CN103555422A - Method for extracting plamochromic pigment in tobacco by use of subcritical extraction technology - Google Patents
Method for extracting plamochromic pigment in tobacco by use of subcritical extraction technology Download PDFInfo
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- CN103555422A CN103555422A CN201310528306.XA CN201310528306A CN103555422A CN 103555422 A CN103555422 A CN 103555422A CN 201310528306 A CN201310528306 A CN 201310528306A CN 103555422 A CN103555422 A CN 103555422A
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Abstract
The invention discloses a method for extracting plamochromic pigment in tobacco and tobacco product by use of a subcritical extraction technology, belonging to the field of a biological extraction method. The method comprises the following steps: putting a sample into a closed extraction pot and vacuumizing; injecting a proper amount of extraction solvent into the extraction pot, and extracting by timing and metering, wherein the extraction time is 10-30 minutes, and 3-5 times of extraction is performed; after the extraction, pumping out the liquid solvent containing the extract plamochromic pigment; performing desolventizing treatment on the raw material and plamochromic pigment respectively to finish separation of the plamochromic pigment in the tobacco or tobacco product from the solvent to obtain a pigment extract; and after the desolventizing, taking out the material from the extraction pot. The removed solvent is recycled. According to the method, the subcritical extraction technology adopting a subcritical fluid as an extraction medium is a low-temperature low-pressure processing process, the energy consumption is low, the extraction efficiency is high, and the product quality is good, thereby being favorable for realizing comprehensive utilization of the raw material and production of high-value-added products.
Description
Technical field
The present invention relates to one grow tobacco or tobacco product in the extracting method of plamochromic pigment, especially a kind of by the method for plamochromic pigment in subcritical abstraction technology rapid extraction tobacco and tobacco product, belong to biological extracting process field.
Background technology
Plamochromic pigment class material is the important fragrance precursor that affects tobacco leaf visual appearance and interior quality, mainly comprise chlorophyll (Chlorophyll) and carotenoid (Carotenoid), to the correlative study of Tobacco Plastid Pigment at home and abroad tobacco industry be a focus always.Scientific worker has furtherd investigate the formation of plamochromic pigment in tobacco leaf, conversion and degradation rule both at home and abroad, illustrated the formation of plamochromic pigment and degraded product thereof and Flue-cured tobacco Quality, and with the relation of the process such as heredity, ecology, cultivation, modulation, alcoholization, this is to having important theory value and realistic meaning by biological and agronomic measures raising tobacco aroma quality and perfume quantity.But the Physiology and biochemistry basis that plamochromic pigment degraded and aroma substance are produced, extraction and the perfumed applications of Tobacco Plastid Pigment are inquired into less.So, set up rapid extraction and the measuring method of plamochromic pigment in tobacco sample, by contribute to further to determine pigment content and quality of tobacco relation, determine scientific and reasonable modulation and ageing condition, and have great importance at the aspects such as degree that become more meticulous that improve cigarette tobacco leaf formulation.
Chlorophyll in plamochromic pigment and carotenoid class pigment stability are poor, all require low temperature, lucifuge, quick during extraction and determination.Main method for extracting pigment is extraction process at present, the microwave extracting and ultrasonic extraction and supercritical fluid extraction (the number of patent application 201210019887.X that comprise solvent extraction, solvent extraction supplementary means, 200810058741.X, 200810058763.6).The extraction agent of solvent extraction (soda acid) method is seriously polluted and have peculiar smell and a dissolvent residual; And as microwave extracting and the ultrasonic extraction of solvent extraction supplementary means, technology is many at laboratory stage at present, following volume production scale need to break through; The equipment of supercritical fluid extraction must be high pressure resistant, therefore also more complicated and cost is high in design, not yet has the report of suitability for industrialized production at present.
Summary of the invention
The object of the present invention is to provide one grow tobacco and tobacco product in the effective rapid extracting method of plamochromic pigment, to achieve these goals, the concrete grammar step of the technical program is:
1) charging: pretreated tobacco or tobacco product raw material are sent in airtight extractor, and charge amount is not more than 80% of extractor volume, and extractor is vacuumized.
