that the microcapsule containing the extract doing Folium Camelliae sinensis can give tobacco product and do Folium Camelliae sinensis
Characteristic perfume, and the releasing effect of described fragrance can be controlled, significantly improve the aroma quality of tobacco product, thus provide
Following invention:
In one aspect, the invention provides a kind of microcapsule, it contains the extract doing Folium Camelliae sinensis.
In one embodiment of the invention, do described in the extract of Folium Camelliae sinensis selected from do Folium Camelliae sinensis hydrosol, do Folium Camelliae sinensis quintessence oil,
Do Folium Camelliae sinensis absolute oil, do Folium Camelliae sinensis tincture and do in Folium Camelliae sinensis extractum one or more.
In one embodiment of the invention, do Folium Camelliae sinensis hydrosol described in be prepared by the method comprised the steps of:
Step (1): do Folium Camelliae sinensis with vapor distillation, obtain distillation；
Optionally, described method is further comprising the steps of:
Step (2): distillation is carried out microfiltration, obtains microfiltration permeate；And/or
Step (3): microfiltration permeate is concentrated.
In one embodiment of the invention, in step (1), in still-process, the temperature of steam is 102 DEG C～110
DEG C, such as 102 DEG C～105 DEG C or 105 DEG C～110 DEG C.
In one embodiment of the invention, in step (1), the time of distillation is 1～3h, such as 1～2h, 2～
2.5h or 2.5～3h.
In one embodiment of the invention, in step (2), micro-filtration membrane is used to carry out microfiltration.
In one embodiment of the invention, the aperture of micro-filtration membrane is 0.05～1 μm, such as 0.05～0.2 μm, 0.2
～0.5 μm or 0.5～1 μm.
In one embodiment of the invention, in step (3), reverse osmosis membrane is used to concentrate.
In one embodiment of the invention, in step (3), the film pressure that goes out using reverse osmosis membrane to carry out concentrating is
0.8～1.5MPa, such as 0.8～1.2MPa or 1.2～1.5MPa.
In one embodiment of the invention, do Folium Camelliae sinensis quintessence oil described in be prepared by the method comprised the steps of:
Step (1): do Folium Camelliae sinensis with vapor distillation, collects distillation, obtains doing Folium Camelliae sinensis hydrosol；With
Step (2): do to isolate Folium Camelliae sinensis hydrosol do Folium Camelliae sinensis quintessence oil from what step (1) obtained；
Optionally, step (1) includes distillation is carried out microfiltration and/or concentration.
In one embodiment of the invention, the separation in described step (2) is realized by extraction.
In one embodiment of the invention, step (2) includes following operation: add saturated food in Folium Camelliae sinensis quintessence oil to doing
Saline, adds organic solvent (such as ethyl acetate) and extracts.
In one embodiment of the invention, step (2) includes concentrating extraction product.
In one embodiment of the invention, step (2) includes following operation: extraction product step (1) obtained
Carry out being evaporated near doing for the first time, add organic solvent (such as dehydrated alcohol) and carry out second time concentrating under reduced pressure.
In one embodiment of the invention, the temperature of described first time concentrating under reduced pressure is 35 DEG C～40 DEG C, such as 35
DEG C～37.5 DEG C or 37.5 DEG C～40 DEG C.
In one embodiment of the invention, the vacuum of described first time concentrating under reduced pressure is 200～230mbar, example
Such as 200～210mbar, 210～220mbar or 220～230mbar.
In one embodiment of the invention, the temperature of described second time concentrating under reduced pressure 40 DEG C～45 DEG C, such as 40 DEG C
～42.5 DEG C or 42.5 DEG C～45 DEG C.
In one embodiment of the invention, the vacuum of described second time concentrating under reduced pressure is 110～130mbar, example
Such as 110～120mbar or 120～130mbar.
In one embodiment of the invention, do Folium Camelliae sinensis quintessence oil described in relative to the yield doing Folium Camelliae sinensis be 0.14～
0.18‰。
In one embodiment of the invention, do Folium Camelliae sinensis tincture described in be prepared by the method comprised the steps of:
Step (1): in a heated state, uses organic solvent (such as ethanol or ethanol solution) to reflux to doing Folium Camelliae sinensis
Extract；
Step (2): the extracting solution obtaining step (1) concentrates.
In one embodiment of the invention, in step (1), the temperature of reflux, extract, is 60 DEG C～70 DEG C, such as 60
DEG C～65 DEG C or 65 DEG C～70 DEG C.
In one embodiment of the invention, being concentrated at 45 DEG C～55 DEG C of step (2) is carried out, such as 45 DEG C～50
DEG C or 50 DEG C～55 DEG C.
In one embodiment of the invention, the concentration of step (2) is carried out at reduced pressure conditions.
In one embodiment of the invention, the vacuum that is concentrated in of step (2) is to enter under conditions of 40～60mbar
OK, such as 40～50mbar or 50～60mbar.
In one embodiment of the invention, the density doing Folium Camelliae sinensis tincture described in is 1.05～1.10g/cm3, such as 1.05
～1.08g/cm3Or 1.08～1.10g/cm3。
In one embodiment of the invention, described in do the yield of Folium Camelliae sinensis tincture be 10%～15%, such as 10%～
12% or 12%～15%.
In one embodiment of the invention, doing Folium Camelliae sinensis extractum described in is to be condensed into paste and prepare by will do Folium Camelliae sinensis tincture
's.
In one embodiment of the invention, described in be concentrated at 45 DEG C～55 DEG C and carry out, such as 45 DEG C～50 DEG C or
50 DEG C～55 DEG C.
In one embodiment of the invention, described concentration is carried out at reduced pressure conditions.
In one embodiment of the invention, described in be concentrated in vacuum be to carry out under conditions of 40～60mbar, example
Such as 40～50mbar or 50～60mbar.
In one embodiment of the invention, the density doing Folium Camelliae sinensis extractum described in is 1.2 ± 0.02g/cm3。
In one embodiment of the invention, do Folium Camelliae sinensis absolute oil described in be prepared by the method comprised the steps of:
Step (1): do Folium Camelliae sinensis extractum with ethanol extraction, be extracted liquid；
Step (2): extract is carried out freezing, is filtered to remove the material insoluble in ethanol；
Step (3): filtrate distilled at reduced pressure conditions, removes ethanol.
In one embodiment of the invention, the extraction in step (1) carries out one or many, such as 2 times, 3 times, 4
Secondary, 5 times or 6 times.
In one embodiment of the invention, being chilled at-15 DEG C in step (2) is carried out.
In one embodiment of the invention, in step (2), freezing carries out 36 hours.
In one embodiment of the invention, in step (2), the method for microfiltration is used to remove the thing insoluble in ethanol
Matter；It is highly preferred that the micro-filtration membrane using aperture to be 1～100nm (such as 1nm, 50nm or 100nm) carries out microfiltration.
In one embodiment of the invention, the decompression distillation of step (3) is in the condition that vacuum is 40～60mbar
Under carry out, such as 40～50mbar or 50～60mbar.
In one embodiment of the invention, Folium Camelliae sinensis is done described in the tea fresh leaves of oolong tea Camellia sinensis and/or the blade that withers
For raw material.
In one embodiment of the invention, described oolong tea Camellia sinensis is Tie Guanyin tea plant and/or Wuyi cliff tea Camellia sinensis.
In one embodiment of the invention, described Wuyi cliff tea Camellia sinensis is selected from Radix Campylotropis Hirtella (Herba Myrsines Africanae) Camellia sinensis, bright fir Camellia sinensis, narcissus
Camellia sinensis, Cortex Cinnamomi Camellia sinensis and one or more planted in Camellia sinensis strange.
