CN102987565A - Method for preparing dropping pills of temperature sensitive controlled-release flavor for tobacco - Google Patents

Method for preparing dropping pills of temperature sensitive controlled-release flavor for tobacco Download PDF

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Publication number
CN102987565A
CN102987565A CN201210544175XA CN201210544175A CN102987565A CN 102987565 A CN102987565 A CN 102987565A CN 201210544175X A CN201210544175X A CN 201210544175XA CN 201210544175 A CN201210544175 A CN 201210544175A CN 102987565 A CN102987565 A CN 102987565A
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Prior art keywords
essence
temperature
matrix
controlled
flavor
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CN201210544175XA
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CN102987565B (en
Inventor
王娜
叶晓川
施璐
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China Tobacco Hunan Industrial Co Ltd
Wuhan Huanghelou Science and Technology Park Co Ltd
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China Tobacco Hunan Industrial Co Ltd
Wuhan Huanghelou Science and Technology Park Co Ltd
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Abstract

The invention discloses a method for preparing dropping pills of temperature sensitive controlled-release flavor for tobacco, comprising the following steps: weighing matrix and heating so that the matrix is melted; weighing the flavor and completely dissolving the same by using ethanol; dropwise adding the completely dissolved flavor to the matrix in the melted state and stirring and mixing evenly; performing dripping, cooling and condensation on the matrix and the flavor stirred and mixed together evenly in the melted state to form pills, and then freezing the pills and performing enrichment drying, thereby obtaining the product. The method provided by the invention obtains the dropping pills of the temperature sensitive controlled-release flavor for tobacco by covering the flavor with the thermo-sensitive matrix; the dripping pills covering the flavor are capable of releasing the flavor slowly and continuously so that the consumer can enjoy the aroma enhancement and throat comforting effects of the flavor while smoking.

Description

The cigarette of the temperature sensitivity controlled release essence preparation method of dripping pill
Technical field
The present invention relates to the cigarette preparation method of dripping pill, the cigarette preparation method of dripping pill who is specifically related to a kind of temperature sensitivity controlled release essence.
Background technology
In the process that Modern Pharmaceutics develops rapidly, the important function of macromolecular material highlights day by day.The temperature sensitivity macromolecular material becomes one of functional material circle study hotspot, is subject to common concern.The temperature sensitivity macromolecular material refers to that thermal stimulus is had response, has LCST one class intelligent macromolecule material, such as polyvinyl isobutyl phthalein amine, polyethylene glycol oxide ether (PEO), polyethylene adjoins pyrrolidone (PVP), poly-isopropyl propylene phthalein amine etc., often contain ehter bond in the thermoresponsive, the acid amides that replaces, the functional groups such as hydroxyl, marked change can occur in its solubility in temperature range, when its aqueous solution was heated on the LCST, particle volume shrank, the solubility rapid drawdown, the aqueous solution resolves into two-phase, presents muddiness on the macroscopic view, and this transformation be have reversible.This temperature sensitive polymer has been used to make gel, microballoon etc., and is widely used in biology, and chemicals discharges, the fields such as phase separation.
The macromolecular material variation with temperature causes the variation of conformation, thereby can be used as temperature detect switch (TDS), is applied to drug delivery system as matrix.Wherein, temperature sensitivity medicine carrying dripping pill can discharge medicine slowly, constantly, and is long-time with site of action generation close contact and absorb the drug, and avoids first pass effect, the bioavilability of raising medicine; Utilize temperature control conformational change, thereby promote to discharge, can reduce administration number of times, prolong drug biological half-life, increase curative effect of medication.
The existing temperature sensitivity controlled-release technology that studies show that is used for tobacco business but not yet have with the temperature sensitivity controlled-release technology at the drug world comparative maturity.If the temperature sensitivity controlled-release technology is applied to make the cigarette dripping pill in the cigarette, need to solve following technical problem:
1, in the existing pharmacy, be human body temperature about the matrix phase transition temperature of temperature sensitivity delivery system, 37 ℃.And during cigarette smoking, the temperature when flue gas arrives the mouth rod is 45 ~ 55 ℃, the matrix that needs the research dripping pill in the solid phase of this temperature to the liquid-phase conversion situation.
