CN107474963A - A kind of cordate houttuynia essential oil cigarette is with quick-fried pearl and preparation method thereof - Google Patents
A kind of cordate houttuynia essential oil cigarette is with quick-fried pearl and preparation method thereof Download PDFInfo
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- CN107474963A CN107474963A CN201710778053.XA CN201710778053A CN107474963A CN 107474963 A CN107474963 A CN 107474963A CN 201710778053 A CN201710778053 A CN 201710778053A CN 107474963 A CN107474963 A CN 107474963A
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- Prior art keywords
- cordate houttuynia
- essential oil
- preparation
- quick
- extraction
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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
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
-
- 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
- A24D3/14—Use of materials for tobacco smoke filters of organic materials as additive
-
- 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
- C11B9/025—Recovery by solvent extraction
-
- 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
Include the steps such as cordate houttuynia pretreatment, extraction, separation and dripping with quick-fried pearl and preparation method thereof, the preparation method the present invention relates to a kind of cordate houttuynia essential oil cigarette.The present invention is had extraction efficiency height, is easily isolated, non-thermal technology, energy-conservation, low cost and other advantages using subcritical fluids extractive technique extraction cordate houttuynia essence.The cigarette is become apparent and comprehensively with quick-fried pearl essence to the improvement of cigarette smoking quality compared with control sample, fragrance enriches, with pungent fragrant, herbal, and oral stimulation weakens, while alleviates throat's sense of discomfort, obvious to increase sense of promoting the production of body fluid, integral suction quality is obviously improved.
Description
【Technical field】
The invention belongs to flavouring essence for tobacco extractive technique field.More particularly it relates to a kind of cordate houttuynia essential oil cigarette is used
Quick-fried pearl, further relate to preparation method of the cordate houttuynia essential oil cigarette with quick-fried pearl.
【Background technology】
Cordate houttuynia is a kind of wild plant of integration of drinking and medicinal herbs, has clearing heat and detoxicating, detumescence and apocenosis, relieving cough and reducing sputum and other effects.
Volatile oil is the primary efficacy material of cordate houttuynia, and it is for the infection of the upper respiratory tract, bronchitis, pneumonia, chronic bronchitis, hundred
Day cough etc. has the effect of preferable；(methyl is just for decanoyl acetaldehyde (decanoy acetaldehyde), the methyln nonyl ketone that the effect is rich in cordate houttuynia
Nonanone), lauryl aldehyde, the aldoketones such as capraldehyde and ter penoidses have substantial connection.Cordate houttuynia is processed can to prepare high-quality
Volatile oil material, these volatile oil materials can be used for exploitation and used with the cigarette that throat is uncomfortable, function is reduced internal heat in anti-inflammatory is extenuated
Quick-fried pearl capsule, wide market.
At present, essential oil extraction method is a variety of just like solvent extraction, steam distillation, supercritical fluid extraction etc.
Method.Solvent extraction cost is higher, is easily introduced impurity, and its process is numerous and diverse and easily causes the loss of volatile oil, and easily exists
Dissolvent residual, do not use typically；Steam distillation, recovery rate are relatively low；CO2Supercritical fluid extraction, technique is simple, extraction
Efficiency high, no solvent residue, temperature is low, is advantageous to protect the bioactivity of target substance, but the technique needs high-tension apparatus, skill
Art requires high, and cost of equipment investment is big, using also not universal.CO2The major defect of means of supercritical extraction is that operating pressure is too high.
The problem of existing for above-mentioned supercritical extraction technique, it is to solve this to ask to screen new low pressure critical pressure extractant
One of approach of topic.The present inventor is whole by lot of experiments and analysis work on the basis for summarizing prior art
In completing the present invention.
【The content of the invention】
[technical problems to be solved]
It is an object of the invention to provide a kind of cordate houttuynia essential oil cigarette with quick-fried pearl.
Preparation method it is a further object to provide the cordate houttuynia essential oil cigarette with quick-fried pearl.