In one embodiment of the invention, Folium Camelliae sinensis is done described in the spring tea of oolong tea Camellia sinensis and/or autumn tea as raw material.
In one embodiment of the invention, do Folium Camelliae sinensis described in be prepared by the method comprised the following steps: fresh to tea
Leaf or the blade that withers carry out one or multi-step rocking of green leaf process, and one or multi-step airing processes.
In one embodiment of the invention, the moisture content doing Folium Camelliae sinensis described in is 60～70%.
In one embodiment of the invention, described microcapsule is possibly together with one or more in following material: benzene second
Ketone, linalool, phenethanol, dihydro jasmone, MDJ, caryophyllene oxide, β-caryophyllenol, β-Tujue's alkene
Ketone, oxidation isophorone, alpha, beta-lonone, dihydroactinidiolide, aglaia odorata flower concrete, yunyan extract, Oleum Pelargonii Graveolentis, Fructus Anisi Stellati
Aldehyde, Megastigmatrienone, vanillin, ethyl vanillin, maltol, ethylmaltol, furanone, 2,3,5-trimethylpyrazine and 2-
Acetyl group pyrazine.
In one embodiment of the invention, described microcapsule is possibly together with one or more in following material: benzene second
Ketone, linalool, phenethanol, dihydro jasmone, MDJ, caryophyllene oxide, β-caryophyllenol, β-Tujue's alkene
Ketone, oxidation isophorone, alpha, beta-lonone, dihydroactinidiolide, aglaia odorata flower concrete and yunyan extract.
In one embodiment of the invention, described microcapsule is possibly together with one or more in following material: benzene second
Ketone, linalool, phenethanol, Oleum Pelargonii Graveolentis, MDJ, anisic aldehyde, β-caryophyllenol, β-Damascenone, huge bean
Three ketenes, alpha, beta-lonone, dihydroactinidiolide, aglaia odorata flower concrete, vanillin, ethyl vanillin, maltol, ethyl Fructus Hordei Germinatus
Phenol, furanone, 2,3,5-trimethylpyrazine, 2-acetyl group pyrazine and yunyan extract.
In one embodiment of the invention, the particle diameter of described microcapsule is 1～25 μm, such as 1～5 μm, 5～10 μ
M, 10～15 μm, 15～20 μm or 20～25 μm.
In one embodiment of the invention, described microcapsule is possibly together with sodium alginate, gelatin, dextrin and optional
Toner.
In one embodiment of the invention, described coloring agent is food grade colorant.An enforcement in the present invention
In scheme, described coloring agent is water-soluble colorant.In one embodiment of the invention, described coloring agent is food stage water
Soluble dye.In one embodiment of the invention, described coloring agent is lemon yellow.In one embodiment of the invention
In, described coloring agent is light blue.
In one embodiment of the invention, described microcapsule is used for preparing tobacco product, such as Medicated cigarette or chewing tobacco.
In one aspect, the invention provides the method preparing described microcapsule, it comprises the following steps:
Step 1: following components is mixed, obtains solution A:
The extract doing Folium Camelliae sinensis (such as does Folium Camelliae sinensis hydrosol, does Folium Camelliae sinensis quintessence oil, does Folium Camelliae sinensis tincture, do Folium Camelliae sinensis absolute oil and/or do green grass or young crops
Tea extract), or comprise do Folium Camelliae sinensis extract (such as do Folium Camelliae sinensis hydrosol, do Folium Camelliae sinensis quintessence oil, do Folium Camelliae sinensis tincture, do Folium Camelliae sinensis absolute oil and/
Or do Folium Camelliae sinensis extractum) essence combination,
The aqueous solution of sodium alginate,
Gelatin,
Dextrin, and
Optional coloring agent；
Step 2: solution A is spray-dried.
In one embodiment of the invention, step 1 is: will do Folium Camelliae sinensis extract, sodium alginate aqueous solution, gelatin,
Dextrin and the mixing of optional coloring agent, obtain solution A.
In one embodiment of the invention, step 1 is: will comprise the essence combination of the extract doing Folium Camelliae sinensis, sea
Sodium alginate aqueous solution, gelatin, dextrin and the mixing of optional coloring agent, obtain solution A.
In one embodiment of the invention, in described essence combination, the content of the extract doing Folium Camelliae sinensis is
3.00%～10.00%, such as 3.00%～5.00%, 5.00%～7.00%, 7.00%～9.00% or 9.00%～
10.00%, such as 3.00%, 4.00%, 5.00%, 6.00%, 7.00%, 8.00%, 9.00% or 10.00%.
In one embodiment of the invention, described essence combination is possibly together with one or more in following material:
1-Phenylethanone., linalool, phenethanol, dihydro jasmone, MDJ, caryophyllene oxide, β-caryophyllenol, β-Tujue
Ketenes, oxidation isophorone, alpha, beta-lonone, dihydroactinidiolide, aglaia odorata flower concrete, yunyan extract, Oleum Pelargonii Graveolentis, Fructus Anisi Stellati
Aldehyde, Megastigmatrienone, vanillin, ethyl vanillin, maltol, ethylmaltol, furanone, 2,3,5-trimethylpyrazine and 2-
Acetyl group pyrazine.
In one embodiment of the invention, described essence combination is possibly together with one or more in following material:
1-Phenylethanone., linalool, phenethanol, dihydro jasmone, MDJ, caryophyllene oxide, β-caryophyllenol, β-Tujue
Ketenes, oxidation isophorone, alpha, beta-lonone, dihydroactinidiolide, aglaia odorata flower concrete and yunyan extract.
In one embodiment of the invention, described essence combination is possibly together with one or more in following material:
1-Phenylethanone., linalool, phenethanol, Oleum Pelargonii Graveolentis, MDJ, anisic aldehyde, β-caryophyllenol, β-Damascenone,
Megastigmatrienone, alpha, beta-lonone, dihydroactinidiolide, aglaia odorata flower concrete, vanillin, ethyl vanillin, maltol, ethyl
Maltol, furanone, 2,3,5-trimethylpyrazine, 2-acetyl group pyrazine and yunyan extract.
In one embodiment of the invention, described essence combination be by have following proportioning component mix after
Obtain: do the extract 3.00%～10.00% of Folium Camelliae sinensis, 1-Phenylethanone. 0.10%～3.00%, linalool 0.10%～
3.00%, phenethanol 0.10%～3.00%, dihydro jasmone 0.10%～3.00%, MDJ 0.10%～
3.00%, caryophyllene oxide 0.10%～3.00%, β-caryophyllenol 0.10%～3.00%, β-Damascenone 0.10%～
3.00%, oxidation isophorone 0.10%～3.00%, alpha, beta-lonone 0.10%～3.00%, dihydroactinidiolide
0.10%～3.00%, aglaia odorata flower concrete 0.10%～3.00%, yunyan extract 0.10%～3.00%, remaining is the second of 70%
Alcohol-water solution.
In one embodiment of the invention, described essence combination comprises do Folium Camelliae sinensis extractum 3.50%～
4.55%, do Folium Camelliae sinensis quintessence oil 1.00%～1.50%, do Folium Camelliae sinensis absolute oil 1.50%～2.15% and do Folium Camelliae sinensis tincture 1.00%～
5.00%.
Percentage composition (%) in the present invention is weight/mass percentage composition.
In one embodiment of the invention, the extract of Folium Camelliae sinensis and the quality of sodium alginate are done described in: mol ratio is
0.03～2g:5～50 μm ol, such as 0.03～0.06g:5～50 μm ol, 0.06～0.1g:5～50 μm ol, 0.1～0.6g:5
～50 μm ol, 0.6～2g:5～50 μm ol, 0.03～2g:5～20 μm ol, 0.03～2g:20～40 μm ol or 0.03～2g:
40～50 μm ol.
