CN109875109B - Preparation method of allspice oleoresin for cigarettes and application of allspice oleoresin in cigarettes - Google Patents
Preparation method of allspice oleoresin for cigarettes and application of allspice oleoresin in cigarettes Download PDFInfo
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- CN109875109B CN109875109B CN201910089972.5A CN201910089972A CN109875109B CN 109875109 B CN109875109 B CN 109875109B CN 201910089972 A CN201910089972 A CN 201910089972A CN 109875109 B CN109875109 B CN 109875109B
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- allspice
- oleoresin
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- passion fruit
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- 240000008474 Pimenta dioica Species 0.000 title claims abstract description 64
- 235000006990 Pimenta dioica Nutrition 0.000 title claims abstract description 64
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 50
- 239000008601 oleoresin Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000002994 raw material Substances 0.000 claims abstract description 24
- 244000288157 Passiflora edulis Species 0.000 claims abstract description 21
- 235000000370 Passiflora edulis Nutrition 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000011347 resin Substances 0.000 claims abstract description 17
- 229920005989 resin Polymers 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000012074 organic phase Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 150000003839 salts Chemical class 0.000 claims abstract description 5
- 241000208125 Nicotiana Species 0.000 claims description 26
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims description 26
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000000047 product Substances 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 8
- 238000000605 extraction Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000012043 crude product Substances 0.000 claims description 4
- 150000007524 organic acids Chemical class 0.000 claims description 4
- 238000005096 rolling process Methods 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 3
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 239000001630 malic acid Substances 0.000 claims description 3
- 235000011090 malic acid Nutrition 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 235000019505 tobacco product Nutrition 0.000 abstract description 8
- 239000000654 additive Substances 0.000 abstract description 7
- 230000000996 additive effect Effects 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 239000012266 salt solution Substances 0.000 description 8
- 239000003205 fragrance Substances 0.000 description 7
- 239000000284 extract Substances 0.000 description 5
- 239000001622 pimenta officinalis fruit oil Substances 0.000 description 5
- 235000013599 spices Nutrition 0.000 description 4
- 230000009467 reduction Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000000391 smoking effect Effects 0.000 description 3
- 235000013399 edible fruits Nutrition 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 244000223760 Cinnamomum zeylanicum Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 244000270834 Myristica fragrans Species 0.000 description 1
- 235000009421 Myristica fragrans Nutrition 0.000 description 1
- 241000208966 Polygala Species 0.000 description 1
- 235000016639 Syzygium aromaticum Nutrition 0.000 description 1
- 244000223014 Syzygium aromaticum Species 0.000 description 1
- 235000017803 cinnamon Nutrition 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 210000000214 mouth Anatomy 0.000 description 1
- 210000003928 nasal cavity Anatomy 0.000 description 1
- 239000001702 nutmeg Substances 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 235000019654 spicy taste Nutrition 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
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- Manufacture Of Tobacco Products (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention provides a preparation method of passion fruit oil resin and application thereof in cigarettes. The pimenta dioica oil resin is prepared by taking pimenta dioica as a raw material, adding water with the pH value of 2.5-5, heating at 60-90 ℃ for 1-5 hours, separating a liquid, drying the pimenta dioica raw material at 30-45 ℃, taking ethyl acetate as an extracting agent, extracting at 50-75 ℃ for 1-3 hours, concentrating the separated liquid to the density of 0.91-0.92, taking saturated salt water as a washing agent, oscillating for 0.5-3 hours, standing for 2 hours, separating an organic phase, and removing the ethyl acetate. The invention increases the new efficacy and effect of the allspice. The allspice oleoresin is used as an additive of tobacco products, has obvious effect and has good application prospect for developing Chinese style cigarette products with special style.
Description
Technical Field
The invention relates to application of natural plant extracts in tobacco products, in particular to a preparation method of a passion fruit oleoresin and application thereof in cigarettes.
Background
The core competitiveness of the Chinese style cigarette is to form the characteristic style of the product, embody individuation and differentiation and adapt to the smoking habits and consumption needs of vast consumers in China. The essence and spice for Chinese cigarette is the 'soul' of Chinese cigarette product, and is the secret place formed by the style and features of Chinese cigarette. The scientific flavoring and casing in the cigarette is an important means for highlighting the personalized style of the cigarette product. Meanwhile, in order to improve the safety of smoking, the harm reduction and the tar reduction become an important component of Chinese style cigarettes. While reducing the tar of the cigarette, the cigarette enhances and improves the smoke concentration and the fragrance, and only by means of the flavoring and feeding technology. With the deepening of harm and tar reduction work of Chinese style cigarettes, the importance of tobacco flavoring and casing is increasingly shown.