[technical scheme]
The present invention is achieved through the following technical solutions.
A kind of preparation method the present invention relates to cordate houttuynia essential oil cigarette with quick-fried pearl.
The step of this method, is as follows：
A, cordate houttuynia pre-processes
Cordate houttuynia is dried in the shade, crushed, screening, the Heartleaf Houttuynia Herb of collection is put into extraction kettle, then vacuumized；
B, extract
According to cordate houttuynia in gram with counting the ratio of extractant as 1 using milliliter：20~50；1,1,1 are added into extraction kettle,
2- HFC-134as extractant and Heartleaf Houttuynia Herb, extracted under conditions of 40~60 DEG C of 1.2~1.5MPa of pressure and temperature
Take, standing separation obtains extract and cordate houttuynia extract remainder；
C, separate
The extract for being obtained step B with force (forcing) pump is imported in knockout drum, is then evaporated under reduced pressure, and the extractant of evaporation returns
Receive and recycle, remaining cordate houttuynia essential oil is collected for subsequent treatment；
D, dripping
Dripping pill is made in the cordate houttuynia essential oil drop that step C is obtained using pill dripping machine, the dripping pill of shaping is collected, it is cold to remove surface
But liquid, dry, obtain described cordate houttuynia essential oil cigarette with quick-fried pearl.
A preferred embodiment of the invention, in step, the vacuum reached when vacuumizing is -0.01~-
0.05MPa。
According to another preferred embodiment of the present invention, in step, the granularity of the Heartleaf Houttuynia Herb be 40 mesh with
Under.
According to another preferred embodiment of the present invention, in stepb, extractant extracts the extraction of Heartleaf Houttuynia Herb
Time is 0.5~2.0h.
According to another preferred embodiment of the present invention, in stepb, last quiet of extractant extraction herba houttuyniae powder
It is 5~10min to put the time.
According to the present invention another preferred embodiment, in step C, described reduction vaporization be pressure 0.05~
Carried out under conditions of 30~50 DEG C of 0.1MPa and temperature.
According to another preferred embodiment of the present invention, in step D, dripping speed during dripping is carried out using pill dripping machine
Degree is 3~5 drops/min；Condensate liquid is paraffin oil or dimethicone；The distance of water dropper and condensate liquid liquid level is 1~5cm.
According to another preferred embodiment of the present invention, in step D, the dripping pill of surface coolant is removed in temperature 40
4~8h is dried under conditions of~60 DEG C.
According to another preferred embodiment of the present invention, in step D, the cordate houttuynia essential oil cigarette diameter of quick-fried pearl
It is 2~4mm.
The invention further relates to the cordate houttuynia essential oil cigarette that the preparation method is prepared with quick-fried pearl.
The present invention is described in more detail below.
A kind of preparation method the present invention relates to cordate houttuynia essential oil cigarette with quick-fried pearl.
The step of this method, is as follows：
A, cordate houttuynia pre-processes
Cordate houttuynia is dried in the shade, crushed, screening, the Heartleaf Houttuynia Herb of collection is put into extraction kettle, then vacuumized；
In the present invention, cordate houttuynia is dried in the shade it should be understood that do not allow cordate houttuynia to be irradiated by direct sunlight, allows it logical
The drying that wind position is gradually carried out, in the active ingredient in cordate houttuynia is retained to greatest extent to the greatest extent the advantages of this drying mode, prevent
Only active ingredient is scattered and disappeared in cordate houttuynia.The water content of cordate houttuynia of drying in the shade is typically by weight less than 4%.
The cordate houttuynia that the present invention uses is from the dry of saururaceae plant houttuynia cordata (Houttuynia cordata Thunb.)
The cordate houttuynia that dry aerial part obtains.
According to the present invention, the granularity of the Heartleaf Houttuynia Herb is below 40 mesh, if Heartleaf Houttuynia Herb granularity is more than 40 mesh
Then can cell membrane it is broken incomplete, be unfavorable for extracting.
