CN105950298A - Preparation methods of tea hydrolat and tea essential oil - Google Patents
Preparation methods of tea hydrolat and tea essential oil Download PDFInfo
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- CN105950298A CN105950298A CN201610564959.7A CN201610564959A CN105950298A CN 105950298 A CN105950298 A CN 105950298A CN 201610564959 A CN201610564959 A CN 201610564959A CN 105950298 A CN105950298 A CN 105950298A
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- China
- Prior art keywords
- tea
- essential oil
- hydrosol
- preparation
- folium camelliae
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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
- C11B9/0003—Compounds of unspecified constitution defined by the chemical reaction for their preparation
-
- 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
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
- A24B15/241—Extraction of specific substances
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
-
- 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
- C11B9/022—Refining
-
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Tea And Coffee (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention provides preparation methods of tea hydrolat and tea essential oil. The preparation method of the tea hydrolat comprises the following steps that (1) a tea raw material is obtained and comprises green tea and/or fixation tea; (2) the tea raw material is distilled by vapor, distillate is collected, the tea hydrolat is obtained, and preferably, the distillate is concentrated. The preparation method of the tea essential oil further comprises step (3) tea essential oil is separated from the tea hydrolat in the step (2) (such as extraction separation). The tea hydrolat and the tea essential oil have unique flower scent and fragrance and are particularly suitable for flavoring cigarettes/electronic cigarettes.
Description
Technical field
The invention belongs to flavouring essence for tobacco field, particularly relate to the preparation method of tea hydrosol and tea essential oil.
Background technology
China is Folium Camelliae sinensis original producton location, and tea district is vast in territory, a multitude of names.According to the difference of Tea Processing technique, can be by tea
Leaf is divided into six big classes: green tea, yellow tea, Ramulus et Folium Mussaendae Pubescentis, Folium Camelliae sinensis (oolong tea), postfermented tea and black tea.
CN102504954A discloses a kind of method extracting essence from Folium Camelliae sinensis, belongs to separation and extraction technology field.This
Invention is solved the technical problem that to there is provided a kind of method extracting essence from Folium Camelliae sinensis, and it is higher that the method can obtain purity
Essence.The present invention extracts the method for essence from Folium Camelliae sinensis, including using supercritical CO2The step of extraction Folium Camelliae sinensis, wherein, surpasses and faces
Boundary CO2Pressure during extraction Folium Camelliae sinensis is 20~50MPa, and extraction temperature is 35~65 DEG C, and separation temperature is 70~80 DEG C.
CN1596687 discloses a kind of tea essence for Folium Camelliae sinensis food and preparation method thereof.The preparation method of tea essence
Comprise the steps: to prepare tea water extract, prepare tea extract extractum, prepare oxidation resistant plant extracting solution, prepare flavouring
Agent, then in the tea extract extractum of 100 weight portions, add the oxidation resistant plant extracting solution of 10~20 weight portions, 20~
The fumet of 30 weight portions, 10~15 Radix Acaciae senegalis of weight portion, high pressure homogenize after stirring, finally it is dried that to prepare tea fragrant
Essence.
CN101928639A discloses natural tea essence prepared by a kind of Folium Camelliae sinensis and preparation method thereof, is former with Folium Camelliae sinensis
Material, through complex enzyme hydrolysis, release, reduced steam distillation, cold-trap reclaims, freezing concentrates, centrifugal oil-water separation, anhydrous sulfur
The method of acid sodium absorption micro-moisture is prepared.
Summary of the invention
It is an object of the present invention to provide the preparation method of a kind of tea hydrosol, it is also another object of the present invention to provide one
Planting the preparation method of tea essential oil, further object of the present invention is to provide a kind of tea hydrosol, it is also another object of the present invention to provide
A kind of tea essential oil.
Inventor finds, compared to the Folium Camelliae sinensis of other kind, oolong tea has the fragrance of a flower and the fruital of uniqueness.Oolong tea only
Special fragrance can effectively give cigarette product tea note feature, and that improves Medicated cigarette returns sweet sense, reduces the dry stimulation of flue gas, improves
Mouth comfort.
Inventor is it has furthermore been found that with Oolong Tea tea and/or the tea that completes as raw material, extract the tea hydrosol or tea obtained
Quintessence oil has the particularly unique fragrance of a flower and delicate fragrance, is particularly suitable for Medicated cigarette/electronic cigarette perfuming.
First aspect present invention provides the preparation method of a kind of tea hydrosol, and it comprises the following steps:
1) obtaining tea raw material, described tea raw material includes doing Folium Camelliae sinensis and/or the tea that completes;
2) vapor distillation tea raw material, collects distillate, obtains tea hydrosol,
Alternatively, distillate is carried out concentration.
Second aspect present invention provides the preparation method of a kind of tea essential oil, and it comprises the following steps:
1) obtaining tea raw material, described tea raw material includes doing Folium Camelliae sinensis and/or the tea that completes;
2) vapor distillation tea raw material, collects distillate, obtains tea hydrosol,
Alternatively, distillate is carried out concentration;
3) from 2) tea hydrosol separate (such as extract and separate) tea essential oil.
In one embodiment, the preparation method of the tea hydrosol of any one of the present invention, or the preparation of any one of the present invention
Method, it has a following one or more feature:
A) step 1) in, described in do Folium Camelliae sinensis or tea that the tea that completes is oolong tea tea tree breed;
B) step 1) in, described in do Folium Camelliae sinensis or tea that the tea that completes is Tie Guanyin tea plant kind and/or Wuyi cliff tea Camellia sinensis product
The tea planted;
C) in step 1, described in do Folium Camelliae sinensis or the tea that completes is the tea selected from Radix Campylotropis Hirtella (Herba Myrsines Africanae) tea tree breed, bright fir tea tree breed
One or more in tea, the tea of narcissus tea tree breed, the tea of Cortex Cinnamomi tea tree breed or the strange tea planting tea tree breed;
D) step 2) in, vapor distillation is water distillation, distilling above water or open steam distillation;
E) step 2) in, in wet distillation process, the temperature of steam is 102~110 DEG C;
F) step 2) in, the time of vapor distillation is 1~3h, such as 2.5~3h;
G) step 2) in, vapor distillation every 10~20kg tea, the speed of response of distillate is 20~40kg/h, such as 25
~35kg/h;
H) step 2) in, vapor distillation every 10~20kg tea, the yield of distillate is 50~110kg, such as 60~
105kg;
I) step 2) in, after vapor distillation, also include the step filtering distillate;
J) step 2) in, after vapor distillation, also including the step of microfiltration distillate, used by microfiltration, the aperture of filter membrane is
0.2~1 μm.