In one embodiment of the invention, the quality of described essence combination and sodium alginate: mol ratio be 1～
20g:5～50 μm ol, such as 1～2g:5～50 μm ol, 1～5g:5～50 μm ol, 5～10g:5～50 μm ol, 10～20g:5
～50 μm ol, 1～20g:5～20 μm ol, 1～20g:20～40 μm ol or 1～20g:40～50 μm ol.
In one embodiment of the invention, the number-average molecular weight of described sodium alginate is 32,000～250,000.
In one embodiment of the invention, the concentration of the aqueous solution of described sodium alginate is 5～50 μm ol/L, such as
5～15 μm ol/L, 15～25 μm ol/L, 25～35 μm ol/L, 35～45 μm ol/L or 45～50 μm ol/L, such as 5 μm ol/L,
10 μm ol/L, 15 μm ol/L, 20 μm ol/L, 25 μm ol/L, 30 μm ol/L, 35 μm ol/L, 40 μm ol/L, 45 μm ol/L or 50 μ
mol/L。
In one embodiment of the invention, the quality of described gelatin is 300～500g, such as 300～350g, 350
～400g, 400～450g or 450～500g, such as 300g, 350g, 400g, 450g or 500g.
In one embodiment of the invention, in described solution A, the concentration of gelatin is 150～500g/L, such as 150
～200g/L, 200～250g/L, 250～300g/L, 300～350g/L, 350～400g/L, 400～450g/L or 450～
500g/L, such as 150g/L, 200g/L, 250g/L, 300g/L, 350g/L, 400g/L, 450g/L or 500g/L.
In one embodiment of the invention, the quality of described dextrin is 300～500g, such as 300～350g, 350
～400g, 400～450g or 450～500g, such as 300g, 350g, 400g, 450g or 500g.
In one embodiment of the invention, in described solution A, the concentration of dextrin is 150～500g/L, such as 150
～200g/L, 200～250g/L, 250～300g/L, 300～350g/L, 350～400g/L, 400～450g/L or 450～
500g/L, such as 150g/L, 200g/L, 250g/L, 300g/L, 350g/L, 400g/L, 450g/L or 500g/L.
In one embodiment of the invention, the component of step 1 comprises coloring agent.
In one embodiment of the invention, described coloring agent is dissolved in the water in advance, forms aqueous solution (the denseest
Degree be the aqueous solution of 0.01～0.1mmol/L, such as concentration be 0.01～0.03mmol/L, 0.03～0.06mmol/L, 0.06
～the aqueous solution of 0.09mmol/L or 0.09～0.1mmol/L, such as concentration be 0.01mmol/L, 0.02mmol/L,
0.03mmol/L、0.04mmol/L、0.05mmol/L、0.06mmol/L、0.07mmol/L、0.08mmol/L、0.09mmol/L
Or the aqueous solution of 0.1mmol/L), then mix with other component.
In one embodiment of the invention, being blended in homogenizer of step 1 is carried out, it is preferable that carry out 3～6 little
Time, such as 3～4 hours, 4～5 hours or 5～6 hours, such as 3 hours, 4 hours, 5 hours or 6 hours.
In one embodiment of the invention, step 1 be blended in 50～60 DEG C (such as 50～52 DEG C, 52～54 DEG C,
54～56 DEG C, 56～58 DEG C or 58～60 DEG C, such as 50 DEG C, 51 DEG C, 52 DEG C, 53 DEG C, 54 DEG C, 55 DEG C, 56 DEG C, 57 DEG C, 58 DEG C,
59 DEG C or 60 DEG C) under conditions of carry out.
In one embodiment of the invention, the spray drying of step 2 uses spray drying instrument to carry out.
In one embodiment of the invention, the inlet temperature being spray-dried instrument is 100 DEG C～150 DEG C, such as 100 DEG C
～120 DEG C, 120 DEG C～140 DEG C or 140 DEG C～150 DEG C.
In one embodiment of the invention, the air exhauster frequency being spray-dried instrument is 100%.
In one embodiment of the invention, be spray-dried instrument peristaltic pump frequency be 10～30%, such as 10～
20% or 20～30%.
In one embodiment of the invention, the cleansing pin frequency being spray-dried instrument is 1.
In one embodiment of the invention, be spray-dried instrument pneumatics air inlet be 30～50, such as 30～40,40～
45 or 45～50.
In one embodiment of the invention, the leaving air temp being spray-dried instrument is 70 DEG C～80 DEG C.
In one aspect, the invention provides a kind of filter stick, it contains the microcapsule of the present invention.
In one embodiment of the invention, during described microcapsule is present in the prefabricated chamber of filter stick.
In one embodiment of the invention, described microcapsule is present in the tow of filter stick.
In one aspect, the invention provides a tobacco articles, its microcapsule containing the present invention or filter stick.
In one embodiment of the invention, described tobacco product is Medicated cigarette.
In one embodiment of the invention, described tobacco product is chewing tobacco.
In one aspect, the invention provides the extract doing Folium Camelliae sinensis for preparing the purposes of microcapsule.
In one embodiment of the invention, described microcapsule is used for preparing tobacco product (such as Medicated cigarette or chewing tobacco).
In one embodiment of the invention, do described in the extract of Folium Camelliae sinensis selected from do Folium Camelliae sinensis hydrosol, do Folium Camelliae sinensis quintessence oil,
Do Folium Camelliae sinensis tincture, do Folium Camelliae sinensis absolute oil and do Folium Camelliae sinensis extractum.
In the present invention, unless otherwise stated, Science and Technology noun used herein has art technology
The implication that personnel are generally understood that.Further, involved herein laboratory operation step is widely used in being corresponding field
Conventional steps.Meanwhile, in order to be more fully understood that the present invention, provide below definition and the explanation of relational language.
" microcapsule " of the present invention refers to utilize macromolecular material (such as sodium alginate, calcium alginate, gelatin and paste
Essence) by solid, liquid or gas entrapment or seal up for safekeeping, the microgranule obtained, its particle diameter is 0.25 μm～1000 μm.
" tea fresh leaves " of the present invention is otherwise known as dark brownish green, refers to from Camellia sinensis Camellia sinensis (Camellia
Sinensis (L.) O.Ktze.) upper bud, leaf, tender stem, the tender tip and/or the twig plucked.
In the present invention, term " does Folium Camelliae sinensis " and refers to the product that tea fresh leaves or the vanes that withers obtain after doing blue or green process.
" doing green grass or young crops " of the present invention is under the effect of mechanical force, makes tea fresh leaves or withered tea leaves edge portion damaged,
Promote the polyphenols partial oxidation of its intension, polymerization, produce coloring matter, and promote the formation of aroma substance.Preferably,
Do blue or green process and include that one or many rocking of green leaf and airing process.
" withering " of the present invention refers to be placed under illumination, ventilation and/or heating condition tea fresh leaves, makes tea fresh leaves lose
Water is wilted.
" rocking of green leaf " of the present invention refers to by hand or machine, makes tea fresh leaves or withered tea leaves justify in a reservoir
Zhou Yundong and stirring up and down.Such as, tea fresh leaves or withered tea leaves are put in big bamboo plaque or vibration machine, carries out the most hand
Or machinery drives rocking of green leaf cage to rotate, and makes Folium Camelliae sinensis blade constantly circle round, stirs up and down, allow leaf margin and leaf margin, leaf margin and compass screen surface phase
Friction, leaf margin cell breakage mutually.Rocking of green leaf can promote polyphenol compound oxidation, polymerization, makes tea generation series of physical chemistry
Change.