In the present invention, it is to be completely exhausted out the air in extraction kettle that extraction axe, which vacuumizes, prevents air to be mixed into extraction
Take in solvent HFC-134a, influence system extracting pressure.
The vacuum reached when vacuumizing is -0.01~-0.05MPa, if the vacuum exceedes the scope,
HFC-134a in extraction axe can be made as air is taken away, to reduce extraction efficiency.
The equipment that the present invention uses in crushing and screening is all current market sales of for processing agricultural byproducts
Disintegrating apparatus and screening plant.
The extraction kettle that the present invention uses is current market sales of product, such as by Applied companies of the U.S. with commodity
The product of name supercritical extract instrument sale.
B, extract
According to cordate houttuynia in gram with counting the ratio of extractant as 1 using milliliter：20~50；1,1,1 are added into extraction kettle,
2- HFC-134as extractant and Heartleaf Houttuynia Herb, extracted under conditions of 40~60 DEG C of 1.2~1.5MPa of pressure and temperature
Take, standing separation obtains extract and cordate houttuynia extract remainder；
HFA 134a (R134a) is nontoxic, non-ignitable, because it not chloride will not damage the ozone layer.At room temperature
Its vapour pressure is 0.5MPa, compares CO2It is much low, the critical extractant of low pressure is highly suitable as, operating pressure is less than
2MPa, therefore it is mainly used in the extraction of Volatile essence spices.Because operating pressure is than relatively low, head fragrant damage during decompression separation
Mistake substantially reduces.Compare CO by the use of R134a as extractant, extracting power2Height, and equipment manufacturing cost, operation energy consumption are greatly lowered.
In the present invention, if the ratio of cordate houttuynia and extractant is more than 1：20, then extractant can not flood cordate houttuynia,
Extraction yield is low；If the ratio of cordate houttuynia and extractant is less than 1：50, then extractant is excessive, causes to waste；Therefore, fish raw meat
The ratio of grass and extractant is 1：20~50 be rational；Preferably 1：26~42；More preferably 1：32~38.
In the present invention, extraction temperature be 40~60 DEG C with extraction time be 0.5~2.0h when, if extracting pressure is low
In 1.2MPa, then extraction yield is influenceed, increases extraction time；If extracting pressure is higher than 1.5MPa, the longevity of abstraction instrument is influenceed
Life, there is potential safety hazard；Therefore, extracting pressure is that 1.2~1.5MPa is rational, preferably 1.2~1.4MPa；
In the present invention, when extracting pressure is 1.2~1.5MPa and extraction time is 0.5~2.0h, if extraction temperature
Degree is less than 40 DEG C, then extractant viscosity increases, and influences to extract yield, increases extraction time；If extraction temperature is higher than 60 DEG C,
Then extractant viscosity diminishes, and reduces extraction efficiency；Therefore, extraction temperature be 40~60 DEG C be it is rational, preferably 46~
54℃；
In the present invention, when extracting pressure is 1.2~1.5MPa and extraction temperature is 40~60 DEG C, if extraction time
Less than 0.5h, then extraction is incomplete；If extraction time is longer than 2.0h, increase production cost, reduce economic benefit；Therefore,
Extraction time is that 0.5~2.0h is rational, preferably 0.8~1.6h；
In this step, the purpose of the extractant extraction last standing of herba houttuyniae powder is to make Heartleaf Houttuynia Herb and solvent
Solid-liquid is layered, and time of repose is 5~10min, if it exceeds this time range, can make Heartleaf Houttuynia Herb hardened, is not easy clear
Wash.
C, separate
The extract for being obtained step B with force (forcing) pump is imported in knockout drum, is then evaporated under reduced pressure, and the extractant of evaporation returns
Receive and recycle, remaining cordate houttuynia essential oil is collected for subsequent treatment；
The knockout drum that the present invention uses is, for example, Rotary Evaporators, glass evaporators, falling film evaporator or triple effect evaporator,
They are all current market sales of products.