2, in the existing pharmacy, longer about the matrix transformation time of temperature sensitivity delivery system, different according to administering mode and position are not waited from 8 hours to half a year.And cigarette is joined in the cigarette with dripping pill, require in the suction A Cigarette Without You, namely 3 ~ 5 minutes, matrix all was converted into liquid state by solid phase.
3, in the existing pharmacy, at 3 ~ 5 mm, comparatively wide in range about the diameter of temperature sensitivity administration dripping pill.Cigarette uses in the middle of cigarette filter tip with the dripping pill General Requirements, and therefore, diameter need to accurately be controlled in 3.6 ~ 4 mm.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide a kind of temperature sensitivity controlled release essence cigarette preparation method of dripping pill.
To achieve these goals, the temperature sensitivity controlled release essence cigarette of the present invention preparation method of dripping pill may further comprise the steps:
A, take by weighing matrix, 75 ~ 90 ℃ of heating, until reach molten condition, described matrix is polyethylene glycol, polyvinyl isobutyl phthalein amine, poloxamer, polyethylene glycol oxide ether, polyvinylpyrrolidone or poly-isopropyl propylene phthalein amine;
B, being that 1 ~ 9:1 takes by weighing essence by the weight ratio of matrix and essence, is the ethanol that mass fractions 50 ~ 95% are added in 1:0.5 ~ 30 by the weight ratio of the ethanol of essence and mass fraction 50 ~ 95%, until essence dissolves fully;
C, temperature are controlled at 75 ~ 90 ℃, consoluet essence are slowly joined in the matrix of molten condition, stir and evenly mix;
D, the matrix after step c stirred and evenly mixed instil in molten state with essence, become ball after cooling and the condensation, collect again that ball is freezing, enrichment dry after, namely get product.
Preferably, in the step b), the weight ratio of described matrix and essence is 1 ~ 5:1, and the weight ratio of the ethanol of described essence and mass fraction 50 ~ 95% is 1:1 ~ 6.
Preferably, in the step c), mixing speed is 100 ~ 500rpm, stirs 30 ~ 120min.
Preferably, in the step d), the instillation temperature is controlled at 75 ~ 90 ℃, and chilling temperature is controlled at 20 ~ 70 ℃, and condensation temperature is controlled at 5 ~ 20 ℃, and collection ball cryogenic temperature is controlled at-10 ~ 10 ℃.
More excellent, temperature sensitivity controlled release essence cigarette method for preparing drop pills of the present invention may further comprise the steps:
A, take by weighing matrix, 75 ~ 90 ℃ of heating, until reach molten condition, described matrix is polyvinyl isobutyl phthalein amine or poloxamer;
B, being that 1 ~ 4:1 takes by weighing essence by the weight ratio of matrix and essence, is the ethanol that mass fractions 50 ~ 95% are added in 1:1 ~ 4 by the weight ratio of the ethanol of essence and mass fraction 50 ~ 95%, until essence dissolves fully;
C, temperature are controlled at 75 ~ 90 ℃, consoluet essence are slowly joined in the matrix of molten condition, and mixing speed is 100 ~ 500rpm, stir 30 ~ 120min, stir and evenly mix;
D, the matrix after step c stirred and evenly mixed instil in molten state with essence, become ball after cooling and the condensation, collect again that ball is freezing, enrichment dry after, namely get product; The instillation temperature is controlled at 75 ~ 90 ℃, and chilling temperature is controlled at 20 ~ 40 ℃, and condensation temperature is controlled at 5 ~ 15 ℃, and collection ball cryogenic temperature is controlled at-10 ~ 5 ℃.