In one embodiment, the preparation method of the tea hydrosol of any one of the present invention, or the caffein of any one of the present invention
The preparation method of oil, described concentration is reverse-osmosis treated, and gained reverse osmosis trapped fluid is the tea hydrosol concentrated;
Preferably, during reverse-osmosis treated, the membrane stack pressure of reverse osmosis membrane is 0.8~2MPa, such as 0.8~
1.5MPa;
Preferably, the desalination rate of the reverse osmosis membrane that reverse-osmosis treated uses is 99.0~99.5%;
Preferably, the weight of described trapped fluid is the 5~15% of distillate weight, such as 6~10%.
In one embodiment, the preparation method of the tea hydrosol of any one of the present invention, or the caffein of any one of the present invention
The preparation method of oil, wherein, does Folium Camelliae sinensis and is prepared by the method comprised the following steps:
I. dark brownish green or after withering and processing dark brownish green one or multi-step rocking of green leaf process and the airing of carrying out is processed;
The moisture content doing Folium Camelliae sinensis is preferably 60-70%.
In one embodiment, the preparation method of the tea hydrosol of any one of the present invention, or the caffein of any one of the present invention
The preparation method of oil, wherein, the tea that completes is prepared by the method comprised the following steps:
I. dark brownish green or after withering and processing dark brownish green one or multi-step rocking of green leaf process and the airing of carrying out is processed, it is thus achieved that do green grass or young crops
Tea;
Ii. complete process to doing Folium Camelliae sinensis;
The moisture content of tea of completing is preferably 50~60%.
In one embodiment, the preparation method of the tea essential oil of any one of the present invention, wherein, step 3) include following
3a)~3c) in one or multi-step:
3a) in tea hydrosol, add saturated NaCl solution and ethyl acetate, extraction, it is then peeled off acetic acid ethyl acetate extract;
Alternatively, repeat step 3a) one or many, combined ethyl acetate extract;
3b) acetic acid ethyl acetate extract is carried out the first concentrating under reduced pressure, remove ethyl acetate, obtain tea essential oil;
3c) alternatively, gained tea essential oil is purified further, gained tea essential oil adds ethanol, then carries out second
Concentrating under reduced pressure, removes ethanol, obtains product.
In one embodiment, the preparation method of the tea essential oil of any one of the present invention, it has following one or more
Feature:
K) step 3b) in, the vacuum of the first concentrating under reduced pressure is 200~220mbar;
L) step 3b) in, the temperature of the first concentrating under reduced pressure is preferably 30~40 DEG C;
M) step 3c) in, the vacuum of the second concentrating under reduced pressure is 110~130mbar;
N) step 3c) in, the temperature of the second concentrating under reduced pressure is 35~45 DEG C.
In one embodiment, the preparation method of the tea hydrosol of any one of the present invention, or the caffein of any one of the present invention
The preparation method of oil, it includes following one or multi-step:
(1) Folium Camelliae sinensis or the tea that completes are done in acquisition;
(2) with vapor distillation still to doing Folium Camelliae sinensis or the tea that completes carries out open steam distillation.Under vapor distillation still
Portion is provided with steam entry, and top is provided with steam outlet, inside vapor distillation still, steam entry and outlet it
Between position, be provided with for placing distilland and through the porose sieve plate of steam.Folium Camelliae sinensis will be done or the tea that completes will be placed in water
On the sieve plate of steam distillation still, steam is entered in distillating still by the bottom of distillating still, through sieve plate with do Folium Camelliae sinensis or the tea that completes
Being fully contacted, then the steam outlet from top is derived, and collects after the condensation of condensed device, and it is pure that the distillation collected is tea
Dew I.
(3) Folium Camelliae sinensis or the tea hydrosol that completes are done in filtration, filter off impurity, then use reverse osmosis membrane that micro-filtrate is carried out reverse osmosis
Process, it is thus achieved that reverse osmosis trapped fluid, this reverse osmosis trapped fluid is tea hydrosol II.
(4) in tea hydrosol II, add a certain amount of saturated aqueous common salt, add ethyl acetate, extraction, separate after extraction
Acetic acid ethyl acetate extract.Alternatively, repeatedly extract by above-mentioned steps 1~5 time, combined ethyl acetate extract.
(5) in acetic acid ethyl acetate extract, anhydrous Na is added2SO4Dehydration, then filters off solid NaSO4.To the second after dehydration
Acetoacetic ester extract carries out the first concentrating under reduced pressure, removes ethyl acetate, and steaming excess is tea essential oil I.
(6) dehydrated alcohol can also be added in TIEGUANYIN autumn tea quintessence oil I and carry out the second concentrating under reduced pressure, remove ethanol and
Residual ethyl acetate (if having remnants), steams excess and is tea essential oil II.
In one embodiment, tea hydrosol is tea hydrosol I or tea hydrosol II, and tea essential oil is tea essential oil I or tea essential oil II.
Third aspect present invention provides a kind of tea hydrosol, and it is prepared by the method for any one of the present invention.
Fourth aspect present invention provides a kind of tea essential oil, and it is prepared by the method for any one of the present invention.
Fifth aspect present invention provides the tea hydrosol of any one of the present invention or the tea essential oil of any one of the present invention to use as cigarette
The purposes of essence;
Preferably, described flavouring essence for tobacco refers to for Nicotiana tabacum L., tobacco shred, stem, thin slice, filter tip, tipping paper, cigarette case, electronics
The essence of cigarette.
Sixth aspect present invention provides a kind of Medicated cigarette or a kind of electronic cigarette, its contain any one of the present invention tea hydrosol or
The tea essential oil of any one of the present invention.
General one-tenth is sampled tea to generally go through and is dried for a long time and fermentation process, and the present invention makes to be used as Folium Camelliae sinensis and the tea that completes
It is dried for a long time or fermentation process without above-mentioned.
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, 2002,24 (2): 6-9.
In one embodiment, tea raw material is to do Folium Camelliae sinensis and/or the tea that completes.
In one embodiment, do Folium Camelliae sinensis or the tea that completes is the tea of oolong tea tea tree breed, e.g. Tie Guanyin tea plant
The tea of kind or the tea of Wuyi cliff tea tea tree breed.
In one embodiment, the tea of Wuyi cliff tea tea tree breed refers to the tea of Radix Campylotropis Hirtella (Herba Myrsines Africanae) tea tree breed, bright fir Camellia sinensis
The tea of kind, the tea of narcissus tea tree breed, the tea of Cortex Cinnamomi tea tree breed or the strange tea planting tea tree breed.