In this step, described reduction vaporization is under conditions of 30~50 DEG C of 0.05~0.1MPa of pressure and temperature
Carry out.
In the present invention, under conditions of temperature is evaporated under reduced pressure and is 30~50 DEG C, it is less than if pressure is evaporated under reduced pressure
0.05MPa, then solvent and cordate houttuynia essential oil can not efficiently separate；If pressure, which is evaporated under reduced pressure, is higher than 0.1MPa, cordate houttuynia
Essential oil can enter returnable bottle, solvent slop with solvent；Therefore, it is that 0.05~0.1MPa is suitable that pressure, which is evaporated under reduced pressure,；
In the present invention, under conditions of pressure is evaporated under reduced pressure and is 0.05~0.1MPa, it is less than if temperature is evaporated under reduced pressure
30 DEG C, then solvent recovery is slow, reduces evaporation efficiency；If be evaporated under reduced pressure temperature be higher than 50 DEG C, cordate houttuynia essential oil can evaporate into
Enter to recycling design bottle, solvent slop；Therefore, it is appropriate temperature to be evaporated under reduced pressure to be 30~50 DEG C.
D, dripping
Dripping pill is made in the cordate houttuynia essential oil drop that step C is obtained using pill dripping machine, the dripping pill of shaping is collected, it is cold to remove surface
But liquid, dry, obtain described cordate houttuynia essential oil cigarette with quick-fried pearl.
The pill dripping machine that the present invention uses is current market sales of product, such as limited by the medicine Thailand Chinese medicine science and technology of Yantai hundred
The product that company is sold with trade name seamless pill dripping machine.
In the present invention, the condition that dripping is carried out using pill dripping machine is as follows：Dripping speed is 3~5 drops/min；Condensate liquid is
Paraffin oil or dimethicone；The distance of water dropper and condensate liquid liquid level is 1~5cm.
Paraffin oil is the oily liquids of semi-transparent clear, is dissolved in volatile oil, not soluble in water, be also insoluble in ethanol, have light,
Heat, absolute acid stability.The atoleine that the present invention uses is current market sales of product, such as is had by Zhong Run Tonghua, Shenzhen work
The product that limit company is sold with trade name atoleine.
Dimethicone is tasteless nontoxic, and chemically stable, physiological inertia, range of viscosities are wide, and freezing point is low, and flash-point is high, hydrophobic
Property is good.The dimethicone that the present invention uses is current market sales of product, such as wins the bright limited public affairs of science and technology by Shenzhen gold
The product that department is sold with trade name dimethicone.
In this step, using ethanol wash method remove surface coolant, then allow this dripping pill temperature 40~
4~8h is dried under conditions of 60 DEG C.
In the present invention,, can dripping pill if drying temperature is less than 40 DEG C when the drying time of this dripping pill is 4~8h
Middle rubber moisture is not volatile, and the phenomenon that eases back is serious；If drying temperature be higher than 60 DEG C, can dripping pill rubber become fragile, it is broken,
It is unfavorable for follow-up upper machining；Therefore, it is appropriate that drying temperature, which is 40~60 DEG C,；
When this dripping pill is dried at 40~60 DEG C of temperature, if drying time is less than 4h, can dripping pill rubber moisture contain
Amount is high, and quick-fried feel is pinched in influence；If drying time is longer than 8h, the mechanical movement time of dripping pill, badly broken can be increased；Cause
This, drying time is that 4~8h is appropriate
According to the present invention, the cordate houttuynia essential oil cigarette is 2~4mm with the diameter of quick-fried pearl.
The invention further relates to use the cordate houttuynia essential oil cigarette that the preparation method is prepared with quick-fried pearl.