Prepared cigarette is used in the middle of cigarette filter tip with dripping pill, and diameter can accurately be controlled in 3.6 ~ 4 mm.When utilizing cigarette smoking, when flue gas arrives the mouth rod 45 ~ 55 ℃ of temperature, cigarette with the matrix of dripping pill gradually by solid phase to liquid-phase conversion.After the cigarette suction was complete, dripping pill all was converted into liquid state.Like this, the essence that wraps up in this matrix can discharge gradually along with the suction of cigarette and the phase transformation of matrix, makes the consumer can experience all the time the easypro larynx effect of flavouring of essence in the process of a cigarette of suction.
Beneficial effect of the present invention: the present invention is wrapped in essence to have in the Thermosensitive matrix, make the cigarette dripping pill of the controlled release essence with temperature sensitivity, the dripping pill that bag carries essence can discharge essence slowly, constantly, thereby improve the comfortableness of suction cigarette, also can reduce as required cigarette to the harm of health.
The specific embodiment
Below in conjunction with specific embodiment the inventive method is described in further detail.
Embodiment 1
A, take by weighing the Macrogol 6000 of 10.07g, join in the round-bottomed flask, put in the constent temperature heater, 75 ℃ of heating, until reach molten condition;
B, being that 1:1 takes by weighing essence 10.07g by the weight ratio of Macrogol 6000 and essence, is the ethanol 10.07g that 1:1 adds mass fraction 50% by the weight ratio of the ethanol of essence and mass fraction 50%, until essence dissolves fully;
C, the round-bottomed flask of step a is placed on constant-temperature heating magnetic stirring apparatus, the temperature of constant-temperature heating magnetic stirring apparatus is controlled in 75 ℃, mixing speed is 100rpm, when Macrogol 6000 is in molten condition, consoluet essence is slowly joined in the Macrogol 6000 of molten condition, stir 75min;
D, Macrogol 6000 and essence that step c is stirred the molten state mixing after complete carry out dripping, in the high temperature instillation system that adds Macrogol 6000 and the essence of molten state mixing to equipment first, control valve, make it to ooze and enter with drops discontinuously low-temperature cooling system and Cryogenic condensation system, be cooled to rapidly ball; And freezing in collection ball system, to take out after the enrichment, drying gets product.
Wherein, high temperature instillation system temperature is controlled at 75 ℃, and the low-temperature cooling system temperature is controlled at 20 ℃, and the Cryogenic condensation system temperature is controlled at 5 ℃, and collection ball system temperature is controlled at-10 ℃.
Prepared cigarette is used in the middle of cigarette filter tip with dripping pill, and diameter can accurately be controlled in 3.6 ~ 4 mm.When utilizing cigarette smoking, when flue gas arrives the mouth rod 45 ~ 55 ℃ of temperature, cigarette with the matrix of dripping pill gradually by solid phase to liquid-phase conversion.After the cigarette suction was complete, dripping pill all was converted into liquid state.
Embodiment 2
A, take by weighing the polyvinyl isobutyl phthalein amine 20000 of 10.08g, join in the round-bottomed flask, put in the constent temperature heater, 80 ℃ of heating, until reach molten condition;
B, being that 4:1 takes by weighing essence 2.52g by the weight ratio of polyvinyl isobutyl phthalein amine 20000 and essence, is the ethanol 5.04g of 1:2 interpolation mass fraction 60% by the weight ratio of the ethanol of essence and mass fraction 60%, until essence dissolves fully;
C, the round-bottomed flask of step a is placed on constant-temperature heating magnetic stirring apparatus, the temperature of constant-temperature heating magnetic stirring apparatus is controlled in 80 ℃, mixing speed is 200rpm, when polyvinyl isobutyl phthalein amine 20000 is in molten condition, consoluet essence is slowly joined in the polyvinyl isobutyl phthalein amine 20000 of molten condition, stir 85min;
D, polyvinyl isobutyl phthalein amine 20000 and essence that step c is stirred the molten state mixing after complete carry out dripping, in the high temperature instillation system that adds polyvinyl isobutyl phthalein amine 20000 and the essence of molten state mixing to equipment first, control valve, make it to ooze and enter with drops discontinuously low-temperature cooling system and Cryogenic condensation system, be cooled to rapidly ball; And freezing in collection ball system, to take out after the enrichment, drying gets product.