In one embodiment, doing Folium Camelliae sinensis is the dark brownish green tea obtained after blue or green process of withering, do.
In one embodiment, the tea that completes is the dark brownish green tea obtained after the green grass or young crops that withers, does, the process that completes.
In one embodiment, dark brownish green or tea fresh leaves 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 one embodiment, process of withering refers to be placed in dark brownish green under illumination, ventilation and/or heating condition, makes tea
Blue or green dehydration is wilted.
In one embodiment, doing blue or green process is under the effect of mechanical force, makes dark brownish green or withered tea leaves edge portion be subject to
Damage, promotes the polyphenols partial oxidation of its intension, polymerization, produces the process on " the red limit of greenery ".
In one embodiment, after doing blue or green process, it is dark green that gained does the stalk base of a fruit of Folium Camelliae sinensis water of satisfying, and vein becomes clear, and mesophyll is yellow
Green, leaf margin becomes vermilion, and the food value of leaf is soft, and blue or green gas disappears, and fragrance is pure, micro-strip flowers and fruits fragrant.
In one embodiment, do blue or green process and include that one or many rocking of green leaf and airing process.
In one embodiment, rocking of green leaf refers to put in big bamboo plaque or vibration machine dark brownish green or withered tea leaves, enters
Pedestrian's work is hand or mechanical drive rocking of green leaf cage rotates, and makes the Folium Camelliae sinensis blade after withering constantly circle round, stirs up and down, allow leaf margin with
Leaf margin, leaf margin mutually rub with compass screen surface, leaf margin cell breakage.Rocking of green leaf can promote that polyphenol compound aoxidizes, and makes tea occur one
Serial physical chemical change.
In one embodiment, the process that completes is to use uniform temperature, makes the enzyme in fresh leaf lose activity, or by enzyme
The process of passivation.
In one embodiment, the mode processed that completes includes: the stir-fry of roller fixation, pot completes, hot air water-removing, steam kill
Blue or green, microwave deactivation of enzyme or steam-hot blast is hybrid completes.
In one embodiment, pot is fried to complete and is referred to, it is simply that ceaselessly stir-fry in the pot of burn-out Folium Camelliae sinensis, in Folium Camelliae sinensis
Moisture be evaporated deliquescing.
In one embodiment, complete and refer to, on the basis of tea is fried, killing, tea is fried the most stiff to limb edge,
Leaf color transfers darker yellow green to, tarnishes, blade face slightly wrinkle, leaf stalk softness, and holding leaf has strong feel, slightly elastic, blue or green
Gas disappears, giving out fragrance.
In one embodiment, the temperature processed that completes can be 80~300 DEG C.
In one embodiment, the tea or be Folium Camelliae sinensis hydrosol I/ of completing of any one during tea hydrosol is following embodiment
II。
In one embodiment, the tea or be Folium Camelliae sinensis tea essential oil I/ of completing of any one during tea essential oil is following embodiment
II。
The invention have the advantages that
1) in some embodiments of the invention, the tea or do Folium Camelliae sinensis and prepare tea hydrosol or tea essential oil, gained tea of completing is used
Hydrosol or tea essential oil have the fragrance of a flower and the delicate fragrance of uniqueness, are highly suitable for as Medicated cigarette/electronic cigarette perfuming;
2) in some embodiments of the invention, the tea or do Folium Camelliae sinensis and prepare tea hydrosol or tea essential oil, with employing of completing is used
Becoming samples tea compares, and preparation section is less, and cost is lower;
3) in some embodiments of the invention, the tea or do Folium Camelliae sinensis and prepare tea hydrosol or tea essential oil, with employing of completing is used
Becoming samples tea compares, and the yield of tea hydrosol or tea essential oil is higher;Such as every kilogram dark brownish green can producing does Folium Camelliae sinensis quintessence oil 0.14~0.18g,
Complete tea essential oil 0.12~0.14g, and every kilogram dark brownish green is only capable of finished product tea essential oil 0.07~0.08g;
4) in some embodiments of the invention, use and include that the method for reverse-osmosis treated prepares tea hydrosol or tea essential oil,
The method treatment temperature is low, is avoided that the volatilization of low-boiling aroma substance, moreover it is possible to reduce change and the loss of heat-sensitive substance,
The tea essential oil prepared has the tea perfume (or spice) feature of uniqueness, is highly suitable for as Medicated cigarette/electronic cigarette essence perfuming;
5) in some embodiments of the invention, employing includes that the method for reverse-osmosis treated prepares tea essential oil, the method institute
The amount of the extractant needed is less;
6) method in some embodiments of the invention, preparing tea hydrosol or tea essential oil, it is possible in the short period of time
Collect more volatile ingredient and nerolidol;
7) in some embodiments of the invention, the method preparing tea hydrosol or tea essential oil, the concentration speed of reverse-osmosis treated
Rate is very fast, and equipment moderate pressure, in trapped fluid, volatile ingredient concentration is higher.
Accompanying drawing explanation
Accompanying drawing described herein is used for providing a further understanding of the present invention, constitutes the part of the application, this
Bright schematic description and description is used for explaining the present invention, is not intended that limitation of the invention.In the accompanying drawings:
Fig. 1 is the total ion current figure that TIEGUANYIN autumn tea is cooked Folium Camelliae sinensis quintessence oil;
Fig. 2 is that TIEGUANYIN autumn tea completes the total ion current figure of tea essential oil;
Fig. 3 is the total ion current figure of TIEGUANYIN autumn tea finished product tea essential oil.
Detailed description of the invention
Below by drawings and Examples, technical scheme is described in further detail.
Embodiment 1
(1) 20kg TIEGUANYIN autumn tea fresh leaves (the most dark brownish green) is plucked, and after blue or green process of withering, do, it is thus achieved that the TIEGUANYIN autumn
Tea is Folium Camelliae sinensis 15kg.
(2) with vapor distillation still, TIEGUANYIN autumn tea is cooked Folium Camelliae sinensis and carry out open steam distillation.Vapor distillation still
Bottom is provided with steam entry, and top is provided with steam outlet, inside vapor distillation still, steam entry and outlet
Between position, be provided with for placing distilland and through the porose sieve plate of steam.15kg TIEGUANYIN autumn tea is cooked green grass or young crops
Tea is placed on the sieve plate of vapor distillation still, and steam (temperature about 105 DEG C) is entered in distillating still by the bottom of distillating still, passes through
Sieve plate does Folium Camelliae sinensis with TIEGUANYIN autumn tea and is fully contacted, and then the steam outlet from top is derived, condensed device (condenser temperature
Spend-5~10 DEG C) condensation after collect, the distillation collected is TIEGUANYIN autumn tea and is Folium Camelliae sinensis hydrosol I.Total distillation time is about
2.5h, the speed of response of distillation is about 25kg/h, and distillation total collection is about 62.5kg.