The essence and spice for Chinese style cigarettes with independent intellectual property rights and a new technology are built, the essence and spice are extracted from natural plants, the health idea is led to consumers along with the elegant fragrance of the cigarettes, and the essence and spice is one of basic researches for developing Chinese style cigarettes.
The allspice has mixed fragrance similar to cinnamon, clove and nutmeg, and can be added into cigarettes to endow the cigarettes with special fragrance style. However, the allspice has strong spicy taste, so that the stimulation of cigarettes to oral cavities and nasal cavities can be increased while the cigarette fragrance is enriched, and the mouthfeel of the cigarettes is damaged. The inventor finds out in the research process that: the pimenta dioica fruit extract obtained by directly carrying out water extraction or alcohol extraction on pimenta dioica fruit has obvious spicy feeling, has larger negative effect when being added into cigarettes, and can not meet the use requirement as a cigarette additive.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method and application of a allspice oleoresin for cigarettes.
The technical scheme provided by the invention is as follows: the preparation method of the allspice oleoresin is characterized by comprising the following steps:
(1) pretreatment: the method comprises the steps of taking the allspice as a raw material, adding organic acid into water, adjusting the pH value of the water to be 2.5-5, and then mixing the water with the pH value of 2.5-5 with the allspice according to a mass ratio of 5-15: 1, heating at 60-90 ℃ for 1-5 hours, separating the discharge liquid, and drying the allspice raw material at 30-45 ℃ to obtain a pretreated allspice raw material;
(2) extraction: extracting the pretreated allspice raw material in the step (1) at 50-75 ℃ for 1-3 hours by using ethyl acetate as an extracting agent, and concentrating the separated feed liquid to the density of 0.91-0.92 to obtain an oleoresin crude product, wherein the mass ratio of the ethyl acetate to the allspice is 3-10: 1;
(3) and (3) post-treatment: and (3) taking saturated salt water as a washing agent, and mixing the saturated salt water with the crude oleoresin product extracted in the step (2) according to the mass ratio of 3-10: 1, oscillating for 0.5-3 hours, standing for 2 hours, separating an organic phase, and removing ethyl acetate to obtain the passion fruit oleoresin.
The invention has the following excellent technical scheme: the organic acid in the step (1) is acetic acid, citric acid, malic acid or citric acid.
The invention provides an application method of allspice oleoresin in cigarettes, which is characterized by comprising the following steps: the passion fruit oil resin prepared by the method is added into tobacco shreds of cigarettes according to the mass ratio of 0.01-0.05%.
The invention has the following excellent technical scheme: the passion fruit oil resin is added into tobacco shreds of cigarettes according to the mass ratio of 0.02-0.04%.
The invention further adopts the technical scheme that: dissolving the passion fruit oleoresin in a solvent, spraying the solvent dissolved with the passion fruit oleoresin on cut tobacco in a rolling process of the cut tobacco in cigarette production, and then evaporating the solvent.
The invention has the following excellent technical scheme: the solvent is ethanol with the mass concentration of 95%.
The inventor shows that the added allspice oil resin can effectively increase the aroma when the tobacco products are smoked through a series of smoking test research results, and the aroma is rich; moreover, the allspice oleoresin can also endow the tobacco products with unique fragrance and charm; and the tobacco product has no obvious negative influence on the aspects of mouthfeel, miscellaneous gas, irritation and the like of the tobacco product.
The invention increases the new efficacy and effect of the allspice, takes the allspice oleoresin as the tobacco product additive, has obvious effect and has good application prospect for developing Chinese style cigarette products with special style.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the specific embodiments.
The preparation method of the allspice oil resin provided in embodiment 1 includes the following specific steps:
1, pretreatment: firstly, adding acetic acid into water, adjusting the pH value to be 2.5, and controlling the mass ratio of the water with the adjusted pH value to the allspice to be 15: 1, heating at 65 ℃ for 3 hours, separating the liquid, and drying the allspice raw material at 35 ℃ to obtain a pretreated allspice raw material;
2, extraction: extracting pretreated allspice raw material with ethyl acetate as extractant at 50 deg.C for 3 hr, and concentrating the separated material liquid to density of 0.91 to obtain crude oleoresin product; wherein the mass ratio of the ethyl acetate to the allspice is 3: 1;
3, post-treatment: adopting saturated salt solution as a washing agent, wherein the mass ratio of the saturated salt solution to the crude oleoresin product is 3: 1, oscillating for 0.5 hour, standing for 2 hours, separating out an organic phase, and removing ethyl acetate to obtain the passion fruit oleoresin. The extract can be used as tobacco additive.