Wherein, high temperature instillation system temperature is controlled at 80 ℃, and the low-temperature cooling system temperature is controlled at 25 ℃, and the Cryogenic condensation system temperature is controlled at 8 ℃, and collection ball system temperature is controlled at-5 ℃.
Prepared cigarette is used in the middle of cigarette filter tip with dripping pill, and diameter can accurately be controlled in 3.6 ~ 4 mm.When utilizing cigarette smoking, when flue gas arrives the mouth rod 45 ~ 55 ℃ of temperature, cigarette with the matrix of dripping pill gradually by solid phase to liquid-phase conversion.After the cigarette suction was complete, dripping pill all was converted into liquid state.
Embodiment 3
A, take by weighing the poloxamer 8000 of 10.06g, join in the round-bottomed flask, put in the constent temperature heater, 85 ℃ of heating, until reach molten condition;
B, being that 7:3 takes by weighing essence 4.311g by the weight ratio of poloxamer 8000 and essence, is the ethanol 12.933g of 1:3 interpolation mass fraction 70% by the weight ratio of the ethanol of essence and mass fraction 70%, until essence dissolves fully;
C, the round-bottomed flask of step a is placed on constant-temperature heating magnetic stirring apparatus, the temperature of constant-temperature heating magnetic stirring apparatus is controlled in 85 ℃, mixing speed is 300rpm, when poloxamer 8000 is in molten condition, consoluet essence is slowly joined in the poloxamer 8000 of molten condition, stir 90min;
D, poloxamer 8000 and essence that step c is stirred the molten state mixing after complete carry out dripping, in the high temperature instillation system that adds poloxamer 8000 and the essence of molten state mixing to equipment first, control valve, make it to ooze and enter with drops discontinuously low-temperature cooling system and Cryogenic condensation system, be cooled to rapidly ball; And freezing in collection ball system, to take out after the enrichment, drying gets product.
Wherein, high temperature instillation system temperature is controlled at 85 ℃, and the low-temperature cooling system temperature is controlled at 30 ℃, and the Cryogenic condensation system temperature is controlled at 10 ℃, and collection ball system temperature is controlled at 0 ℃.
Prepared cigarette is used in the middle of cigarette filter tip with dripping pill, and diameter can accurately be controlled in 3.6 ~ 4 mm.When utilizing cigarette smoking, when flue gas arrives the mouth rod 45 ~ 55 ℃ of temperature, cigarette with the matrix of dripping pill gradually by solid phase to liquid-phase conversion.After the cigarette suction was complete, dripping pill all was converted into liquid state.
Embodiment 4
A, take by weighing the polyethylene glycol oxide ether (PEO) 15000 of 10.06g, join in the round-bottomed flask, put in the constent temperature heater, 90 ℃ of heating, until reach molten condition;
B, being that 3:2 takes by weighing essence 6.707g by the weight ratio of polyethylene glycol oxide ether 15000 and essence, is the ethanol 26.827g of 1:4 interpolation mass fraction 75% by the weight ratio of the ethanol of essence and mass fraction 75%, until essence dissolves fully;
C, the round-bottomed flask of step a is placed on constant-temperature heating magnetic stirring apparatus, the temperature of constant-temperature heating magnetic stirring apparatus is controlled in 90 ℃, mixing speed is 400rpm, when polyethylene glycol oxide ether 15000 is in molten condition, consoluet essence is slowly joined in the polyethylene glycol oxide ether 15000 of molten condition, stir 100min;
D, polyethylene glycol oxide ether 15000 and essence that step c is stirred the molten state mixing after complete carry out dripping, in the high temperature instillation system that adds polyethylene glycol oxide ether 15000 and the essence of molten state mixing to equipment first, control valve, make it to ooze and enter with drops discontinuously low-temperature cooling system and Cryogenic condensation system, be cooled to rapidly ball; And freezing in collection ball system, to take out after the enrichment, drying gets product.