(3) the micro-filtrate membrane filtration TIEGUANYIN autumn tea using 0.2 μm aperture is cooked Folium Camelliae sinensis hydrosol, filters off impurity, obtains microfiltration and pass through
Liquid (about 60.0kg).Then use reverse osmosis membrane (GE HWS RO 8040HR, salt rejection rate NaCl 99.5%) to microfiltration permeate
Carrying out reverse-osmosis treated, membrane stack pressure is 0.8MPa, keeps temperature of liquid 20~30 by cooling water recirculation system during process
Between DEG C, it is thus achieved that reverse osmosis trapped fluid the most about 5kg (being equivalent to 8.3% for microfiltration permeate weight).This reverse osmosis retains
Liquid is TIEGUANYIN autumn tea and is Folium Camelliae sinensis hydrosol II.
(4) in TIEGUANYIN autumn tea is cooked Folium Camelliae sinensis hydrosol II, add a certain amount of saturated aqueous common salt, add 1.5kg acetic acid second
Ester (is equivalent to above-mentioned TIEGUANYIN autumn tea and does the 30% of Folium Camelliae sinensis hydrosol II weight), extraction, separating ethyl acetate extract after extraction.
Repeatedly extract by above-mentioned steps 5 times, combined ethyl acetate extract, obtain acetic acid ethyl acetate extract 6.80kg altogether.
(5) in acetic acid ethyl acetate extract, anhydrous Na is added2SO4Dehydration, then filters off solid NaSO4.To the second after dehydration
Acetoacetic ester 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 remaining
Thing is that TIEGUANYIN autumn tea is cooked Folium Camelliae sinensis quintessence oil I, and weight is 5.0g.
(6) about 15.0g dehydrated alcohol can also be added in TIEGUANYIN autumn tea quintessence oil I and (be equivalent to TIEGUANYIN autumn tea essence
3 times of oil I weight) carry out the second concentrating under reduced pressure, vapo(u)rizing temperature is 40 DEG C, and vacuum is 120mbar, removes ethanol and remaining second
Acetoacetic ester (if having remnants), steaming excess is TIEGUANYIN autumn tea and is Folium Camelliae sinensis quintessence oil II, and weight is 2.90g, relative to doing Folium Camelliae sinensis
Yield be 0.19 ‰, be 0.14 ‰ relative to dark brownish green yield.
Embodiment 2
(1) 27.0kg TIEGUANYIN spring tea fresh leaves (the most dark brownish green) is plucked, and after the green grass or young crops that withers, does, the process that completes, it is thus achieved that
15kg TIEGUANYIN spring tea completes tea.
(2) open steam distillation is carried out with vapor distillation still TIEGUANYIN spring tea completed tea.Vapor distillation still
Bottom is provided with steam entry, and top is provided with steam outlet, inside vapor distillation still, steam entry and outlet
Between position, be provided with for placing distilland and through the porose sieve plate of steam.15kg TIEGUANYIN spring tea is completed
Tea is placed on the sieve plate of vapor distillation still, and steam is entered in distillating still by the bottom of distillating still, through sieve plate and TIEGUANYIN
The spring tea tea that completes is fully contacted, and then the steam outlet from top is derived, and condensed device (condenser temperature-5~10 DEG C) is cold
Collecting after Ning, the distillation collected is TIEGUANYIN spring tea and completes tea hydrosol I.Total distillation time is about 2.5h, distillation
The speed of response is about 30kg/h, and distillation total collection is about 75.0kg.
(3) the micro-filtrate membrane filtration TIEGUANYIN spring tea using 0.8 μm aperture completes tea hydrosol, filters off impurity, obtains microfiltration and pass through
Liquid (about 72.0kg).Then use reverse osmosis membrane (GE HWS RO 8040HR) that microfiltration permeate is carried out reverse-osmosis treated, film
Heap pressure is 1.0MPa, during process by cooling water recirculation system keep temperature of liquid between 20~30 DEG C, it is thus achieved that reverse osmosis
Trapped fluid the most about 7.2kg (being equivalent to 10% for microfiltration permeate weight) thoroughly.This reverse osmosis trapped fluid is TIEGUANYIN spring tea
Complete tea hydrosol II.
(4) in TIEGUANYIN spring tea completes tea hydrosol II, add a certain amount of saturated aqueous common salt, add 2.25kg acetic acid
Ethyl ester (be equivalent to above-mentioned TIEGUANYIN spring tea complete the 30% of tea hydrosol II weight), extraction, separating ethyl acetate extraction after extraction
Liquid.Repeatedly extract by above-mentioned steps 6 times, combined ethyl acetate extract, obtain acetic acid ethyl acetate extract 12.8kg altogether.
(5) in acetic acid ethyl acetate extract, anhydrous Na is added2SO4Dehydration, then filters off solid NaSO4.To the second after dehydration
Acetoacetic ester 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 remaining
Thing is that TIEGUANYIN spring tea completes tea essential oil I, and weight is 5.5g.
(6) 16.5g dehydrated alcohol can also be added in TIEGUANYIN spring tea quintessence oil I and (be equivalent to TIEGUANYIN spring tea quintessence oil I
3 times of weight), carry out the second concentrating under reduced pressure, vapo(u)rizing temperature is 40 DEG C, and vacuum is 120mbar, removes ethanol and Residual acetic acid
Ethyl ester (if there is), steams excess and is TIEGUANYIN spring tea and completes tea essential oil II, and weight is 3.50g, relative to the yield of the tea that completes
Yield is 0.23 ‰, is 0.13 ‰ relative to dark brownish green yield.
Embodiment 3
(1) 27.0kg TIEGUANYIN autumn tea fresh leaves (the most dark brownish green) is plucked, and after the green grass or young crops that withers, does, the process that completes, it is thus achieved that
15kg TIEGUANYIN autumn tea completes tea.
(2) open steam distillation is carried out with vapor distillation still TIEGUANYIN autumn tea completed tea.Vapor distillation still
Bottom is provided with steam entry, and top is provided with steam outlet, inside vapor distillation still, steam entry and outlet
Between position, be provided with for placing distilland and through the porose sieve plate of steam.15kg TIEGUANYIN autumn tea is completed
Tea is placed on the sieve plate of vapor distillation still, and steam is entered in distillating still by the bottom of distillating still, through sieve plate and TIEGUANYIN
The autumn tea tea that completes is fully contacted, and then the steam outlet from top is derived, and condensed device (condenser temperature-5~10 DEG C) is cold
Collecting after Ning, the distillation collected is TIEGUANYIN autumn tea and completes tea hydrosol I.Total distillation time is about 3.0h, distillation
The speed of response is about 35kg/h, and distillation total collection is about 105.0kg.
