CN102987565B - 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 PDFInfo
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- CN102987565B CN102987565B CN201210544175.XA CN201210544175A CN102987565B CN 102987565 B CN102987565 B CN 102987565B CN 201210544175 A CN201210544175 A CN 201210544175A CN 102987565 B CN102987565 B CN 102987565B
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- 239000006187 pill Substances 0.000 title claims abstract description 36
- 238000013270 controlled release Methods 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title abstract description 7
- 241000208125 Nicotiana Species 0.000 title abstract description 4
- 235000002637 Nicotiana tabacum Nutrition 0.000 title abstract description 4
- 239000000796 flavoring agent Substances 0.000 title abstract 10
- 235000019634 flavors Nutrition 0.000 title abstract 10
- 239000011159 matrix material Substances 0.000 claims abstract description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 238000009833 condensation Methods 0.000 claims abstract description 14
- 230000005494 condensation Effects 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 238000007710 freezing Methods 0.000 claims abstract description 8
- 230000008014 freezing Effects 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 235000019504 cigarettes Nutrition 0.000 claims description 45
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 18
- 230000035945 sensitivity Effects 0.000 claims description 16
- 150000001412 amines Chemical class 0.000 claims description 13
- 239000002202 Polyethylene glycol Substances 0.000 claims description 12
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 claims description 10
- 229920001223 polyethylene glycol Polymers 0.000 claims description 10
- 229920002554 vinyl polymer Polymers 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 230000000391 smoking effect Effects 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 3
- 238000005303 weighing Methods 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 1
- RVGRUAULSDPKGF-UHFFFAOYSA-N Poloxamer Chemical compound C1CO1.CC1CO1 RVGRUAULSDPKGF-UHFFFAOYSA-N 0.000 description 8
- 238000003760 magnetic stirring Methods 0.000 description 8
- 229960000502 poloxamer Drugs 0.000 description 8
- 229920001983 poloxamer Polymers 0.000 description 8
- 239000003814 drug Substances 0.000 description 7
- 239000007790 solid phase Substances 0.000 description 7
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000003546 flue gas Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000007791 liquid phase Substances 0.000 description 6
- 229960003511 macrogol Drugs 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229940079593 drug Drugs 0.000 description 4
- 239000012071 phase Substances 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000036760 body temperature Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 238000010579 first pass effect Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 210000000867 larynx Anatomy 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- Medicinal Preparation (AREA)
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
Technical field
The present invention relates to the preparation method of dripping pill for cigarette, be specifically related to the preparation method of dripping pill for a kind of cigarette of temperature sensitivity controlled release essence.
Background technology
In the process developing rapidly at Modern Pharmaceutics, the important function of macromolecular material highlights day by day.Temperature sensitivity macromolecular material becomes one of functional material circle study hotspot, is subject to common concern.Temperature sensitivity macromolecular material refers to that thermal stimulus is had to response, there is LCST one class intelligent macromolecule material, as polyvinyl isobutyl phthalein amine, polyethylene glycol oxide ether (PEO), polyethylene adjoins pyrrolidone (PVP), poly-isopropyl propylene phthalein amine etc., in thermoresponsive, often contain ehter bond, the acid amides replacing, the functional groups such as hydroxyl, in temperature range, can there is marked change in its solubility, when its aqueous solution is heated on LCST, particle volume shrinks, solubility rapid drawdown, the aqueous solution resolves into two-phase, in macroscopic view, present muddiness, 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 thing field such as be separated.
Macromolecular material variation with temperature causes the variation of conformation, thereby can be used as temperature detect switch (TDS), as matrix, is applied to drug delivery system.Wherein, temperature sensitivity medicine carrying dripping pill can discharge medicine slowly, constantly, 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 to control conformational change, thereby promote to discharge, can reduce administration number of times, prolong drug biological half-life, increase curative effect of medication.
Existing research shows that temperature sensitivity controlled-release technology is at drug world comparative maturity, but not yet has temperature sensitivity controlled-release technology for tobacco business.If temperature sensitivity controlled-release technology is applied to make cigarette dripping pill in cigarette, need to solve following technical problem:
1,, in existing pharmacy, about the matrix phase transition temperature of temperature sensitivity delivery system, be human body temperature, 37 ℃.And during cigarette smoking, temperature when flue gas arrives mouth rod is 45 ~ 55 ℃, the matrix that need to study dripping pill in the solid phase of this temperature to liquid-phase conversion situation.
2, in existing pharmacy, longer about the matrix transformation time of temperature sensitivity delivery system, according to the difference at administering mode and position, from 8 hours to half a year not etc.And cigarette is joined in cigarette with dripping pill, require in suction A Cigarette Without You, 3 ~ 5 minutes, matrix was all converted into liquid state by solid phase.