Wherein, high temperature instillation system temperature is controlled at 90 ℃, and the low-temperature cooling system temperature is controlled at 35 ℃, and the Cryogenic condensation system temperature is controlled at 15 ℃, and collection ball system temperature is controlled at 5 ℃.
Prepared cigarette is used in the middle of cigarette filter tip with dripping pill, and diameter can accurately be controlled in 3.6 ~ 4 mm.When utilizing cigarette smoking, when flue gas arrives the mouth rod 45 ~ 55 ℃ of temperature, cigarette with the matrix of dripping pill gradually by solid phase to liquid-phase conversion.After the cigarette suction was complete, dripping pill all was converted into liquid state.

Claims (4)

1. a temperature sensitivity controlled release essence cigarette may further comprise the steps with the preparation method of dripping pill:
A, take by weighing matrix, 75 ~ 90 ℃ of heating, until reach molten condition, described matrix is polyethylene glycol, polyvinyl isobutyl phthalein amine, poloxamer, polyethylene glycol oxide ether, polyvinylpyrrolidone or poly-isopropyl propylene phthalein amine;
B, being that 1 ~ 9:1 takes by weighing essence by the weight ratio of matrix and essence, is the ethanol that mass fractions 50 ~ 95% are added in 1:0.5 ~ 30 by the weight ratio of the ethanol of essence and mass fraction 50 ~ 95%, until essence dissolves fully;
C, temperature are controlled at 75 ~ 90 ℃, consoluet essence are slowly joined in the matrix of molten condition, stir and evenly mix;
D, the matrix after step c stirred and evenly mixed instil in molten state with essence, become ball after cooling and the condensation, collect again that ball is freezing, enrichment dry after, namely get product.
2. temperature sensitivity controlled release essence cigarette according to claim 1 is with the preparation method of dripping pill, it is characterized in that: in step b), the weight ratio of described matrix and essence is 1 ~ 5:1, and the weight ratio of the ethanol of described essence and mass fraction 50 ~ 95% is 1:1 ~ 6.
3. temperature sensitivity controlled release essence cigarette according to claim 1 is with the preparation method of dripping pill, and it is characterized in that: in step c), mixing speed is 100 ~ 500rpm, stirs 30 ~ 120min.
4. temperature sensitivity controlled release essence cigarette according to claim 1 is with the preparation method of dripping pill, it is characterized in that: in step d), the instillation temperature is controlled at 75 ~ 90 ℃, and chilling temperature is controlled at 20 ~ 70 ℃, condensation temperature is controlled at 5 ~ 20 ℃, and collection ball cryogenic temperature is controlled at-10 ~ 10 ℃.
CN201210544175.XA 2012-12-13 2012-12-13 Method for preparing dropping pills of temperature sensitive controlled-release flavor for tobacco Active CN102987565B (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103251131A (en) * 2013-06-07 2013-08-21 安徽中烟工业有限责任公司 Preparation method of perfuming filter stick with perfumed substance released slowly
CN103263082A (en) * 2013-06-07 2013-08-28 安徽中烟工业有限责任公司 Fragrance slow-release cigarette filter stick containing polyethylene glycol granules and preparation method thereof
CN103271442A (en) * 2013-06-07 2013-09-04 安徽中烟工业有限责任公司 Linear polyethylene glycol fragrance slow-release cigarette filter rod and production method thereof
CN103380900A (en) * 2013-06-19 2013-11-06 安徽恒星制药有限公司 Preparation method for novel corrective flavor type oral rehydration salt powders and novel corrective flavor type oral rehydration salt powders
CN105686077A (en) * 2016-03-25 2016-06-22 湖北中烟工业有限责任公司 Preparation method of cigarette filter tip rod with blending material controlled-release cool sense essence