Determination, described cordate houttuynia essential oil are detected under the conditions of thin-layer chromatography according to 2010 editions pharmacopeia volatile oil examination criterias
Cigarette has following performances with quick-fried pearl：
Main component is the group compounds of aldehydes and ketones such as decanoyl acetaldehyde, methyln nonyl ketone, lauryl aldehyde, capraldehyde in cordate houttuynia essential oil,
According to pharmacopeia to Herba Houttuyniae volatile oil detection method, extraction is obtained Herba Houttuyniae volatile oil and carries out thin-layer chromatography ratio with reference substance
Compared with composition is consistent, has clearing heat and detoxicating, the carbuncle that disappears apocenosis, inducing diuresis for treating strangurtia, relieving cough and reducing sputum and other effects.
[beneficial effect]
The beneficial effects of the invention are as follows：The present invention is had and carried using subcritical fluids extractive technique extraction cordate houttuynia essence
Take efficiency high, be easily isolated, non-thermal technology, energy-conservation, low cost and other advantages.Cordate houttuynia is a kind of wild plant of integration of drinking and medicinal herbs,
With clearing heat and detoxicating, detumescence and apocenosis, relieving cough and reducing sputum and other effects.The cigarette with quick-fried pearl essence to the improvement of cigarette smoking quality compared with
Control sample becomes apparent and comprehensively, fragrance is abundant, weakens with pungent fragrant, herbal, oral stimulation, while alleviates throat's discomfort
Sense, hence it is evident that increase sense of promoting the production of body fluid, integral suction quality is obviously improved.
【Embodiment】
The present invention is will be better understood that by following embodiments.
Embodiment 1：Cordate houttuynia essential oil cigarette is prepared with quick-fried pearl
The implementation steps of the embodiment are as follows：
A, cordate houttuynia pre-processes
It is by weight 3.8% that cordate houttuynia, which is dried in the shade to water content, is crushed, screening, the Heartleaf Houttuynia Herb of collection be put into by
In the extraction kettle that Applied companies of the U.S. are sold with trade name supercritical extract instrument, then vacuumize reach vacuum for-
0.01MPa；
B, extract
According to cordate houttuynia in gram with counting the ratio of extractant as 1 using milliliter：38；1,1,1,2- tetra- is added into extraction kettle
Fluoroethane extractant and Heartleaf Houttuynia Herb, extraction 2.0h is carried out under conditions of 40 DEG C of pressure 1.4MPa and temperature, stand and divide
From 8min, extract and cordate houttuynia extract remainder are obtained；
C, separate
The extract that step B is obtained is imported to point sold by Shanghai Rong Ya companies with commodity Rotary Evaporators with force (forcing) pump
From in tank, then it is evaporated under reduced pressure under conditions of 30 DEG C of pressure 0.05MPa and temperature, the extractant recovery of evaporation is sharp again
With remaining cordate houttuynia essential oil is collected for subsequent treatment；
D, dripping
Dripping pill is made in the cordate houttuynia essential oil drop that step C is obtained using pill dripping machine, the dripping pill of shaping is collected, is washed using alcohol
Wash method and remove surface coolant, 6h is dried under conditions of 54 DEG C of temperature, obtain described cordate houttuynia essential oil cigarette with quick-fried
Pearl.
The method described according to this specification, which detects, to be determined, described cordate houttuynia essential oil cigarette has following performances with quick-fried pearl：
Main component is the group compounds of aldehydes and ketones such as decanoyl acetaldehyde, methyln nonyl ketone, lauryl aldehyde, capraldehyde in cordate houttuynia essential oil,
According to pharmacopeia to Herba Houttuyniae volatile oil detection method, extraction is obtained Herba Houttuyniae volatile oil and carries out thin-layer chromatography ratio with reference substance
Compared with composition is consistent, has clearing heat and detoxicating, the carbuncle that disappears apocenosis, inducing diuresis for treating strangurtia, relieving cough and reducing sputum and other effects.
Cordate houttuynia essential oil cigarette prepared by the embodiment is put into cloud and mist (purple) cigarette filter rod with quick-fried pearl, according to YC/T138-
1998 tobaccos and tobacco product sensory evaluation method regulation organizes expert group of smokeing panel test carry out sensory evaluating smoking, and smoking result is listed in down
In table 1.