(3) the micro-filtrate membrane filtration TIEGUANYIN autumn tea using 0.5 μm aperture completes tea hydrosol, filters off impurity, obtains microfiltration and pass through
Liquid (about 103.0kg).Then use reverse osmosis membrane (GE HWS RO 8040HR) that microfiltration permeate is carried out reverse-osmosis treated, film
Heap pressure is 1.0MPa, during process by cooling water recirculation system keep temperature of liquid between 20~30 DEG C, it is thus achieved that reverse osmosis
Trapped fluid the most about 6.3kg (being equivalent to 6.1% for microfiltration permeate weight) thoroughly.This reverse osmosis trapped fluid is TIEGUANYIN autumn tea
Complete tea hydrosol II.
(4) in TIEGUANYIN autumn tea completes tea hydrosol II, add a certain amount of saturated aqueous common salt, add 1.89kg acetic acid
Ethyl ester (be equivalent to above-mentioned TIEGUANYIN autumn tea complete the 30% of tea hydrosol II weight), extraction, separating ethyl acetate extraction after extraction
Liquid.Repeatedly extract by above-mentioned steps 6 times, combined ethyl acetate extract, obtain acetic acid ethyl acetate extract 10.0kg altogether.
(5) in acetic acid ethyl acetate extract, anhydrous Na is added2SO4Dehydration, then filters off NaSO4.To the acetic acid second after dehydration
Ester 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 and is
TIEGUANYIN autumn tea completes tea essential oil I, and weight is 5.60g.
(6) about 16.8g dehydrated alcohol can also be added in TIEGUANYIN autumn tea quintessence oil I (to be equivalent to TIEGUANYIN autumn tea kill
3 times of Folium Camelliae sinensis quintessence oil I weight), carry out the second concentrating under reduced pressure, vapo(u)rizing temperature is 40 DEG C, and vacuum is 120mbar, removes ethanol
With Residual ethyl acetate (if there is), steaming excess and be TIEGUANYIN autumn tea and do Folium Camelliae sinensis and complete tea essential oil II, weight is 3.20g, phase
Yield for the tea that completes is 0.21 ‰, is 0.12 ‰ relative to dark brownish green yield.
Embodiment 4
(1) 28.0kg Cortex Cinnamomi tea fresh leaves (the most dark brownish green) is plucked, and after the green grass or young crops that withers, does, the process that completes, it is thus achieved that cinnamon tea
Complete tea.
(2) open steam distillation is carried out with vapor distillation still cinnamon tea completed tea.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.The tea that 15kg cinnamon tea completed is placed in water
On the sieve plate of steam distillation still, steam is entered in distillating still by the bottom of distillating still, fills through sieve plate and the cinnamon tea tea that completes
Tap is touched, and then the steam outlet from top is derived, and collects, collect after condensed device (condenser temperature-5~10 DEG C) condensation
To distillation be and do cinnamon tea and complete tea hydrosol I.Total distillation time is about 3.0h, and the speed of response of distillation is about
30kg/h, distillation total collection is about 90.0kg.
(3) the micro-filtrate membrane filtration cinnamon tea using 1.0 μm apertures completes tea hydrosol, filters off impurity, obtains microfiltration permeate (about
87.5kg).Then use reverse osmosis membrane (GE HWS RO 8040HR) that microfiltration permeate carries out reverse-osmosis treated, membrane stack pressure
For 1.0MPa, during process, keep temperature of liquid between 20~30 DEG C by cooling water recirculation system, it is thus achieved that reverse osmosis retain
Liquid the most about 8.0kg (is equivalent to 9.1% for microfiltration permeate weight).This reverse osmosis trapped fluid is cinnamon tea and completes tea hydrosol
II。
(4) in cinnamon tea completes tea hydrosol II, add a certain amount of saturated aqueous common salt, add 2.0kg ethyl acetate
(be equivalent to above-mentioned cinnamon tea complete the 25% of tea hydrosol II weight), 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 11.2kg altogether.
(5) in acetic acid ethyl acetate extract, anhydrous Na is added2SO4Dehydration, then filters off NaSO4.To the acetic acid second after dehydration
Ester 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 and is
Cinnamon tea completes tea essential oil I, and weight is 5.8g.
(6) about 17.4g dehydrated alcohol can also be added in cinnamon tea quintessence oil I and (be equivalent to cinnamon tea quintessence oil I weight
3 times), carry out the second concentrating under reduced pressure, vapo(u)rizing temperature is 40 DEG C, and vacuum is 120mbar, removes ethanol and Residual ethyl acetate,
Steaming excess to be cinnamon tea and complete tea essential oil II, weight is 3.8g, is 0.25 ‰ relative to the yield of the tea that completes, relative to dark brownish green
Yield be 0.14 ‰.
Comparative example 1
(1) pluck TIEGUANYIN autumn tea fresh leaves (the most dark brownish green), and after the green grass or young crops that withers, does, the process that completes, it is thus achieved that the TIEGUANYIN autumn
Tea completes tea.
(2) open steam distillation is carried out with vapor distillation still TIEGUANYIN autumn tea completed tea.Vapor distillation still
Bottom is provided with steam entry, and top is provided with steam outlet, inside vapor distillation still, steam entry and outlet
Between position, be provided with for placing distilland and through the porose sieve plate of steam.15kg TIEGUANYIN autumn tea is completed
Tea is placed on the sieve plate of vapor distillation still, and steam is entered in distillating still by the bottom of distillating still, through sieve plate and TIEGUANYIN
The autumn tea tea that completes is fully contacted, and then the steam outlet from top is derived, and condensed device (condenser temperature-5~10 DEG C) is cold
Collecting after Ning, the distillation collected is TIEGUANYIN autumn tea and completes tea hydrosol Ia.Total distillation time is about 2.5h, distillation
The speed of response is about 35kg/h, and distillation total collection is about 87.5kg.Throw two batch raw materials simultaneously, prepare two batch TIEGUANYIN
Autumn tea completes the contrast for condensing mode of the tea hydrosol.