The preparation method of the allspice oil resin provided in embodiment 2 includes the following specific steps:
(1) pretreatment: the method comprises the following steps of (1) adding citric acid into water by taking the allspice as a raw material, adjusting the pH value to 3.5, wherein the mass ratio of the water with the adjusted pH value to the allspice is 10: 1, heating at 60 ℃ for 5 hours, separating the discharged liquid, and drying the allspice raw material at 30 ℃ to obtain a pretreated allspice raw material;
(2) extraction: adopting a pretreated allspice raw material, taking ethyl acetate as an extracting agent, wherein the mass ratio of the ethyl acetate to the allspice is 10: 1, extracting at 75 ℃ for 1 hour, and concentrating the separated feed liquid to the density of 0.92 to obtain an oleoresin crude product;
(3) and (3) post-treatment: adopting saturated salt solution as a washing agent, wherein the mass ratio of the saturated salt solution to the crude oleoresin product is 10: 1, oscillating for 3 hours, standing for 2 hours, separating out an organic phase, and removing ethyl acetate to obtain the allspice oleoresin. The extract can be used as tobacco additive.
The preparation method of the allspice oil resin provided in embodiment 3 includes the following specific steps:
(1) pretreatment: firstly, adding malic acid into water, adjusting the pH value to be 4.5, and mixing the water with the adjusted pH value and the allspice according to a mass ratio of 5:1, heating at 80 ℃ for 2 hours, separating the discharged liquid, and drying the allspice raw material at 45 ℃ to obtain a pretreated allspice raw material;
(2) extraction: adopting a pretreated allspice raw material, taking ethyl acetate as an extracting agent, wherein the mass ratio of the ethyl acetate to the allspice is 5:1, extracting for 2 hours at 65 ℃, concentrating the separated feed liquid to the density of 0.91, and obtaining crude oleoresin.
(3) And (3) post-treatment: adopting saturated salt solution as a washing agent, wherein the mass ratio of the saturated salt solution to the crude oleoresin product is 8: 1, fully mixing, oscillating for 1 hour, standing for 2 hours, separating out an organic phase, and removing ethyl acetate to obtain the allspice oleoresin. The extract can be used as tobacco additive.
The preparation method of the passion fruit oil resin provided in embodiment 4 comprises the following specific steps:
(1) pretreatment: the method comprises the following steps of taking the allspice as a raw material, adding citric acid into water, adjusting the pH value to be 5, and adjusting the mass ratio of the water with the adjusted pH value to the allspice to be 8: 1, heating at 90 ℃ for 1 hour, separating the discharged liquid, and drying the allspice raw material at 40 ℃ to obtain a pretreated allspice raw material;
(2) extraction: adopting a pretreated allspice raw material, taking ethyl acetate as an extracting agent, wherein the mass ratio of the ethyl acetate to the allspice is 7: 1, extracting for 2.5 hours at 55 ℃, and concentrating the separated feed liquid to the density of 0.92 to obtain an oleoresin crude product;
(3) and (3) post-treatment: and (3) taking saturated salt solution as a washing agent, fully mixing the saturated salt solution and the crude oleoresin product according to the mass ratio of 5:1, oscillating for 2 hours, standing for 2 hours, separating an organic phase, and removing ethyl acetate to obtain the allspice oleoresin. The extract can be used as tobacco additive.
Example 5 Polygala oil resin prepared by the above method was added to cut tobacco of cigarette
The allspice oleoresin prepared in example 1 was added to the cut tobacco during the rolling of the cut tobacco in cigarette production. The passion fruit oleoresin added into the tobacco shreds accounts for 0.03 percent of the weight of the tobacco shreds. The specific method comprises the steps of firstly dissolving the passion fruit oleoresin in 95% ethanol by mass, uniformly spraying the diluted ethanol in which the passion fruit oleoresin is dissolved on the cut tobacco, and then evaporating the ethanol. And (5) rolling the tobacco shreds into the cigarette sample by a cigarette making machine.