Felt using being not added with cordate houttuynia essential oil cigarette of the present invention by the use of cloud and mist (purple) cigarette filter rod of quick-fried pearl as control sample
Official is smoked panel test, and smoking result is also found in table 1 below.
Embodiment 2：Cordate houttuynia essential oil cigarette is prepared with quick-fried pearl
The implementation steps of the embodiment are as follows：
A, cordate houttuynia pre-processes
It is by weight 3.4% that cordate houttuynia, which is dried in the shade to water content, is crushed, screening, the Heartleaf Houttuynia Herb of collection be put into by
In the extraction kettle that Applied companies of the U.S. are sold with trade name supercritical extract instrument, then vacuumize reach vacuum for-
0.02MPa；
B, extract
According to cordate houttuynia in gram with counting the ratio of extractant as 1 using milliliter：20；1,1,1,2- tetra- is added into extraction kettle
Fluoroethane extractant and Heartleaf Houttuynia Herb, extraction 0.5h is carried out under conditions of pressure 1.2MPa and temperature 60 C, stand and divide
From 5min, extract and cordate houttuynia extract remainder are obtained；
C, separate
The extract for being obtained step B with force (forcing) pump is imported by Shanghai Rong Ya companies with the knockout drum of commodity Rotary Evaporators
In, then pressure 0.1MPa under conditions of temperature 50 C with being evaporated under reduced pressure, the extractant recycling of evaporation, remaining
Cordate houttuynia essential oil collect for subsequent treatment；
D, dripping
Dripping pill is made in the cordate houttuynia essential oil drop that step C is obtained using pill dripping machine, the dripping pill of shaping is collected, is washed using alcohol
Wash method and remove surface coolant, 8h is dried under conditions of 40 DEG C of temperature, obtain described cordate houttuynia essential oil cigarette with quick-fried
Pearl.
The method described according to this specification, which detects, to be determined, described cordate houttuynia essential oil cigarette has following performances with quick-fried pearl：
Main component is the group compounds of aldehydes and ketones such as decanoyl acetaldehyde, methyln nonyl ketone, lauryl aldehyde, capraldehyde in cordate houttuynia essential oil,
According to pharmacopeia to Herba Houttuyniae volatile oil detection method, extraction is obtained Herba Houttuyniae volatile oil and carries out thin-layer chromatography ratio with reference substance
Compared with composition is consistent, has clearing heat and detoxicating, the carbuncle that disappears apocenosis, inducing diuresis for treating strangurtia, relieving cough and reducing sputum and other effects.
Cordate houttuynia essential oil cigarette prepared by the embodiment is put into cloud and mist (purple) cigarette filter rod with quick-fried pearl, according to YC/T138-
1998 tobaccos and tobacco product sensory evaluation method regulation organizes expert group of smokeing panel test carry out sensory evaluating smoking, and smoking result is listed in down
In table 1.
Embodiment 3：Cordate houttuynia essential oil cigarette is prepared with quick-fried pearl
The implementation steps of the embodiment are as follows：
A, cordate houttuynia pre-processes
It is by weight 3.1% that cordate houttuynia, which is dried in the shade to water content, is crushed, screening, the Heartleaf Houttuynia Herb of collection be put into by
In the extraction kettle that Applied companies of the U.S. are sold with trade name supercritical extract instrument, then vacuumize reach vacuum for-
0.05MPa；
B, extract
According to cordate houttuynia in gram with counting the ratio of extractant as 1 using milliliter：32；1,1,1,2- tetra- is added into extraction kettle
Fluoroethane extractant and Heartleaf Houttuynia Herb, extraction 1.6h is carried out under conditions of 46 DEG C of pressure 1.5MPa and temperature, stand and divide
From 10min, extract and cordate houttuynia extract remainder are obtained；
C, separate
The extract that step B is obtained is imported to point sold by Shanghai Rong Ya companies with commodity Rotary Evaporators with force (forcing) pump
From in tank, then it is evaporated under reduced pressure under conditions of 38 DEG C of pressure 0.6MPa and temperature, the extractant recycling of evaporation,
Remaining cordate houttuynia essential oil is collected for subsequent treatment；
D, dripping
Dripping pill is made in the cordate houttuynia essential oil drop that step C is obtained using pill dripping machine, the dripping pill of shaping is collected, is washed using alcohol
Wash method and remove surface coolant, 7h is dried under conditions of 46 DEG C of temperature, obtain described cordate houttuynia essential oil cigarette with quick-fried
Pearl.