(3) concentrating under reduced pressure: utilize concentrating under reduced pressure equipment TIEGUANYIN autumn tea is completed tea hydrosol Ia to carry out concentrating under reduced pressure, steam
Valve opening 70, pressure-0.82bar, vapor (steam) temperature 60 DEG C, feeding temperature 38 DEG C, separator temperature 50 DEG C, feed rate
0.2m3/ h, circulating temperature 50 DEG C, evaporate flow 130L/h, circular flow 1620Kg/h.Gained decompressed concentrate is TIEGUANYIN
Autumn tea completes tea hydrosol IIa.
Comparative example 2
(1) pluck 60.0kg TIEGUANYIN autumn tea fresh leaves (the most dark brownish green), and through withering, do green grass or young crops, complete, rolling and drying etc.
After process, make TIEGUANYIN autumn tea and become the 15kg that samples tea.
(2) become to sample tea and carry out open steam distillation to TIEGUANYIN autumn tea with vapor distillation still.Vapor distillation still
Bottom is provided with steam entry, and top is provided with steam outlet, inside vapor distillation still, steam entry and outlet
Between position, be provided with for placing distilland and through the porose sieve plate of steam.By 15kg TIEGUANYIN autumn tea finished product
Tea is placed on the sieve plate of vapor distillation still, and steam is entered in distillating still by the bottom of distillating still, through sieve plate and TIEGUANYIN
Autumn tea one-tenth is sampled tea and is fully contacted, and then the steam outlet from top is derived, and condensed device (condenser temperature-5~10 DEG C) is cold
Collecting after Ning, the distillation collected is TIEGUANYIN autumn tea and becomes the hydrosol Ib that samples tea.Total distillation time is about 3.0h, distillation
The speed of response is about 30kg/h, and distillation total collection is about 90.0kg.
(3) the micro-filtrate membrane filtration TIEGUANYIN autumn tea using 0.8 μm aperture becomes the hydrosol Ib that samples tea, and filters off impurity, obtains microfiltration saturating
Cross liquid (about 87.0kg).Then using reverse osmosis membrane that microfiltration permeate carries out reverse-osmosis treated, membrane stack pressure is 1.0MPa, place
During reason by cooling water recirculation system keep temperature of liquid between 20~30 DEG C, it is thus achieved that reverse osmosis trapped fluid the most about 7.0kg
(being equivalent to 8.0% for microfiltration permeate weight).This reverse osmosis trapped fluid is TIEGUANYIN autumn tea and becomes the hydrosol IIb that samples tea.
(4) in TIEGUANYIN autumn tea becomes the hydrosol IIb that samples tea, add a certain amount of saturated aqueous common salt, add 2.1kg acetic acid
Ethyl ester (is equivalent to above-mentioned TIEGUANYIN autumn tea and becomes the 30% of hydrosol IIb weight of sampling tea), extraction, separating ethyl acetate extraction after extraction
Liquid.Repeatedly extract by above-mentioned steps 6 times, combined ethyl acetate extract, obtain acetic acid ethyl acetate extract 12.0kg altogether.
(5) in acetic acid ethyl acetate extract, anhydrous Na is added2SO4Dehydration, then filters off NaSO4.To the acetic acid second after dehydration
Ester 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 and is
TIEGUANYIN autumn tea finished product tea essential oil Ib, weight is 10.25g.
(6) about 16.8g dehydrated alcohol can also be added in TIEGUANYIN autumn tea finished product tea essential oil Ib and (be equivalent to TIEGUANYIN
3 times of autumn tea finished product tea essential oil Ib weight), carry out the second concentrating under reduced pressure, vapo(u)rizing temperature is 40 DEG C, and vacuum is 120mbar, removes
Going ethanol and Residual ethyl acetate (if there is), steaming excess to be TIEGUANYIN autumn tea and become the tea essential oil IIb that samples tea, weight is 5.20g,
It is 0.35 ‰ relative to becoming the yield sampled tea, is 0.08 ‰ relative to dark brownish green yield.
The tea essential oil II of embodiment 1~4 is 0.12~0.14 ‰ relative to dark brownish green yield, and the tea essential oil of comparative example 2
II is only 0.08 ‰ relative to dark brownish green yield.The yield that the method for this explanation employing embodiment 1~4 prepares tea essential oil is higher.
Analysis detection 1: derived essential oil analysis
Use in the tea essential oil II of Gas Chromatography/Mass Spectrometric Method detection embodiment 1, the 3 and tea essential oil IIb of comparative example 2
Chemical composition.Testing conditions is as follows:
Extraction conditions: accurately weigh a certain amount of tea essential oil sample, uses dichloromethane extraction, and nitrogen blows concentration, adds second
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.TIEGUANYIN autumn tea is cooked Folium Camelliae sinensis quintessence oil, TIEGUANYIN autumn tea completes tea essential oil, TIEGUANYIN autumn tea
The total ion current figure of finished product tea essential oil is respectively Fig. 1, Fig. 2 and Fig. 3, uses area normalization method to calculate the percentage ratio of each component,
Result is as shown in table 1.
Table 1
As shown in table 1, compared to TIEGUANYIN autumn tea finished product tea essential oil, TIEGUANYIN autumn tea is cooked in Folium Camelliae sinensis quintessence oil: Multiple components
Content the highest, the content of such as phenethanol and benzyl alcohol is higher;TIEGUANYIN autumn tea completes in tea essential oil: containing of Multiple components
Measuring the highest, the such as content of benzyl alcohol, 1-Phenylethanone., indole and nerolidol is higher.
Phenethanol has: gentle hyacinth-Fructus Gardeniae fragrance, flower, earth, Mel fragrance, the taste of fruit sample.
Benzyl alcohol has: faint, sweet, the fragrance of fruity, distinctive pleasant fruit aroma.Indole has: have close to jasmine
The fragrance of the jasmine fragrance of a flower.Nerolidol has: be similar to the faint fragrance of a flower of Flos Rosae Rugosae and Fructus Mali pumilae, the sweetest, the freshest, persistently
Fragrance.1-Phenylethanone. has: have note as May bloom fragrance, Acacia farnesiana Willd. and Herba Mimosae Pudicae.
The mentioned component content that TIEGUANYIN autumn tea is cooked Folium Camelliae sinensis quintessence oil and TIEGUANYIN autumn tea completes in tea essential oil higher it was confirmed
TIEGUANYIN autumn tea is cooked Folium Camelliae sinensis quintessence oil and TIEGUANYIN autumn tea completes, and tea essential oil has the more prominent fragrance of a flower and/or delicate fragrance.