In the present invention, term " hydrosol " refers to tissue (such as flower, leaf branch, stem, the tree of spice berry or medicinal plants
Skin, root, fruit etc.) carry out distilling the distillation obtained, optionally, also distillation can be filtered and/or concentrate.
In the present invention, term " quintessence oil " refers to by steam distillation, squeezing, cold grinding or dry distilling, from spice berry, medicinal
Plant the goods processing the oily fragrant containing substance obtained by extracting.Quintessence oil can also be by extracting hydrosol and being concentrated to give
Arrive.
In the present invention, term " absolute oil " refers to by ethanol extraction extractum or balsam, face cream, extraction containing fragrant distilled water
Taking liquid, chilled process, filter off the material insoluble in ethanol, the most under reduced pressure low temperature boils off ethanol, the product of gained.
In the present invention, term " tincture " refers to the ethanol extraction of natural perfume material, including cold process tincture and full-boiled process tincture.Cold
Method tincture is the alcohol leaching liquid at room temperature (not heating) extraction natural perfume material gained with ethanol, and through filtering what clarification obtained
Goods.Full-boiled process tincture is the ethanol extract extracting natural perfume material gained with ethanol in a heated condition, and through optional concentration
And/or filter the goods that clarification obtains.
In the present invention, term " extractum " refers to extract natural perfume material with organic solvent, and carries out lixiviating solution concentrating institute
The aroma material preparation obtained, is typically paste.Extractum can also be by being concentrated to give tincture.
Natural perfume material of the present invention, including tissue (such as flower, leaf branch, stem, the tree of spice berry and medicinal plants
Skin, root, fruit etc.) and exudate (such as resin, natural oil), and secrete fragrant animal containing fragrant secretions.
" tobacco product " of the present invention refer to completely or partially by Nicotiana tabacum L. be that raw material produces, for aspirating, sucking,
Chew or the goods of snuffing.Described tobacco product includes but not limited to Medicated cigarette and chewing tobacco.
" filter stick " of the present invention refers in Medicated cigarette, with filtering material (such as cigarette fibre bundle and core paper
Deng) it is raw material, what processing rolled has strainability and has the circular rod of certain length.
As used in this article, term " particle diameter " i.e. " equivalent grain size ", refer to when tested granule certain physical characteristic or
When physical behavio(u)r is the most close with the homogenous spheres of a certain diameter (or combination), just using the diameter (or combination) of this spheroid as tested
The equivalent grain size (or particle size distribution) of granule.
The present invention quotes in full following document:
GBT 30766-2014 Classification of Tea；GBT 30357.2-2013 oolong tea part 2: TIEGUANYIN；GBT
30357.3-2015 oolong tea third portion: Murrayae Folium Et Cacumen；GBT 30357.4-2015 oolong tea the 4th part: narcissus；GBT
30357.5-2015 oolong tea the 5th part: Cortex Cinnamomi；Chen Rongbing, Yao Xinen, Huang Fuping. fujian oolong tea kind [J]. Chinese tea
Leaf, 2002,24 (2): 6-9.
The beneficial effect of the invention
The microcapsule of the present invention have the effect that in one or more:
(1) containing the extract doing Folium Camelliae sinensis in the microcapsule of the present invention.The aromatic style of the extract doing Folium Camelliae sinensis has tea concurrently
Fragrant and the fragrance of a flower, odor type is pleasant especially, has elegant sweet, feature that breath is pleasant.
(2) microcapsule of the present invention can efficiently control the release of aroma substance, improves and does the extract of Folium Camelliae sinensis and wave
The property sent out is relatively strong, hold the shortcoming that fragrant ability is more weak, and makes it easy to transport and storage；
(3) microcapsule of the present invention is applied to tobacco product, such as, in Medicated cigarette, the aroma quality of tobacco product can be made
Being significantly improved, Hui Tian promotes the production of body fluid, flue gas harmony, and tea fragrant breeze lattice are obvious；
(4) microcapsule of the present invention has expanded the scope of application of the extract doing Folium Camelliae sinensis, is applicable not only to traditional Medicated cigarette
Product, it is possible to be applied to new cigarette, such as electronic cigarette, or the product such as chewing medicated cigarette；
(5) in certain embodiments, the microcapsule of the present invention contains coloring agent, can improve the detection of inferior microcapsule
Rate.Microcapsule containing coloring agent is put in tobacco product, it is also possible to improve the suction desire of consumer, promote suction product
Matter.
Detailed description of the invention
Below in conjunction with embodiment, embodiment of the present invention are described in detail, but those skilled in the art will
Understanding, the following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.In embodiment unreceipted specifically
Condition person, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same or instrument unreceipted production firm person, be
Can by city available from conventional products.
Accompanying drawing explanation
Fig. 1 is the total ion current figure that TIEGUANYIN autumn tea is cooked Folium Camelliae sinensis quintessence oil.
Fig. 2 is the total ion current figure of TIEGUANYIN autumn tea finished product tea essential oil.
Embodiment 1: do the preparation of Folium Camelliae sinensis hydrosol
Pluck 20kg TIEGUANYIN autumn tea fresh leaves, and after withering and doing blue or green process, obtain TIEGUANYIN autumn tea and do Folium Camelliae sinensis
15kg。
With vapor distillation still, TIEGUANYIN autumn tea is cooked Folium Camelliae sinensis and carry out open steam distillation.The bottom of vapor distillation still
Being provided with steam entry, top is provided with steam outlet, inside vapor distillation still, between steam entry and outlet
Position, be provided with for placing distilland and through the porose sieve plate of steam.15kg TIEGUANYIN autumn tea is cooked Folium Camelliae sinensis put
On the sieve plate of vapor distillation still, steam (temperature about 105 DEG C) is entered in distillating still by the bottom of distillating still, through sieve plate
Doing Folium Camelliae sinensis with TIEGUANYIN autumn tea to be fully contacted, then the steam outlet from top is derived, condensed device (condenser temperature-5 DEG C
～10 DEG C) condensation, collect distillation.Total distillation time is about 2.5h, and the speed of response of distillation is about 25kg/h, and distillation is total
Collecting amount is about 62.5kg.
Use micro-filtration membrane (aperture is 0.2 μm) that distillation carries out microfiltration, after removing float and antibacterial, obtain microfiltration saturating
Cross liquid about 60.0kg.Microfiltration permeate concentrates through reverse osmosis membrane (GEHWSRO8040HR, salt rejection rate NaCl 99.5%), reverse osmosis
The film pressure that goes out concentrated is 0.8MPa, during process by cooling water recirculation system holding temperature of liquid between 20 DEG C～30 DEG C,
Obtain being Folium Camelliae sinensis hydrosol 5.0kg.
Embodiment 2: do the preparation of Folium Camelliae sinensis quintessence oil
Do addition saturated aqueous common salt in Folium Camelliae sinensis hydrosol what embodiment 1 obtained, add ethyl acetate extraction, ethyl acetate
Weight is do Folium Camelliae sinensis hydrosol weight 30%, separating ethyl acetate extract.Repeatedly extract according to above-mentioned steps 5 times, merge second
Acetoacetic ester extract.Add anhydrous Na2SO4After drying, carrying out concentrating under reduced pressure, the condition of concentrating under reduced pressure is temperature 35 DEG C, vacuum
For 210mbar, stop concentrating when being concentrated near doing, obtain steaming excess 5.0g.Add the anhydrous second of 3 times amount steaming excess weight
Alcohol, continues concentrating under reduced pressure, and the temperature of concentrating under reduced pressure is 40 DEG C, and vacuum is 120mbar, is concentrated into dehydrated alcohol and ethyl acetate
Close to all steaming, obtain being Folium Camelliae sinensis quintessence oil 2.90g, be 0.19 ‰ relative to the yield doing Folium Camelliae sinensis, obtaining relative to tea fresh leaves
Rate is 0.14 ‰.