The method described according to this specification, which detects, to be determined, described cordate houttuynia essential oil cigarette has following performances with quick-fried pearl：
Main component is the group compounds of aldehydes and ketones such as decanoyl acetaldehyde, methyln nonyl ketone, lauryl aldehyde, capraldehyde in cordate houttuynia essential oil,
According to pharmacopeia to Herba Houttuyniae volatile oil detection method, extraction is obtained Herba Houttuyniae volatile oil and carries out thin-layer chromatography ratio with reference substance
Compared with composition is consistent, has clearing heat and detoxicating, the carbuncle that disappears apocenosis, inducing diuresis for treating strangurtia, relieving cough and reducing sputum and other effects.
Cordate houttuynia essential oil cigarette prepared by the embodiment is put into cloud and mist (purple) cigarette filter rod with quick-fried pearl, according to YC/T138-
1998 tobaccos and tobacco product sensory evaluation method regulation organizes expert group of smokeing panel test carry out sensory evaluating smoking, and smoking result is listed in down
In table 1.
Embodiment 4：Cordate houttuynia essential oil cigarette is prepared with quick-fried pearl
The implementation steps of the embodiment are as follows：
A, cordate houttuynia pre-processes
It is by weight 2.7% that cordate houttuynia, which is dried in the shade to water content, is crushed, screening, the Heartleaf Houttuynia Herb of collection be put into by
In the extraction kettle that Applied companies of the U.S. are sold with trade name supercritical extract instrument, then vacuumize reach vacuum for-
0.04MPa；
B, extract
According to cordate houttuynia in gram with counting the ratio of extractant as 1 using milliliter：50；1,1,1,2- tetra- is added into extraction kettle
Fluoroethane extractant and Heartleaf Houttuynia Herb, extraction 0.8h is carried out under conditions of 54 DEG C of pressure 1.3MPa and temperature, stand and divide
From 6min, extract and cordate houttuynia extract remainder are obtained；
C, separate
The extract that step B is obtained is imported to point sold by Shanghai Rong Ya companies with commodity Rotary Evaporators with force (forcing) pump
From in tank, then it is evaporated under reduced pressure under conditions of 46 DEG C of pressure 0.8MPa and temperature, the extractant recycling of evaporation,
Remaining cordate houttuynia essential oil is collected for subsequent treatment；
D, dripping
Dripping pill is made in the cordate houttuynia essential oil drop that step C is obtained using pill dripping machine, the dripping pill of shaping is collected, is washed using alcohol
Wash method and remove surface coolant, 4h is dried under conditions of temperature 60 C, obtain described cordate houttuynia essential oil cigarette with quick-fried
Pearl.
The method described according to this specification, which detects, to be determined, described cordate houttuynia essential oil cigarette has following performances with quick-fried pearl：
Main component is the group compounds of aldehydes and ketones such as decanoyl acetaldehyde, methyln nonyl ketone, lauryl aldehyde, capraldehyde in cordate houttuynia essential oil,
According to pharmacopeia to Herba Houttuyniae volatile oil detection method, extraction is obtained Herba Houttuyniae volatile oil and carries out thin-layer chromatography ratio with reference substance
Compared with composition is consistent, has clearing heat and detoxicating, the carbuncle that disappears apocenosis, inducing diuresis for treating strangurtia, relieving cough and reducing sputum and other effects.