Analysis detection 2: the different condensing mode impacts on volatile ingredient
For embodiment 3, (i.e. TIEGUANYIN autumn tea kills to collect the reverse osmosis trapped fluid sample of reverse-osmosis treated in step (3)
Folium Camelliae sinensis hydrosol II) and reverse osmosis permeate sample.For comparative example 1, collect the concentrated solution sample of concentrating under reduced pressure in step (3)
(i.e. TIEGUANYIN autumn tea complete tea hydrosol IIa) and the distillate sample of concentrating under reduced pressure.Above-mentioned sample respectively pipettes 2.0ml, adds
0.4ml saturated nacl aqueous solution, carries out its volatile fragrant components of HS GC-mass spectral analysis.Head space condition is: PE
TurboMatrix 40 Static Headspace instrument, 20ml ml headspace bottle, Sample equilibration temperature 90 DEG C, equilibration time 60min, sample introduction needle temperature
100 DEG C, transmission line temperature 120 DEG C, sample bottle 1.0min pressing time, sample injection time 0.06min, pull out pin time 0.50min, enter
Original mold formula: high pressure sample introduction.Gas chromatography-mass spectrum testing conditions is with analyzing detection 1, and analysis result is as shown in table 2 below.
The contrast of the different condensing mode of table 2
As seen in Table 2, TIEGUANYIN autumn tea completes the volatile component content of tea hydrosol II (embodiment 3) apparently higher than Tie Guan
Sound autumn tea completes tea hydrosol IIa (comparative example 1), and the volatile component content of reverse osmosis permeate (embodiment 3) is the lowest
Distillate (comparative example 1) in concentrating under reduced pressure.The reverse osmosis concentration that this explanation embodiment 3 uses can retain more volatility
Composition is in concentrated solution (TIEGUANYIN autumn tea complete tea hydrosol II), and comparative example 1 uses the method volatile ingredient of concentrating under reduced pressure
Loss is big.
Analysis detection 3: the selection of vapor distillation time
During embodiment 3 prepares dark brownish green hydrosol, start every 10min collection 1 in chronological order from distillation and distillate
Liquid sample, 3h collects 18 samples altogether.Each sample pipettes 2.0ml, add 0.4ml saturated nacl aqueous solution carry out head space-
Gas chromatography-mass spectrometry analysis, test condition is as analyzed detection 2.
Volatile ingredient concentration (C1, unit mg/g) in hydrosol, nerolidol concentration (C2, unit in hydrosol
Mg/g) data changed with distillation time (unit: minute) are as shown in table 3.According to table 3, prolongation over time, in hydrosol
The concentration of volatile ingredient (and nerolidol) is gradually lowered, and in hydrosol, the content of volatile ingredient (and nerolidol) gradually rises
Height also tends to be steady.This explanation, when the time of vapor distillation is 2~3h (preferably 2.5h), it is possible in the short period of time
Collect more volatile ingredient and nerolidol.
Table 3
Analyze detection 4: the permeable membrane pressure of reverse-osmosis treated selects
During dark brownish green hydrosol in preparing above-described embodiment, when using reverse osmosis membrane to concentrate dark brownish green hydrosol, adjust reverse osmosis membrane
Go out film pressure be respectively 0.1,0.2,0.3,0.5,0.8,1.0,1.5,2.0MPa, under each pressure, stable being followed by negates infiltration thoroughly
Cross liquid, use HS GC-mass spectral analysis (head space, gas chromatogram and Mass Spectrometry Conditions are with analyzing detection 1) to investigate permeate
The concentration (C3, unit mg/g) of middle volatile ingredient,
And concentrating speed (S1, units/kg/h), result is as shown in table 4.
Table 4
Pressure/MPa | 0.1 | 0.2 | 0.3 | 0.5 | 0.8 | 1.0 | 1.5 | 2.0 |
C3 | 0.0007 | 0.0008 | 0.0008 | 0.0009 | 0.0011 | 0.0011 | 0.0011 | 0.0011 |
R3 | 7.05 | 8.33 | 8.53 | 9.38 | 11.13 | 11.19 | 11.18 | 11.91 |
S1 | 5.80 | 8.29 | 10.23 | 13.61 | 18.61 | 21.77 | 27.31 | 35.04 |
As table 4 result shows, when pressure is less than 0.8MPa, with the increase permeate volatile ingredient concentration of pressure
(C3) volatile component content is gradually increased with the percentage ratio (R3) of volatile component content in trapped fluid and in permeate;When
After pressure reaches 0.8MPa, with the basic held stationary of increase C3 and R3 of pressure.Additionally, concentrate speed (S1) with the increase of pressure
It is gradually increased.When reverse osmosis membrane stack pressure is 0.8-1.5MPa, concentrate speed very fast, equipment moderate pressure, volatilizees in trapped fluid
Property constituent concentration is higher.
Analysis detection 5: quintessence oil organoleptic analysis
To embodiment 1~4 and the tea essential oil of comparative example 1~2 smell fragrant analysis respectively.Analysis result is as shown in table 5 below.
Table 5
Analysis detection 6: Sensory Quality of Cigarette evaluation
The tea hydrosol II of embodiment 1~4, the tea essential oil II of embodiment 1~4, the tea essential oil IIb of comparative example 2 are put on
Medicated cigarette, carries out Sensory Quality of Cigarette evaluation with blank sample according to national standard (GB5606.4-2005), and marking is evaluated such as table 6
Shown in, describe and evaluate as shown in table 7.
By the tea hydrosol II of embodiment 1~4, be diluted to the edible ethanol that mass fraction is 70% 10% perfuming molten
Liquid, and be uniformly sprayed onto on tobacco shred by the 0.1% of tobacco shred weight, processing technique rolls into Medicated cigarette routinely.By embodiment 1~4
Tea essential oil II and the edible ethanol that tea essential oil IIb mass fraction is 70% of comparative example 2 be diluted to 0.4% perfuming molten
Liquid, is uniformly sprayed onto on tobacco shred by the 0.2% of tobacco shred weight, and technique rolls into Medicated cigarette routinely.
The Medicated cigarette numbering of the tea hydrosol II containing embodiment 1~4 is respectively A1~A4, containing the tea essential oil of embodiment 1~4
The numbered C2 of Medicated cigarette of numbered B1~B4 of Medicated cigarette of II, the tea essential oil IIb containing comparative example 2.
Table 6
Table 7
From the analysis of table 6, the score of Medicated cigarette A1~A4, Medicated cigarette B1~B4 and Medicated cigarette C1 is higher than blank Medicated cigarette, Medicated cigarette
A1~A4, the score of Medicated cigarette B1~B4 are higher than Medicated cigarette C2.
From the analysis of table 7, the evaluation of Medicated cigarette A1~A4, Medicated cigarette B1~B4 and Medicated cigarette C1 is better than blank Medicated cigarette, Medicated cigarette
A1~A4, the evaluation of Medicated cigarette B1~B4 are better than Medicated cigarette C2.