CN105686076A (en) * 2016-03-25 2016-06-22 湖北中烟工业有限责任公司 Method for preparing cigarette filter tip containing temperature sensibility controlled-released cool essence
CN105996121A (en) * 2016-06-28 2016-10-12 云南瑞升烟草技术(集团)有限公司 Filter stick additive capable of releasing functional substance through phase change and preparation method and application thereof
CN112159719A (en) * 2020-08-28 2021-01-01 深圳波顿香料有限公司 Flavoring particle for electronic cigarette and preparation method and application thereof
CN114011329A (en) * 2021-11-29 2022-02-08 江苏大亚滤嘴材料有限公司 Preparation method of water particles capable of increasing smoke moistening feeling

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CN102108136A (en) * 2009-12-25 2011-06-29 湖北中烟工业有限责任公司 Tobacco additive dropping pill wrapping material, dropping pill wrapped thereby and application of dropping pill
CN102273733A (en) * 2010-06-08 2011-12-14 湖北中烟工业有限责任公司 Sustained-release pellet capsule of sweet cooling agent for cigarette with filter plug

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EP1635657A2 (en) * 2003-06-13 2006-03-22 Philip Morris Products S.A. Cigarette wrapper with catalytic filler and methods of making same
CN101375834A (en) * 2007-09-02 2009-03-04 杨喜鸿 Solid dispersion of Ailamode and preparation method thereof and medicament application
CN101152197A (en) * 2007-09-24 2008-04-02 北京华睿鼎信科技有限公司 Compound glycyrrhizin dropping pills and method for preparing the same
CN102038659A (en) * 2009-10-16 2011-05-04 北京润德康医药技术有限公司 Pills taking nicotine as main active ingredient and preparation method thereof
CN102108136A (en) * 2009-12-25 2011-06-29 湖北中烟工业有限责任公司 Tobacco additive dropping pill wrapping material, dropping pill wrapped thereby and application of dropping pill
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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103251131A (en) * 2013-06-07 2013-08-21 安徽中烟工业有限责任公司 Preparation method of perfuming filter stick with perfumed substance released slowly
CN103263082A (en) * 2013-06-07 2013-08-28 安徽中烟工业有限责任公司 Fragrance slow-release cigarette filter stick containing polyethylene glycol granules and preparation method thereof
CN103271442A (en) * 2013-06-07 2013-09-04 安徽中烟工业有限责任公司 Linear polyethylene glycol fragrance slow-release cigarette filter rod and production method thereof
CN103380900A (en) * 2013-06-19 2013-11-06 安徽恒星制药有限公司 Preparation method for novel corrective flavor type oral rehydration salt powders and novel corrective flavor type oral rehydration salt powders
CN105686077A (en) * 2016-03-25 2016-06-22 湖北中烟工业有限责任公司 Preparation method of cigarette filter tip rod with blending material controlled-release cool sense essence
CN105686076A (en) * 2016-03-25 2016-06-22 湖北中烟工业有限责任公司 Method for preparing cigarette filter tip containing temperature sensibility controlled-released cool essence
CN105686077B (en) * 2016-03-25 2019-10-11 湖北中烟工业有限责任公司 The cigarette mouth stick preparation method of intermingling material controlled release cool feeling essence
CN105996121A (en) * 2016-06-28 2016-10-12 云南瑞升烟草技术(集团)有限公司 Filter stick additive capable of releasing functional substance through phase change and preparation method and application thereof
CN105996121B (en) * 2016-06-28 2019-12-27 云南瑞升烟草技术(集团)有限公司 Filter stick additive capable of releasing functional substances through phase change and preparation method and application thereof
CN112159719A (en) * 2020-08-28 2021-01-01 深圳波顿香料有限公司 Flavoring particle for electronic cigarette and preparation method and application thereof
CN114011329A (en) * 2021-11-29 2022-02-08 江苏大亚滤嘴材料有限公司 Preparation method of water particles capable of increasing smoke moistening feeling
CN114011329B (en) * 2021-11-29 2024-03-26 江苏大亚滤嘴材料有限公司 Preparation method of water particles capable of increasing smoke moist feeling

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