Cordate houttuynia essential oil cigarette prepared by the embodiment is put into cloud and mist (purple) cigarette filter rod with quick-fried pearl, according to YC/T138-
1998 tobaccos and tobacco product sensory evaluation method regulation organizes expert group of smokeing panel test carry out sensory evaluating smoking, and smoking result is listed in down
In table 1.
Felt using being not added with cordate houttuynia essential oil cigarette of the present invention by the use of cloud and mist (purple) cigarette filter rod of quick-fried pearl as control sample
Official is smoked panel test, and smoking result is also found in table 1 below.
Table 1：Add smoking result of the cordate houttuynia essential oil cigarette of the present invention with quick-fried pearl cigarette filter rod
Claims (10)
1. a kind of cordate houttuynia essential oil cigarette preparation method of quick-fried pearl, it is characterised in that as follows the step of this method：
A, cordate houttuynia pre-processes
Cordate houttuynia is dried in the shade, crushed, screening, the Heartleaf Houttuynia Herb of collection is put into extraction kettle, then vacuumized；
B, extract
According to cordate houttuynia in gram with counting the ratio of extractant as 1 using milliliter：20~50；1,1,1,2- tetra- is added into extraction kettle
Fluoroethane extractant and Heartleaf Houttuynia Herb, extracted under conditions of 40~60 DEG C of 1.2~1.5MPa of pressure and temperature, it is quiet
Put isolated extract and cordate houttuynia extract remainder；
C, separate
The extract for being obtained step B with force (forcing) pump is imported in knockout drum, is then evaporated under reduced pressure, and the extractant recovery of evaporation is again
Utilize, remaining cordate houttuynia essential oil is collected for subsequent treatment；
D, dripping
Dripping pill is made in the cordate houttuynia essential oil drop that step C is obtained using pill dripping machine, the dripping pill of shaping is collected, removes surface cooling
Liquid, dry, obtain described cordate houttuynia essential oil cigarette with quick-fried pearl.
2. preparation method according to claim 1, it is characterised in that in step, the vacuum reached when vacuumizing is-
0.01~-0.05MPa.
3. preparation method according to claim 1, it is characterised in that in step, the granularity of the Heartleaf Houttuynia Herb is
Below 40 mesh.
4. preparation method according to claim 1, it is characterised in that in stepb, extractant extraction Heartleaf Houttuynia Herb
Extraction time be 0.5~2.0h.
5. preparation method according to claim 1, it is characterised in that in stepb, extractant extraction Heartleaf Houttuynia Herb
Time of repose afterwards is 5~10min.
6. preparation method according to claim 1, it is characterised in that in step C, described reduction vaporization is in pressure
Carried out under conditions of 30~50 DEG C of 0.05~0.1MPa and temperature.
7. preparation method according to claim 1, it is characterised in that in step D, using pill dripping machine carry out dripping when
Dripping speed is 3~5 drops/min；Condensate liquid is paraffin oil or dimethicone；The distance of water dropper and condensate liquid liquid level is 1~
5cm。
8. preparation method according to claim 1, it is characterised in that in step D, the dripping pill for removing surface coolant exists
4~8h is dried under conditions of 40~60 DEG C of temperature.
9. preparation method according to claim 1, it is characterised in that in step D, the cordate houttuynia essential oil cigarette is with quick-fried pearl
Diameter be 2~4mm.
10. according to the cordate houttuynia essential oil cigarette that preparation method described in any one of claim 1-9 claim is prepared with quick-fried
Pearl.
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| CN110804497A (en) * | 2019-11-18 | 2020-02-18 | 湖北中烟工业有限责任公司 | Preparation method of saffron extract for tobacco bead blasting |
| CN115844968A (en) * | 2023-02-24 | 2023-03-28 | 云南云科特色植物提取实验室有限公司 | Houttuynia cordata extract and preparation method and application thereof |
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Application publication date: 20171215 |