Embodiment 3: do the preparation of Folium Camelliae sinensis tincture
In the extraction system that embodiment 1 obtains after doing Folium Camelliae sinensis hydrosol, by doing Folium Camelliae sinensis initial weight and the weight of 95% ethanol
The amount ratio than 1:10, adds 95% ethanol.Controlling heating-up temperature is 60 DEG C～70 DEG C, and extraction time is 1～2h, and hot reflux carries
Take 2 times.Merge the alcohol extract of twice, be 45 DEG C～55 DEG C in temperature, vacuum be reduce pressure under conditions of 40～60mbar dense
Contracting, obtains doing Folium Camelliae sinensis tincture, and density is 1.08 ± 0.02g/cm3, yield is 12%.
Embodiment 4: do the preparation of Folium Camelliae sinensis extractum
According to the concentration condition in embodiment 3, the Folium Camelliae sinensis tincture that does obtaining embodiment 3 concentrates further, by therein greatly
Partial solvent removes, and is concentrated into paste, obtains doing Folium Camelliae sinensis extractum, and density is 1.2 ± 0.02g/cm3。
Embodiment 5: do the preparation of Folium Camelliae sinensis absolute oil
Do Folium Camelliae sinensis extractum with what ethanol extraction embodiment 4 obtained, at-15 DEG C after freezing 36h, be filtered to remove insoluble matter,
Then decompression, less than room temperature under conditions of ethanol is distilled off, obtain doing Folium Camelliae sinensis absolute oil.
Comparative example 1: become the preparation of hydrosol of sampling tea
Pluck 60.0kg TIEGUANYIN autumn tea fresh leaves, and through the green grass or young crops that withers, does, complete, after rolling and drying etc. process, make
TIEGUANYIN autumn tea becomes the 15kg that samples tea.
Become to sample tea and carry out open steam distillation to TIEGUANYIN autumn tea with vapor distillation still.The bottom of vapor distillation still
Being provided with steam entry, top is provided with steam outlet, inside vapor distillation still, between steam entry and outlet
Position, be provided with for placing distilland and through the porose sieve plate of steam.Become to sample tea by 15kg TIEGUANYIN autumn tea and put
On the sieve plate of vapor distillation still, steam is entered in distillating still by the bottom of distillating still, through sieve plate and TIEGUANYIN autumn tea
Becoming samples tea is fully contacted, and then the steam outlet from top is derived, and condensed device (condenser temperature-5 DEG C～10 DEG C) condenses
Rear collection distillation.Total distillation time is about 3.0h, and the speed of response of distillation is about 30kg/h, and distillation total collection is about
90.0kg。
Use the micro-filtrate membrane filtration distillation in 0.8 μm aperture, filter off impurity, obtain microfiltration permeate (about 87.0kg).Then
Using reverse osmosis membrane that microfiltration permeate is carried out reverse-osmosis treated, going out film pressure is 1.0MPa, by cooling water circulation during process
System keeps temperature of liquid between 20 DEG C～30 DEG C, it is thus achieved that 7.0kg becomes hydrosol of sampling tea.
Comparative example 2: the preparation of finished product tea essential oil
The one-tenth obtained in comparative example 1 is sampled tea and is added saturated aqueous common salt in hydrosol, adds 2.1kg ethyl acetate extraction (phase
When becoming, in above-mentioned TIEGUANYIN autumn tea, the 30% of hydrosol weight of sampling tea), extraction, separating ethyl acetate extract after extraction.By above-mentioned
Step extracts 6 times repeatedly, combined ethyl acetate extract, obtains acetic acid ethyl acetate extract 12.0kg altogether.
Anhydrous Na is added in acetic acid ethyl acetate extract2SO4Dehydration, then filters off Na2SO4.To the ethyl acetate after dehydration
Extract carries out the first concentrating under reduced pressure, and vapo(u)rizing temperature is 35 DEG C, and vacuum is 210mbar, removes ethyl acetate, steams excess weight
For 10.25g.
Steam and excess adds about 16.8g dehydrated alcohol (being equivalent to steam 3 times of excess weight), carry out the second decompression dense
Contracting, vapo(u)rizing temperature is 40 DEG C, and vacuum is 120mbar, removes ethanol and Residual ethyl acetate, steams excess and is into caffein of sampling tea
Oil, weight is 5.20g, is 0.35 ‰ relative to becoming the yield sampled tea, is 0.08 ‰ relative to the yield of tea fresh leaves.
Embodiment 6: the preparation of the essence combination containing the extract doing Folium Camelliae sinensis
Material source: do Folium Camelliae sinensis extractum, do Folium Camelliae sinensis quintessence oil, do Folium Camelliae sinensis absolute oil and do Folium Camelliae sinensis tincture and obtained by embodiment 2-5, its
His essence is provided by Hua Bao essence and flavoring agent (Shanghai) Co., Ltd..
1, the preparation of essence combination 1
According to the proportioning in table 1, each component is mixed, obtain essence combination 1.
The proportioning of table 1. essence combination 1
2, the preparation of essence combination 2
According to the proportioning in table 2, each component is mixed, obtain essence combination 2.
The proportioning of table 2. essence combination 2
3, the preparation of essence combination 3
According to the proportioning in table 3, each component is mixed, obtain essence combination 3.
The proportioning of table 3. essence combination 3
| Component | Consumption (%) |
| Do Folium Camelliae sinensis extractum | 4.55 |
| Do Folium Camelliae sinensis quintessence oil | 1.50 |
| Do Folium Camelliae sinensis absolute oil | 2.15 |
| Do Folium Camelliae sinensis tincture | 3.35 |
| 1-Phenylethanone. | 0.10 |
| Linalool | 0.15 |
| Phenethanol | 0.10 |
| Dihydro jasmone | 0.45 |
| MDJ | 0.10 |
| Caryophyllene oxide | 0.45 |
| β-caryophyllenol | 0.25 |
| β-Damascenone | 0.15 |
| Oxidation isophorone | 0.35 |
| Alpha, beta-lonone | 0.25 |
| Dihydroactinidiolide | 0.35 |
| Aglaia odorata flower concrete | 0.25 |
| Yunyan extract | 0.20 |
| 70% ethanol | 85.30 |
| Add up to | 100 |
Analyze and detect example 1: derived essential oil analysis
The TIEGUANYIN autumn tea using Gas Chromatography/Mass Spectrometric Method detection embodiment 2 is cooked the ferrum of Folium Camelliae sinensis quintessence oil and comparative example 2 and sees
Chemical composition in sound autumn tea finished product tea essential oil.Testing conditions is as follows:
Extraction conditions: accurately weigh a certain amount of essential oil smaple, uses dichloromethane extraction, and nitrogen blows concentration, adds acetic acid
Phenethyl ester internal standard, to be measured.
GC conditions: gas chromatograph (Agilent 7890), chromatographic column HP-INNOWAX (60m × 0.25mm ×
0.25μm)；Injector temperature 250 DEG C；Column oven heating schedule: initial temperature 60 DEG C, keeps 2min, is warmed up to 2 DEG C/min
180 DEG C, then 5 DEG C/min is warmed up to 230 DEG C, keeps 40min；Sample size: 1 μ L；Carrier gas: helium (purity 99.999%)；Carrier gas
Flow 1.0mL/min；Split ratio 50:1.
Mass Spectrometry Conditions: mass detector (Agilent 5975N): transmission line temperature 280 DEG C, ion source temperature 230 DEG C, adjust
Humorous voltage 1600V, solvent delay is: 5min；Quality of scanning number scope is: 35～455u, and detection pattern is full scan pattern, spectrum
Library searching uses NIST storehouse to retrieve.Do the total ion current figure of Folium Camelliae sinensis quintessence oil and finished product tea essential oil as depicted in figs. 1 and 2.Adopt
Calculate the percentage ratio of each component by area normalization method, result is as shown in table 4.