3, in existing pharmacy, at 3 ~ 5 mm, comparatively wide in range about the diameter of temperature sensitivity administration dripping pill.Cigarette is used in the middle of cigarette filter tip with 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 the preparation method of dripping pill for a kind of temperature sensitivity controlled release essence cigarette.
To achieve these goals, the preparation method of dripping pill for temperature sensitivity controlled release essence cigarette of the present invention, comprises the following steps:
A, take 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, by the weight ratio of matrix and essence, being that 1 ~ 9:1 takes essence, is the ethanol that mass fraction 50 ~ 95% is added in 1:0.5 ~ 30 by the weight ratio of the ethanol of essence and mass fraction 50 ~ 95%, until essence dissolves completely;
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 is stirred and evenly mixed instils in molten state with essence, coolingly become ball with after condensation, then collect that ball is freezing, enrichment dry after, obtain product.
Preferably, 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.
Preferably, in step c), mixing speed is 100 ~ 500rpm, stirs 30 ~ 120min.
Preferably, in step d), 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 ℃.
Preferably, temperature sensitivity controlled release essence cigarette method for preparing drop pills of the present invention, comprises the following steps:
A, take matrix, 75 ~ 90 ℃ of heating, until reach molten condition, described matrix is polyvinyl isobutyl phthalein amine or poloxamer;
B, by the weight ratio of matrix and essence, being that 1 ~ 4:1 takes essence, is the ethanol that mass fraction 50 ~ 95% is added in 1:1 ~ 4 by the weight ratio of the ethanol of essence and mass fraction 50 ~ 95%, until essence dissolves completely;
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 is stirred and evenly mixed instils in molten state with essence, coolingly become ball with after condensation, then collect that ball is freezing, enrichment dry after, obtain product; 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.While utilizing cigarette smoking, when flue gas arrives mouth rod 45 ~ 55 ℃ of temperature, cigarette by the matrix of dripping pill gradually by solid phase to liquid-phase conversion.After cigarette suction is complete, dripping pill is all converted into liquid state.Like this, the essence wrapping up in this matrix can discharge gradually along with the suction of cigarette and the phase transformation of matrix, makes consumer in the process of a cigarette of suction, can experience all the time the easypro larynx effect of flavouring of essence.
Beneficial effect of the present invention: the present invention is wrapped in essence in the matrix with Thermo-sensitive, 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 the comfortableness that improves suction cigarette, also can reduce the harm of cigarette to health as required.
The specific embodiment
Below in conjunction with specific embodiment, the inventive method is described in further detail.
Embodiment 1
A, take the Macrogol 6000 of 10.07g, join in round-bottomed flask, put in constent temperature heater, 75 ℃ of heating, until reach molten condition;
B, by the weight ratio of Macrogol 6000 and essence, being that 1:1 takes essence 10.07g, 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 completely;
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, at Macrogol 6000 during in molten condition, consoluet essence is slowly joined in the Macrogol 6000 of molten condition, stir 75min;
D, Macrogol 6000 and essence that the molten state after step c stirring is mixed carry out dripping, the Macrogol 6000 first molten state being mixed and essence add in the high temperature instillation system of equipment, control valve, make it with drops, to ooze and enter discontinuously low-temperature cooling system and Cryogenic condensation system, be cooled to rapidly ball; And freezing in collection ball system, after enrichment, take out, dry, get product.
Wherein, high temperature instillation system temperature is controlled at 75 ℃, and low-temperature cooling system temperature is controlled at 20 ℃, and 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.While utilizing cigarette smoking, when flue gas arrives mouth rod 45 ~ 55 ℃ of temperature, cigarette by the matrix of dripping pill gradually by solid phase to liquid-phase conversion.After cigarette suction is complete, dripping pill is all converted into liquid state.
Embodiment 2
A, take the polyvinyl isobutyl phthalein amine 20000 of 10.08g, join in round-bottomed flask, put in constent temperature heater, 80 ℃ of heating, until reach molten condition;
B, by polyvinyl isobutyl phthalein amine 20000, being that 4:1 takes essence 2.52g with the weight ratio of 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 completely;
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, at polyvinyl isobutyl phthalein amine 20000 during 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 the molten state after step c stirring is mixed carry out dripping, in the high temperature instillation system that the polyvinyl isobutyl phthalein amine 20000 first molten state being mixed and essence add equipment to, control valve, make it with drops, to ooze and enter discontinuously low-temperature cooling system and Cryogenic condensation system, be cooled to rapidly ball; And freezing in collection ball system, after enrichment, take out, dry, get product.