2) extraction: inject appropriate subcritical fluids as extraction solvent until by the complete submergence of sample in extractor, carry out 3～5 extractions, extraction time is 10～30 minutes, and temperature is 0～60 ℃, and pressure is the saturation vapour pressure of solvent for use under corresponding extraction temperature.Auxiliary with 10～200rpm mechanical stirring (or bottom air-blowing, ultrasonic), to improve extraction efficiency in extraction process.
3) material precipitation: after extraction finishes, extract the liquid solvent that contains extract plamochromic pigment out, raw material and plamochromic pigment are carried out respectively to carrying out precipitation treatment, complete plamochromic pigment and separated from solvent in tobacco or tobacco product.During precipitation, temperature can change between 0～60 ℃ in tank, and when maintaining temperature of charge and being not less than 10 ℃, solvent removal effect is better.After precipitation completes, from extractor, take out material.All solvent recovery cycle that remove are used.
4) washing: gained pigment medicinal extract is again with anti-oxidant washing lotion washing 2～3 times, and the medicinal extract after washing is the plamochromic pigment of slightly carrying.
5) solvent recuperation: the solvent gas evaporating from material and in extraction liquid, through compressor compresses liquefaction, solvent streams back dissolving agent circulation tank, recycles.
The time of described extraction is 10～30 minutes.
Described subcritical fluids solvent is one or more the mixing in propane, butane, Tetrafluoroethane, dme.
In described filter residue, plamochromic pigment remains in below 0.8%.
The oxidation inhibitor butylated hydroxytoluene that described anti-oxidant washing lotion is 90% acetone and 0.1～1.0% is formulated.
Described extraction Raw and solvent ratio are: 1:1～10.
Described precipitation extraction temperature is 0～60 ℃, and pressure is 0.1～1.0Mpa.
When described raw material is the tobacco leaf goods after baking, before inserting extractor, also pass through pre-treatment, dry 0.5～10h, pulverizing and cross 1～100 mesh sieve.Temperature of charge≤100 ℃ during pre-treatment; When raw material is the new fresh tobacco leaf in field, should be freeze-drying at-100～0 ℃, conducting powder is broken and sieve.
The present invention adopts subcritical fluids (being mainly propane, butane, Tetrafluoroethane, dme) for extracting the subcritical abstraction technology of medium, is the course of processing of a low-temp low-pressure.Energy consumption of the present invention is low, and extraction efficiency is high, superior product quality, and yield surpasses 97%; And the variable color of never degenerating of gained plamochromic pigment, dissolvent residual is far below 1ppm, and quality meets edible and medical standard completely, and every quality index all reaches export standard, is conducive to the comprehensive utilization of raw material and the realization of high added value processing.
Accompanying drawing explanation
Fig. 1 extracts schema
Embodiment
embodiment 1
According to sample sampling standard, extract cured tobacco leaf sample 500g, at 40 ℃ of following 4h of drying, pulverize, cross 40 mesh sieve, sample preparation finishes; Accurately take sample 200.0g after preparation, insert airtight extractor, vacuumize after closing feeding-passage, inject appropriate butane solvent to submergence sample completely, under the molten condition that is 0.29MPa than 1:3,30 ℃ of temperature, pressure of material, carry out 3 extractions, each 30min; After having extracted, carry out solvent removal processing, and stripped sample is taken out from tank; The extraction liquid of gained enters vapo(u)rization system, makes solvent gasification separated with extract, obtains plamochromic pigment medicinal extract.The solvent gas evaporating from tobacco sample and extraction liquid, through compressor compresses liquefaction, solvent streams back dissolving agent circulation tank, recycles.Extraction gained plamochromic pigment medicinal extract uses anti-oxidant washing lotion (90% acetone and 0.1% oxidation inhibitor butylated hydroxytoluene are formulated) to wash again 2～3 times, and gained medicinal extract is the plamochromic pigment of slightly carrying.The yield of this Technology reaches 97%, and the variable color of never degenerating of gained plamochromic pigment, and dissolvent residual is lower than 1ppm.Quality meets edible and medical standard completely, and every quality index all reaches relevant national standard.
embodiment 2
Sample is cigarette finished product 200g, expects moltenly than 1:4, and extraction is dme with solvent, and pressure is 0.68MPa, carries out 4 times and extracts, and all the other treatment condition are with embodiment 1.The plamochromic pigment that this Technology gained plamochromic pigment yield is 98%, the variable color of never degenerating, dissolvent residual is lower than 1ppm.Quality meets edible and medical standard completely, and every quality index all reaches relevant national standard.