Table 4 does Folium Camelliae sinensis quintessence oil and the composition analysis result of finished product tea essential oil
As shown in table 4, compared to finished product tea essential oil, do the content of multiple fragrance component in Folium Camelliae sinensis quintessence oil the highest, such as
The content of phenethanol and benzyl alcohol is higher.Phenethanol has the hyacinth-Fructus Gardeniae fragrance of gentleness, flower, earth, Mel perfume (or spice)
Gas and the taste of fruit sample.Benzyl alcohol has fragrance faint, sweet, fruity, distinctive pleasant fruit aroma.This
Outward, doing Folium Camelliae sinensis quintessence oil and have the fragrance component not having in multiple finished product tea essential oil, such as dihydro-β-ionone, it has
The Radix Aucklandiae, the fragrance of a flower and fruital fragrance, and terpinenyl aceatae, its tool delicate fragrance band is sweet, has the breath of similar bergamot and lavandula angustifolia.
Analyze and detect example 2: quintessence oil and essence organoleptic analysis
Embodiment 2 is obtained do Folium Camelliae sinensis quintessence oil, finished product tea essential oil that comparative example 2 obtains and the perfume (or spice) that embodiment 6 obtains
Essence compositions 1 carries out smelling fragrant analysis respectively, and analysis result is as shown in table 5.
Table 5 quintessence oil and essence organoleptic analysis
Result shows, what the present invention obtained do Folium Camelliae sinensis quintessence oil has the fragrance different from finished product tea essential oil style.By doing green grass or young crops
The essence that the extract of tea prepares has the aroma quality close with the extract doing Folium Camelliae sinensis.
Embodiment 7: contain essence combination 1-3 respectively, do the preparation of the microcapsule of Folium Camelliae sinensis quintessence oil and finished product tea essential oil
The TIEGUANYIN autumn tea using the essence combination 1-3 that obtains of embodiment 6, embodiment 2 to obtain respectively is cooked Folium Camelliae sinensis quintessence oil
The TIEGUANYIN autumn tea finished product tea essential oil obtained with comparative example 2, according to following preparation process and technological parameter, by be spray-dried
Method prepares following microcapsule 1-5:
Microcapsule 1: containing essence combination 1；
Microcapsule 2: containing essence combination 2；
Microcapsule 3: containing essence combination 3；
Microcapsule 4: do Folium Camelliae sinensis quintessence oil containing TIEGUANYIN autumn tea；
Microcapsule 5: containing TIEGUANYIN autumn tea finished product tea essential oil.
Preparation process: by water-soluble to quintessence oil or essence combination, sodium alginate (the equal molecular mass 32,000～250,000 of number)
Liquid, gelatin, dextrin and the mixing of optional coloring agent, carry out homogenizing in high-shear homogenizer, obtain solution A, spray solution A
Mist is dried, and obtains the microcapsule that particle diameter is 1～25 μm.
Spray drying device: Buchi Mini Spray Dryer B-290 is spray-dried instrument.
The technological parameter being spray-dried:
Inlet temperature (Inlet): 100 DEG C～150 DEG C；Air exhauster frequency (Aspirator): 100%；Peristaltic pump frequency
(Pump): 10～30%；Cleansing pin frequency (Nozzle cleaner): 1；Pneumatics air inlet (Q-Flow by vogtlin): 30～
50；Last leaving air temp: 70 DEG C～80 DEG C.
As a example by the essence combination 2 obtained by embodiment 6 and essence combination 3, the preparation process of microcapsule is as follows:
(1) by 1g essence combination 2,25 μm ol/L sodium alginate aqueous solution 1L, 300g gelatin, 300g dextrin and
0.01mmol/L light blue (food stage) aqueous solution 1L mixes, homogenizing 3 hours in high-shear homogenizer, under conditions of 50～60 DEG C,
Obtain solution A.
Use Buchi Mini Spray Dryer B-290 to be spray-dried instrument, solution A is spray-dried, spray dried
Dry condition is: inlet temperature (Inlet): 120 DEG C；Air exhauster frequency (Aspirator): 100%；Peristaltic pump frequency
(Pump): 20%；Cleansing pin frequency (Nozzle cleaner): 1；Pneumatics air inlet (Q-Flow by vogtlin): 40.Through overspray
Mist is dried, and obtains microcapsule 2, and particle diameter is 1～25 μm.
(2) by 2g essence combination 3,50 μm ol/L sodium alginate aqueous solution 1L, 400g gelatin, 400g dextrin and
0.05mmol/L lemon yellow (food stage) aqueous solution 1L mixes, and in high-shear homogenizer, under conditions of 50～60 DEG C, homogenizing 6 is little
Time, obtain solution A.
Use Buchi Mini Spray Dryer B-290 to be spray-dried instrument, solution A is spray-dried, spray dried
Dry condition is: inlet temperature (Inlet): 140 DEG C；Air exhauster frequency (Aspirator): 100%；Peristaltic pump frequency
(Pump): 30%；Cleansing pin frequency (Nozzle cleaner): 1；Pneumatics air inlet (Q-Flow by vogtlin): 45.Through overspray
Mist is dried, and obtains microcapsule 3, and particle diameter is 1～25 μm.
The preparation of the embodiment 8 Medicated cigarette containing microcapsule
Microcapsule 1, microcapsule 4 and the microcapsule 5 embodiment 7 obtained, is respectively applied in the filter stick of long 15mm, makes
Binary compound filter candle Medicated cigarette.Measured essence combination 1 in filter stick respectively by gas chromatography, TIEGUANYIN autumn tea is cooked Folium Camelliae sinensis quintessence oil
With the content of TIEGUANYIN autumn tea finished product tea essential oil, about 1.2mg/ props up.The blank cigarette sample of preparation, it differs only in filter stick not
Apply microcapsule.In above-mentioned Medicated cigarette, tobacco shred does not apply quintessence oil or essence.
Sensory Quality of Cigarette evaluation test 1
The Medicated cigarette obtained embodiment 8 according to national standard (GB5606.4-2005) carries out sensory quality assessment, and marking is commented
Valency is as shown in table 6, describes and evaluates as shown in table 7.
Medicated cigarette is numbered:
A1: use Medicated cigarette prepared by microcapsule 1 (containing essence combination 1)；
A2: use Medicated cigarette prepared by microcapsule 4 (doing Folium Camelliae sinensis quintessence oil containing TIEGUANYIN autumn tea)；
A3: use Medicated cigarette prepared by microcapsule 5 (containing TIEGUANYIN autumn tea finished product tea essential oil).
The aesthetic quality of table 6 Medicated cigarette A1, A2, A3 gives a mark evaluation table
The aesthetic quality of table 7 Medicated cigarette A1, A2, A3 describes evaluation table
From the analysis of table 6, the score of Medicated cigarette A1-A3 is above blank Medicated cigarette, and, the score of Medicated cigarette A2 is higher than volume
Cigarette A3.
From the analysis of table 7, the evaluation of Medicated cigarette A1-A3 is higher than blank Medicated cigarette.In terms of fragrance, Medicated cigarette A2 and A3 has
Floral notes, Medicated cigarette A2 is had also to have fruital.The above results shows, the microcapsule containing the extract doing Folium Camelliae sinensis is applied to volume
In cigarette, miscellaneous QI can be covered, reduce and stimulate, improve mouthfeel, and give the characteristic perfume that Medicated cigarette does Folium Camelliae sinensis, the such as fragrance of a flower and/
Or fruital note, make the fragrance of Medicated cigarette enrich pleasant.