Wherein, high temperature instillation system temperature is controlled at 80 ℃, and low-temperature cooling system temperature is controlled at 25 ℃, and 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.While utilizing cigarette smoking, when flue gas arrives mouth rod 45 ~ 55 ℃ of temperature, cigarette by the matrix of dripping pill gradually by solid phase to liquid-phase conversion.After cigarette suction is complete, dripping pill is all converted into liquid state.
Embodiment 3
A, take the poloxamer 8000 of 10.06g, join in round-bottomed flask, put in constent temperature heater, 85 ℃ of heating, until reach molten condition;
B, by poloxamer 8000, being that 7:3 takes essence 4.311g with the weight ratio of 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 completely;
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, at poloxamer 8000 during in molten condition, consoluet essence is slowly joined in the poloxamer 8000 of molten condition, stir 90min;
D, poloxamer 8000 and essence that the molten state after step c stirring is mixed carry out dripping, in the high temperature instillation system that the poloxamer 8000 first molten state being mixed and essence add equipment to, control valve, make it with drops, to ooze and enter discontinuously low-temperature cooling system and Cryogenic condensation system, be cooled to rapidly ball; And freezing in collection ball system, after enrichment, take out, dry, get product.
Wherein, high temperature instillation system temperature is controlled at 85 ℃, and low-temperature cooling system temperature is controlled at 30 ℃, and 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.While utilizing cigarette smoking, when flue gas arrives mouth rod 45 ~ 55 ℃ of temperature, cigarette by the matrix of dripping pill gradually by solid phase to liquid-phase conversion.After cigarette suction is complete, dripping pill is all converted into liquid state.
Embodiment 4
A, take the polyethylene glycol oxide ether (PEO) 15000 of 10.06g, join in round-bottomed flask, put in constent temperature heater, 90 ℃ of heating, until reach molten condition;
B, by polyethylene glycol oxide ether 15000, being that 3:2 takes essence 6.707g with the weight ratio of 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 completely;
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, at polyethylene glycol oxide ether 15000 during 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 the molten state after step c stirring is mixed carry out dripping, in the high temperature instillation system that the polyethylene glycol oxide ether 15000 first molten state being mixed and essence add equipment to, control valve, make it with drops, to ooze and enter discontinuously low-temperature cooling system and Cryogenic condensation system, be cooled to rapidly ball; And freezing in collection ball system, after enrichment, take out, dry, get product.
Wherein, high temperature instillation system temperature is controlled at 90 ℃, and low-temperature cooling system temperature is controlled at 35 ℃, and 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.While utilizing cigarette smoking, when flue gas arrives mouth rod 45 ~ 55 ℃ of temperature, cigarette by the matrix of dripping pill gradually by solid phase to liquid-phase conversion.After cigarette suction is complete, dripping pill is all converted into liquid state.
Claims (1)
1. the preparation method of dripping pill for temperature sensitivity controlled release essence cigarette, comprises the following steps:
A, take matrix, 75～90 ℃ of heating, until reach molten condition, described matrix is polyvinyl isobutyl phthalein amine, polyethylene glycol oxide ether, polyvinylpyrrolidone or poly-isopropyl propylene phthalein amine;
B, by the weight ratio of matrix and essence, being that 1～5:1 takes essence, is the ethanol that mass fraction 50～95% is added in 1:1～6 by the weight ratio of the ethanol of essence and mass fraction 50～95%, until essence dissolves completely;
C, temperature are controlled at 75～90 ℃, consoluet essence are slowly joined in the matrix of molten condition, stir and evenly mix, and mixing speed is 100～500rpm, stir 30～120min;
D, the matrix after step c is stirred and evenly mixed instils 75～90 ℃ of molten states with essence, 20～70 ℃ cooling with after 5～20 ℃ of condensations, become ball, then, enrichment freezing at-10～10 ℃ of collection balls dry after, obtain product.
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| CN201210544175.XA CN102987565B (en) | 2012-12-13 | 2012-12-13 | Method for preparing dropping pills of temperature sensitive controlled-release flavor for tobacco |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210544175.XA CN102987565B (en) | 2012-12-13 | 2012-12-13 | Method for preparing dropping pills of temperature sensitive controlled-release flavor for tobacco |
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| CN102987565A CN102987565A (en) | 2013-03-27 |
| CN102987565B true CN102987565B (en) | 2014-03-26 |
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| 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 |
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| 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 |
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| CN102987565A (en) | 2013-03-27 |
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