Example 6 Effect test in cigarette Smoke
Weighing 40 g of two finished cut tobacco balanced at the temperature of 22 +/-1 ℃ and the Relative Humidity (RH) of 60 +/-2%, weighing 0.04% of the mass of the allspice oleoresin, diluting the allspice oleoresin with 95% ethanol, uniformly spraying the diluted allspice and unflavored cut tobacco on the cut tobacco by a throat nozzle, balancing the aromatized and unflavored cut tobacco samples in a constant-temperature and constant-humidity box at the temperature of 22 +/-1 ℃ and the RH60 +/-2% for 48 hours, respectively preparing the aromatized and unflavored cut tobacco into cigarettes by a cigarette filler, balancing the aromatized and unflavored cut tobacco samples for 48 hours at the temperature of 22 +/-1 ℃ and the RH 60% +/-2%, and asking a sensory cigarette panel to evaluate the cigarettes.
The evaluation personnel consistently think that the added allspice oil resin can effectively increase the aroma when the tobacco products are smoked, and the aroma is rich; moreover, the allspice oleoresin can also endow the cigarettes with unique fragrance and charm.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (6)
1. A preparation method of allspice oleoresin is characterized by comprising the following steps:
(1) pretreatment: the method comprises the steps of taking the allspice as a raw material, adding organic acid into water, adjusting the pH value of the water to be 2.5-5, and then mixing the water with the pH value of 2.5-5 with the allspice according to a mass ratio of 5-15: 1, heating at 60-90 ℃ for 1-5 hours, separating the discharge liquid, and drying the allspice raw material at 30-45 ℃ to obtain a pretreated allspice raw material;
(2) extraction: extracting the pretreated allspice raw material in the step (1) at 50-75 ℃ for 1-3 hours by using ethyl acetate as an extracting agent, and concentrating the separated feed liquid to the density of 0.91-0.92 to obtain an oleoresin crude product, wherein the mass ratio of the ethyl acetate to the allspice is 3-10: 1;
(3) and (3) post-treatment: and (3) taking saturated salt water as a washing agent, and mixing the saturated salt water with the crude oleoresin product extracted in the step (2) according to the mass ratio of 3-10: 1, oscillating for 0.5-3 hours, standing for 2 hours, separating an organic phase, and removing ethyl acetate to obtain the passion fruit oleoresin.
2. The method of claim 1, wherein the method comprises the steps of: the organic acid in the step (1) is acetic acid, citric acid, malic acid or citric acid.
3. Use of the allspice oleoresin prepared according to the method of claim 1 in cigarettes, characterized in that: the passion fruit oil resin prepared by the method is added into tobacco shreds of cigarettes according to the mass ratio of 0.01-0.05%.
4. The application of the passion fruit oil resin prepared by the preparation method of the passion fruit oil resin according to claim 3 in cigarettes is characterized in that: the passion fruit oil resin is added into tobacco shreds of cigarettes according to the mass ratio of 0.02-0.04%.
5. The use of the allspice oleoresin prepared by the method of claim 3 or 4 in cigarettes, characterized in that: dissolving the passion fruit oleoresin in a solvent, spraying the solvent dissolved with the passion fruit oleoresin on cut tobacco in a rolling process of the cut tobacco in cigarette production, and then evaporating the solvent.
6. The application of the passion fruit oil resin prepared by the preparation method of the passion fruit oil resin according to claim 5 in cigarettes is characterized in that: the solvent is ethanol with the mass concentration of 95%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910089972.5A CN109875109B (en) | 2019-01-30 | 2019-01-30 | Preparation method of allspice oleoresin for cigarettes and application of allspice oleoresin in cigarettes |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910089972.5A CN109875109B (en) | 2019-01-30 | 2019-01-30 | Preparation method of allspice oleoresin for cigarettes and application of allspice oleoresin in cigarettes |
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| CN110591812A (en) * | 2019-09-25 | 2019-12-20 | 湖北中烟工业有限责任公司 | Preparation method and application of allspice oleoresin for cigarettes |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1128194C (en) * | 2000-11-03 | 2003-11-19 | 海南绿田园高新技术发展有限公司 | Process for preparing pepper oil resin |
| CN1128145C (en) * | 2000-11-03 | 2003-11-19 | 海南绿田园高新技术发展有限公司 | Process for preparing piperine |
| CN1458253A (en) * | 2002-05-17 | 2003-11-26 | 徐晓杰 | Method for extracting pepper il resin |
| RU2593110C1 (en) * | 2015-04-20 | 2016-07-27 | Олег Иванович Квасенков | Method for production of hookah smoking composition |
| CN104997158B (en) * | 2015-05-29 | 2017-01-18 | 湖北中烟工业有限责任公司 | Preparation method and application of spicy tobacco flavor extract product |
| CN106221940A (en) * | 2016-10-12 | 2016-12-14 | 湖北中烟工业有限责任公司 | A kind of stage extraction method of allspice quintessence oil and the application in Medicated cigarette thereof |
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