The preparation of the embodiment 9 Medicated cigarette containing microcapsule 2 and the preparation of the Medicated cigarette without microcapsule
According to the method for embodiment 8, use microcapsule 2 (containing essence combination 2) to make binary compound filter candle Medicated cigarette and (contain
The long 15mm of filter stick of microcapsule), it is that 1.2mg/ props up by the content of essence combination in gas chromatography determination filter stick, tobacco shred is not
Apply essence, numbered Medicated cigarette I.
Use the tobacco shred identical with Medicated cigarette I, essence combination 2 is applied in tobacco shred, use common filter stick cigarette to become
Medicated cigarette, numbered Medicated cigarette II, wherein, the content of essence combination 2 is that 1.5mg/ props up.
Sensory Quality of Cigarette evaluation test 2
12 experts are organized to enter respectively at Medicated cigarette I and the Medicated cigarette II that embodiment 9 is prepared by April, 2015 and in October, 2015
Row is smoked panel test, and assessment item includes: the tea that Folium Camelliae sinensis odor characteristic is done in fragrance, coordination, miscellaneous QI, stimulation, pleasant impression and representative is fragrant；Averagely comment
Suction result is as shown in table 8.
The smoking result of table 8 Medicated cigarette I and II
Note: in table, fragrance, harmony, miscellaneous QI, stimulation, the score value of pleasant impression are the meansigma methods that 12 experts provide score value；Tea is fragrant
The most sufficient, score value is the highest；Remaining index quality is the best, and score value is the highest.During tea perfume (or spice) is smoked panel test, a represents the smoking result in April, 2015
(12 experts), b represents the smoking result (12 experts) in October, 2015.
Evaluation result shows:
1, relative to the Medicated cigarette (Medicated cigarette II) being directly applied to obtain in tobacco shred by essence, micro-glue made by essence by the present invention
Capsule, puts on the Medicated cigarette (Medicated cigarette I) obtained in filter stick, more excellent in the index of the aspects such as fragrance, harmony, miscellaneous QI, stimulation, pleasant impression
Elegant.
2, for representing the tea perfume (or spice) index doing Folium Camelliae sinensis odor characteristic, the tea of Medicated cigarette II is fragrant relatively big in 1-2 mouth intensity, but
3-4 mouth starts substantially to weaken；Although and the fragrant 1-2 mouth of the tea of Medicated cigarette I is more weak compared with Medicated cigarette II, but from the 1st mouthful to having aspirated
Finishing, be always held at close level, aggregate performance is outstanding compared with Medicated cigarette II.Further, again to Medicated cigarette I and Medicated cigarette after half a year
II smokes panel test, and the tea perfume of Medicated cigarette I was more or less the same before half a year, and the tea perfume (or spice) of Medicated cigarette II occurs significantly loss.
These results suggest that, the extract doing Folium Camelliae sinensis is made microcapsule and puts in Medicated cigarette, Medicated cigarette can be given and do green grass or young crops
The characteristic perfume of tea, and hold fragrant ability more preferably, odor characteristic loss is little, and aggregate performance is more excellent.
Although the detailed description of the invention of the present invention has obtained detailed description, but those skilled in the art will appreciate that root
According to disclosed all teachings, details can be carried out various modifications and changes, and these change all the guarantor of the present invention
Within the scope of protecting.The four corner of the present invention is given by claims and any equivalent thereof.
Claims (17)
1. a microcapsule, it contains the extract doing Folium Camelliae sinensis；
Preferably, do described in the extract of Folium Camelliae sinensis selected from do Folium Camelliae sinensis hydrosol, do Folium Camelliae sinensis quintessence oil, do Folium Camelliae sinensis absolute oil, do Folium Camelliae sinensis tincture and
Do one or more in Folium Camelliae sinensis extractum.
2. the microcapsule of claim 1, described in do Folium Camelliae sinensis hydrosol and prepared by the method that comprises the steps of:
Step (1): do Folium Camelliae sinensis with vapor distillation, obtain distillation；
Optionally, described method is further comprising the steps of:
Step (2): distillation is carried out microfiltration, obtains microfiltration permeate；And/or
Step (3): microfiltration permeate is concentrated.
3. the microcapsule of claim 1 or 2, described in do Folium Camelliae sinensis quintessence oil and prepared by the method that comprises the steps of:
Step (1): do Folium Camelliae sinensis with vapor distillation, collects distillation, obtains doing Folium Camelliae sinensis hydrosol；With
Step (2): do to isolate Folium Camelliae sinensis hydrosol do Folium Camelliae sinensis quintessence oil from what step (1) obtained；
Optionally, step (1) includes distillation is carried out microfiltration and/or concentration；
Preferably, the separation in described step (2) is realized by extraction.
Preferably, step (2) includes concentrating extraction product.
4. the microcapsule of any one of claim 1-3, described in do Folium Camelliae sinensis tincture and prepared by the method that comprises the steps of:
Step (1): in a heated state, uses organic solvent (such as ethanol or ethanol solution) to carry out backflow and carry doing Folium Camelliae sinensis
Take；
Step (2): the extracting solution obtaining step (1) concentrates；
Preferably, the concentration of step (2) is carried out at reduced pressure conditions；
Preferably, the density doing Folium Camelliae sinensis tincture described in is 1.05～1.10g/cm3。
5. the microcapsule of any one of claim 1-4, described in do Folium Camelliae sinensis extractum be to be condensed into paste and prepare by will do Folium Camelliae sinensis tincture
's；
Preferably, described concentration is carried out at reduced pressure conditions.
6. the microcapsule of any one of claim 1-5, described in do Folium Camelliae sinensis absolute oil and prepared by the method that comprises the steps of:
Step (1): do Folium Camelliae sinensis extractum with ethanol extraction, be extracted liquid；
Step (2): extract is carried out freezing, is filtered to remove the material insoluble in ethanol；
Step (3): filtrate distilled at reduced pressure conditions, removes ethanol.
7. the microcapsule of any one of claim 1-6, wherein, described in do Folium Camelliae sinensis and with the tea fresh leaves of oolong tea Camellia sinensis and/or wither
Blade is raw material；
Preferably, described oolong tea Camellia sinensis is Tie Guanyin tea plant and/or Wuyi cliff tea Camellia sinensis；
Preferably, described Wuyi cliff tea Camellia sinensis selected from Radix Campylotropis Hirtella (Herba Myrsines Africanae) Camellia sinensis, bright fir Camellia sinensis, narcissus Camellia sinensis, Cortex Cinnamomi Camellia sinensis and very plants tea
One or more in tree；
Preferably, Folium Camelliae sinensis is done described in the spring tea of oolong tea Camellia sinensis and/or autumn tea as raw material.
8. the microcapsule of any one of claim 1-7, described microcapsule is possibly together with one or more in following material: benzene second
Ketone, linalool, phenethanol, dihydro jasmone, MDJ, caryophyllene oxide, β-caryophyllenol, β-Tujue's alkene
Ketone, oxidation isophorone, alpha, beta-lonone, dihydroactinidiolide, aglaia odorata flower concrete, yunyan extract, Oleum Pelargonii Graveolentis, Fructus Anisi Stellati
Aldehyde, Megastigmatrienone, vanillin, ethyl vanillin, maltol, ethylmaltol, furanone, 2,3,5-trimethylpyrazine and 2-
Acetyl group pyrazine；
Preferably, described microcapsule is possibly together with one or more in following material: 1-Phenylethanone., linalool, phenethanol, dihydro jasmine
Jasmine ketone, MDJ, caryophyllene oxide, β-caryophyllenol, β-Damascenone, oxidation isophorone, β-violet
Ketone, dihydroactinidiolide, aglaia odorata flower concrete and yunyan extract；
Preferably, described microcapsule is possibly together with one or more in following material: 1-Phenylethanone., linalool, phenethanol, Herba Pelargonii Graveolentis
Oil, MDJ, anisic aldehyde, β-caryophyllenol, β-Damascenone, Megastigmatrienone, alpha, beta-lonone, dihydro
Actinidia lactone, aglaia odorata flower concrete, vanillin, ethyl vanillin, maltol, ethylmaltol, furanone, 2,3,5-trimethyl
Pyrazine, 2-acetyl group pyrazine and yunyan extract.