embodiment 3
Get the new fresh tobacco leaf 3000g in field, freeze-drying at-20 ℃, pulverizes, and crosses 40 mesh sieve, and sample preparation finishes; Accurately take the rear sample 200.0g of preparation, insert airtight extractor and vacuumize, then the appropriate extraction of injection is molten than 1:5 to expecting with solvent Tetrafluoroethane, and pressure is 0.77MPa, and all the other conditions, with embodiment 1, are carried out 5 extractions, at every turn 30min; After extraction finishes, according to the method desolvation in embodiment 1, take out and washing sample.It is 99% plamochromic pigment that this Technology can be produced yield, and the variable color of never degenerating of gained pigment, and dissolvent residual is far below 1ppm.Quality meets edible and medical standard completely, and every quality index all reaches relevant national standard.
It should be noted last that: above embodiment is only in order to explanation, and unrestricted technical scheme of the present invention, although the present invention is had been described in detail with reference to above-described embodiment, those of ordinary skill in the art is to be understood that: still can modify or be equal to replacement the present invention, and not departing from any modification or partial replacement of the spirit and scope of the present invention, it all should be encompassed in the middle of claim scope of the present invention.
Claims (8)
1. utilize subcritical abstraction technology to extract a method for Plastid Pigment from Tobacco, its feature comprises the steps:
1) extract: will insert in extractor through pretreated tobacco or tobacco product raw material, and after airtight vacuumizing, inject
Appropriate subcritical fluids, as extracting solvent, is flooded raw material completely, carries out 3～5 times of plamochromic pigment under certain condition and extracts;
2) desolventizing: after extraction finishes, under 10～60 ℃ of conditions, extract the liquid solvent that contains plamochromic pigment out, raw material and plamochromic pigment are carried out respectively to carrying out precipitation treatment, complete plamochromic pigment and separated from solvent in tobacco or tobacco product, obtain pigment medicinal extract, finally control the residual of plamochromic pigment in raw material and reach below 0.8%, all solvent recovery cycle that remove are used;
3) washing: anti-oxidant washing lotion washing 2～3 times for gained pigment medicinal extract, the medicinal extract after washing is the plamochromic pigment of slightly carrying.
2. the extracting method of plamochromic pigment claimed in claim 1, is characterized in that described extraction conditions is: extraction pressure is 0.1～1.0Mpa, and extraction time is 10～30 minutes, and extracting temperature is 0～60 ℃.
3. the extracting method of plamochromic pigment claimed in claim 1, is characterized in that described subcritical fluids is one or more the mixing in propane, butane, Tetrafluoroethane, dme.
4. the extracting method of plamochromic pigment claimed in claim 1, is characterized in that described extraction Raw and extraction solvent ratio are: 1:1～10.
5. the extracting method of plamochromic pigment claimed in claim 1, is characterized in that can using mechanical stirring to make material and solvent in described leaching process.
6. the extracting method of plamochromic pigment claimed in claim 1, is characterized in that the oxidation inhibitor butylated hydroxytoluene that described anti-oxidant washing lotion is 90% acetone and 0.1～1.0% is formulated.
7. the extracting method of plamochromic pigment claimed in claim 1, is characterized in that described wash temperature is 0～60 ℃, and pressure is 0.1～1.0Mpa.