Finally should be noted that: above example is only in order to illustrate that technical scheme is not intended to limit;To the greatest extent
The present invention has been described in detail by pipe with reference to preferred embodiment, and those of ordinary skill in the field are it is understood that still
The detailed description of the invention of the present invention can be modified or portion of techniques feature is carried out equivalent;Without deviating from this
The spirit of bright technical scheme, it all should be contained in the middle of the technical scheme scope that the present invention is claimed.
Claims (12)
1. a preparation method for tea hydrosol, it comprises the following steps:
1) obtaining tea raw material, described tea raw material includes doing Folium Camelliae sinensis and/or the tea that completes;
2) tea raw material described in vapor distillation, collects distillate, obtains tea hydrosol,
Alternatively, distillate is carried out concentration.
2. a preparation method for tea essential oil, it comprises the following steps:
1) obtaining tea raw material, described tea raw material includes doing Folium Camelliae sinensis and/or the tea that completes;
2) tea raw material described in vapor distillation, collects distillate, obtains tea hydrosol,
Alternatively, distillate is carried out concentration;
3) from 2) tea hydrosol separate (such as extract and separate) tea essential oil.
3. the preparation method of the tea hydrosol of claim 1, or the preparation method of the tea essential oil of claim 2, it has with next
Item or multinomial feature:
A) step 1) in, described in do Folium Camelliae sinensis or tea that the tea that completes is oolong tea tea tree breed;
B) step 1) in, described in do Folium Camelliae sinensis or tea that the tea that completes is Tie Guanyin tea plant kind and/or Wuyi cliff tea tea tree breed
Tea;
C) in step 1, described in do Folium Camelliae sinensis or the tea that completes is the tea selected from Radix Campylotropis Hirtella (Herba Myrsines Africanae) tea tree breed, the tea of bright fir tea tree breed, water
One or more in the celestial tea of tea tree breed, the tea of Cortex Cinnamomi tea tree breed or the strange tea planting tea tree breed;
D) step 2) in, vapor distillation is water distillation, distilling above water or open steam distillation;
E) step 2) in, in wet distillation process, the temperature of steam is 102~110 DEG C;
F) step 2) in, the time of vapor distillation is 1~3h, such as 2.5~3h;
G) step 2) in, vapor distillation every 10~20kg tea, the speed of response of distillate is 20~40kg/h, such as 25~
35kg/h;
H) step 2) in, vapor distillation every 10~20kg tea, the yield of distillate is 50~110kg, such as 60~105kg;
I) step 2) in, after vapor distillation, also include the step filtering distillate;
J) step 2) in, after vapor distillation, also including the step of microfiltration distillate, the aperture of filter membrane used by microfiltration is 0.2~1
μm。
4. the preparation method of the tea hydrosol of claim 1, or the preparation method of the tea essential oil of claim 2, described concentration
For reverse-osmosis treated, gained reverse osmosis trapped fluid is the tea hydrosol concentrated;
Preferably, during reverse-osmosis treated, the membrane stack pressure of reverse osmosis membrane is 0.8~2MPa, such as 0.8~1.5MPa;
Preferably, the desalination rate of the reverse osmosis membrane that reverse-osmosis treated uses is 99.0~99.5%;
Preferably, the weight of described trapped fluid is the 5~15% of distillate weight, such as 6~10%.
5. the preparation method of the tea hydrosol of claim 1, or the preparation method of the tea essential oil of claim 2, wherein, do Folium Camelliae sinensis by
The method comprised the following steps prepares:
I. dark brownish green or after withering and processing dark brownish green one or multi-step rocking of green leaf process and the airing of carrying out is processed;
The moisture content doing Folium Camelliae sinensis is preferably 60-70%.
6. the preparation method of the tea hydrosol of claim 1, or the preparation method of the tea essential oil of claim 2, wherein, complete tea by
The method comprised the following steps prepares:
I. dark brownish green or after withering and processing dark brownish green one or multi-step rocking of green leaf process and the airing of carrying out is processed, it is thus achieved that do Folium Camelliae sinensis;
Ii. complete process to doing Folium Camelliae sinensis;
The moisture content of tea of completing is preferably 50~60%.
7. the preparation method of the tea essential oil of claim 2, wherein, step 3) include following 3a)~3c) in one or multi-step:
3a) in tea hydrosol, add saturated NaCl solution and ethyl acetate, extraction, it is then peeled off acetic acid ethyl acetate extract;
Alternatively, repeat step 3a) one or many, combined ethyl acetate extract;
3b) acetic acid ethyl acetate extract is carried out the first concentrating under reduced pressure, remove ethyl acetate, obtain tea essential oil;
3c) alternatively, gained tea essential oil is purified further, gained tea essential oil adds ethanol, then carries out the second decompression
Concentrate, remove ethanol, obtain product.
8. the preparation method of the tea essential oil of claim 7, it has a following one or more feature:
K) step 3b) in, the vacuum of the first concentrating under reduced pressure is 200~220mbar;
L) step 3b) in, the temperature of the first concentrating under reduced pressure is preferably 30~40 DEG C;
M) step 3c) in, the vacuum of the second concentrating under reduced pressure is 110~130mbar;
N) step 3c) in, the temperature of the second concentrating under reduced pressure is 35~45 DEG C.
9. a tea hydrosol, it is prepared by the method for any one of claim 1,3~6.
10. a tea essential oil, it is prepared by the method for any one of claim 2~8.
The tea hydrosol of 11. claim 9 or the tea essential oil of claim 10 are as the purposes of flavouring essence for tobacco;
Preferably, described flavouring essence for tobacco refers to for Nicotiana tabacum L., tobacco shred, stem, thin slice, filter tip, tipping paper, cigarette case, electronic cigarette
Essence.
12. 1 kinds of Medicated cigarette or a kind of electronic cigarette, its tea hydrosol containing claim 9 or the tea essential oil of claim 10.
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Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103484248A (en) * | 2013-09-27 | 2014-01-01 | 福建中烟工业有限责任公司 | Tea flower essence with fresh and sweet characteristics, and application of essence in cigarettes |
-
2016
- 2016-07-18 CN CN201610564959.7A patent/CN105950298B/en active Active
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103484248A (en) * | 2013-09-27 | 2014-01-01 | 福建中烟工业有限责任公司 | Tea flower essence with fresh and sweet characteristics, and application of essence in cigarettes |
Non-Patent Citations (1)
Title |
---|
陈林等: "做青工艺对乌龙茶香气组成化学模式的影响", 《茶叶科学》 * |
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