9. the microcapsule of any one of claim 1-8, the particle diameter of described microcapsule is 1～25 μm.
10. the microcapsule of any one of claim 1-9, described microcapsule is possibly together with sodium alginate, gelatin, dextrin and optional
Toner.
The method of microcapsules of 11. preparation any one of claim 1-10, it comprises the following steps:
Step 1: following components is mixed, obtains solution A:
Do Folium Camelliae sinensis extract (such as do Folium Camelliae sinensis hydrosol, do Folium Camelliae sinensis quintessence oil, do Folium Camelliae sinensis tincture, do Folium Camelliae sinensis absolute oil and/or do Folium Camelliae sinensis leaching
Cream), or comprise and do the extract of Folium Camelliae sinensis and (such as do Folium Camelliae sinensis hydrosol, do Folium Camelliae sinensis quintessence oil, do Folium Camelliae sinensis tincture, do Folium Camelliae sinensis absolute oil and/or do
Folium Camelliae sinensis extractum) essence combination,
The aqueous solution of sodium alginate,
Gelatin,
Dextrin, and
Optional coloring agent；
Step 2: solution A is spray-dried.
The method of 12. claim 11, in described essence combination, the content of the extract doing Folium Camelliae sinensis be 3.00%～
10.00%；
Preferably, described essence combination is possibly together with one or more in following material: 1-Phenylethanone., linalool, phenethanol, two
Hydrogen jasmone, MDJ, caryophyllene oxide, β-caryophyllenol, β-Damascenone, oxidation isophorone, β-purple
Rowland ketone, dihydroactinidiolide, aglaia odorata flower concrete, yunyan extract, Oleum Pelargonii Graveolentis, anisic aldehyde, Megastigmatrienone, vanillin,
Ethyl vanillin, maltol, ethylmaltol, furanone, 2,3,5-trimethylpyrazine and 2-acetyl group pyrazine；
Preferably, described essence combination is possibly together with one or more in following material: 1-Phenylethanone., linalool, phenethanol, two
Hydrogen jasmone, MDJ, caryophyllene oxide, β-caryophyllenol, β-Damascenone, oxidation isophorone, β-purple
Rowland ketone, dihydroactinidiolide, aglaia odorata flower concrete and yunyan extract；
Preferably, described essence combination is possibly together with one or more in following material: 1-Phenylethanone., linalool, phenethanol, perfume (or spice)
Leaf oil, MDJ, anisic aldehyde, β-caryophyllenol, β-Damascenone, Megastigmatrienone, alpha, beta-lonone, two
Hydrogen actinidia lactone, aglaia odorata flower concrete, vanillin, ethyl vanillin, maltol, ethylmaltol, furanone, 2,3,5-front three
Base pyrazine, 2-acetyl group pyrazine and yunyan extract；
Preferably, described essence combination be by have following proportioning component mix after obtain: do the extract of Folium Camelliae sinensis
3.00%～10.00%, 1-Phenylethanone. 0.10%～3.00%, linalool 0.10%～3.00%, phenethanol 0.10%～
3.00%, dihydro jasmone 0.10%～3.00%, MDJ 0.10%～3.00%, caryophyllene oxide
0.10%～3.00%, β-caryophyllenol 0.10%～3.00%, β-Damascenone 0.10%～3.00%, oxidation isophorone
0.10%～3.00%, alpha, beta-lonone 0.10%～3.00%, dihydroactinidiolide 0.10%～3.00%, SHULANHUA leaching
Cream 0.10%～3.00%, yunyan extract 0.10%～3.00%, remaining is the ethanol water of 70%；
Preferably, described essence combination comprises do Folium Camelliae sinensis extractum 3.50%～4.55%, do Folium Camelliae sinensis quintessence oil 1.00%～
1.50%, Folium Camelliae sinensis absolute oil 1.50%～2.15% and do Folium Camelliae sinensis tincture 1.00%～5.00% is done.
The method of 13. any one of claim 11-12, described in do the extract of Folium Camelliae sinensis and the quality of sodium alginate: mol ratio is
0.03～2g:5～50 μm ol；
Preferably, described essence combination and the quality of sodium alginate: mol ratio is 1～20g:5～50 μm ol；
Preferably, the concentration of the aqueous solution of described sodium alginate is 5～50 μm ol/L；
Preferably, the quality of described gelatin is 300～500g；
Preferably, in described solution A, the concentration of gelatin is 150～500g/L；
Preferably, the quality of described dextrin is 300～500g；
Preferably, in described solution A, the concentration of dextrin is 150～500g/L；
Preferably, the component of step 1 comprises coloring agent；
Preferably, being dissolved in the water in advance by described coloring agent, (such as concentration is 0.01～0.1mmol/L to form aqueous solution
Aqueous solution), then mix with other component.
The method of 14. any one of claim 11-13, being blended in homogenizer of step 1 is carried out；
Preferably, the mixing of step 1 carries out 3～6 hours；
Preferably, step 1 be blended in 50～60 DEG C under conditions of carry out；
Preferably, the spray drying of step 2 uses spray drying instrument to carry out.
15. 1 kinds of filter sticks, it contains the microcapsule of any one of claim 1-10；
Preferably, during described microcapsule is present in the prefabricated chamber of filter stick；
Preferably, described microcapsule is present in the tow of filter stick.
16. 1 tobacco articles, its microcapsule containing any one of claim 1-10 or the filter stick of claim 15；
Preferably, described tobacco product is Medicated cigarette or chewing tobacco.
17. do the extract of Folium Camelliae sinensis for preparing the purposes of microcapsule；
Preferably, described microcapsule is used for preparing tobacco product (such as Medicated cigarette or chewing tobacco)；
Preferably, do described in the extract of Folium Camelliae sinensis selected from do Folium Camelliae sinensis hydrosol, do Folium Camelliae sinensis quintessence oil, do Folium Camelliae sinensis tincture, do Folium Camelliae sinensis absolute oil and
Do Folium Camelliae sinensis extractum.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106804801A (en) * | 2016-12-26 | 2017-06-09 | 中国农业科学院茶叶研究所 | A kind of processing method of flowers and fruits taste capsule tea |
| CN106804801B (en) * | 2016-12-26 | 2020-10-09 | 中国农业科学院茶叶研究所 | Processing method of flower and fruit flavored capsule tea |
| CN107034021A (en) * | 2017-04-27 | 2017-08-11 | 河南中烟工业有限责任公司 | A kind of cigarette quick-fried pearl savory essence of lily and its application in cigarette |
| CN109181875A (en) * | 2018-09-20 | 2019-01-11 | 云南中烟工业有限责任公司 | A kind of extracting and purifying method of the green tea absolute oil for tobacco flavoring |
| CN113730299A (en) * | 2021-08-06 | 2021-12-03 | 广州市芳香时代进出口有限公司 | Preparation process of essential oil microcapsule containing essential oil |
| CN113730299B (en) * | 2021-08-06 | 2023-06-02 | 广州市芳香时代进出口有限公司 | Preparation process of essential oil microcapsule containing essential oil |
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