8. the extracting method of plamochromic pigment claimed in claim 1 while it is characterized in that described raw material is the tobacco leaf goods after baking, needs pre-treatment before inserting extractor, at 0～100 ℃, dries 0.5～10h, pulverizing and crosses 1～100 mesh sieve; When raw material is the new fresh tobacco leaf in field ,-100～0 ℃ of freeze-drying, then pulverize and sieve.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103977595A (en) * | 2014-05-23 | 2014-08-13 | 中国烟草总公司郑州烟草研究院 | Method for reducing content of heavy metal in extract for cigarettes by subcritical extraction technology |
| CN105132176A (en) * | 2015-09-28 | 2015-12-09 | 中国烟草总公司郑州烟草研究院 | Preparation method of Mao cigarette extract and application of Mao cigarette extract to cigarette filter stick |
| CN107033626A (en) * | 2017-04-28 | 2017-08-11 | 常德华馥生物技术有限公司 | A kind of method that subcritical abstraction is combined separate tobacco natural pigment with molecular distillation |
| CN107057855A (en) * | 2017-01-13 | 2017-08-18 | 河南工业大学 | A kind of ultrasound removal is subcritical to produce the residual molten method of giving off a strong fragrance chilli seed crude oil |
| CN112755156A (en) * | 2021-02-25 | 2021-05-07 | 河南骨痹中医研究院(有限合伙) | External traditional Chinese medicine preparation for treating HPV infection and preparation method thereof |
| CN112755142A (en) * | 2021-02-25 | 2021-05-07 | 河南骨痹中医研究院(有限合伙) | Skin treatment cream and preparation method thereof |
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| CN101487820A (en) * | 2008-01-18 | 2009-07-22 | 河南中烟工业公司 | Fast extraction and measurement method for plastid pigment in tobacco and tobacco products |
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2013
- 2013-10-30 CN CN201310528306.XA patent/CN103555422A/en active Pending
Patent Citations (1)
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| CN101487820A (en) * | 2008-01-18 | 2009-07-22 | 河南中烟工业公司 | Fast extraction and measurement method for plastid pigment in tobacco and tobacco products |
Non-Patent Citations (1)
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| 刘月蓉等: "天然植物精油提取技术——亚临界流体萃取", 《莆田学院学报》, vol. 18, no. 2, 30 April 2011 (2011-04-30), pages 67 - 70 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103977595A (en) * | 2014-05-23 | 2014-08-13 | 中国烟草总公司郑州烟草研究院 | Method for reducing content of heavy metal in extract for cigarettes by subcritical extraction technology |
| CN103977595B (en) * | 2014-05-23 | 2015-11-18 | 中国烟草总公司郑州烟草研究院 | A kind of method utilizing subcritical abstraction technology to reduce tobacco extract content of beary metal |
| CN105132176A (en) * | 2015-09-28 | 2015-12-09 | 中国烟草总公司郑州烟草研究院 | Preparation method of Mao cigarette extract and application of Mao cigarette extract to cigarette filter stick |
| CN107057855A (en) * | 2017-01-13 | 2017-08-18 | 河南工业大学 | A kind of ultrasound removal is subcritical to produce the residual molten method of giving off a strong fragrance chilli seed crude oil |
| CN107033626A (en) * | 2017-04-28 | 2017-08-11 | 常德华馥生物技术有限公司 | A kind of method that subcritical abstraction is combined separate tobacco natural pigment with molecular distillation |
| CN112755156A (en) * | 2021-02-25 | 2021-05-07 | 河南骨痹中医研究院(有限合伙) | External traditional Chinese medicine preparation for treating HPV infection and preparation method thereof |
| CN112755142A (en) * | 2021-02-25 | 2021-05-07 | 河南骨痹中医研究院(有限合伙) | Skin treatment cream and preparation method thereof |
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Inventor after: Pang Huili Inventor after: Ma Yuping Inventor after: Wang Wenling Inventor after: Qin Guangyong Inventor after: Qi Kun Inventor before: Pang Huili Inventor before: Qin Guangyong Inventor before: Qi Kun Inventor before: Wang Wenling Inventor before: Ma Yuping |
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Effective date of registration: 20140928 Address after: 455000 Henan Anyang Development Zone advanced technology equipment Park Applicant after: HENAN YALINJIE BIOLOGICAL TECHNOLOGY CO., LTD. Applicant after: Zhengzhou University Applicant after: China Tobacco Henan Industrial Co., Ltd. Address before: 455000 Henan Anyang Development Zone advanced technology equipment Park Applicant before: HENAN YALINJIE BIOLOGICAL TECHNOLOGY CO., LTD. Applicant before: Zhengzhou University |
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Correction item: Applicant|Address|Applicant Correct: Henan Yalinjie Biological Technology Co., Ltd.|455000 Henan Anyang Development Zone advanced technology equipment Park|Zhengzhou University|China Tobacco Henan Industrial Co., Ltd. False: HENAN YALINJIE BIOLOGICAL TECHNOLOGY CO., LTD.|455000 Henan Anyang Development Zone advanced technology equipment Park|Zhengzhou University|China Tobacco Henan Industrial Co., Ltd. Number: 43 Volume: 30 |
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Application publication date: 20140205 |