CN105011357A - Method for preparing cigarette-used smoked plum extract - Google Patents
Method for preparing cigarette-used smoked plum extract Download PDFInfo
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- CN105011357A CN105011357A CN201510390201.1A CN201510390201A CN105011357A CN 105011357 A CN105011357 A CN 105011357A CN 201510390201 A CN201510390201 A CN 201510390201A CN 105011357 A CN105011357 A CN 105011357A
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- medicinal extract
- smoked plum
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- extraction
- alcohol precipitation
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- 239000000284 extract Substances 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 238000000605 extraction Methods 0.000 claims abstract description 38
- 235000019504 cigarettes Nutrition 0.000 claims abstract description 23
- 239000012528 membrane Substances 0.000 claims abstract description 20
- 238000001556 precipitation Methods 0.000 claims abstract description 19
- 239000012535 impurity Substances 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 10
- 239000006228 supernatant Substances 0.000 claims abstract description 9
- 238000000108 ultra-filtration Methods 0.000 claims description 15
- 239000000706 filtrate Substances 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 239000012141 concentrate Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 239000012510 hollow fiber Substances 0.000 claims description 10
- 239000005543 nano-size silicon particle Substances 0.000 claims description 8
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 8
- 229920000053 polysorbate 80 Polymers 0.000 claims description 8
- 239000000919 ceramic Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 239000012467 final product Substances 0.000 claims description 7
- 238000000703 high-speed centrifugation Methods 0.000 claims description 7
- 238000005374 membrane filtration Methods 0.000 claims description 7
- 102000011759 adducin Human genes 0.000 claims description 4
- 108010076723 adducin Proteins 0.000 claims description 4
- 239000003205 fragrance Substances 0.000 abstract description 2
- 206010013911 Dysgeusia Diseases 0.000 abstract 1
- 238000009833 condensation Methods 0.000 abstract 1
- 230000005494 condensation Effects 0.000 abstract 1
- 230000007794 irritation Effects 0.000 abstract 1
- 235000021018 plums Nutrition 0.000 abstract 1
- 239000000779 smoke Substances 0.000 abstract 1
- 230000000391 smoking effect Effects 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 239000004480 active ingredient Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- -1 albumen Chemical class 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 229920001282 polysaccharide Polymers 0.000 description 2
- 239000005017 polysaccharide Substances 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 244000061176 Nicotiana tabacum Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 240000006394 Sorghum bicolor Species 0.000 description 1
- 235000011684 Sorghum saccharatum Nutrition 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 230000005493 condensed matter Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000001471 micro-filtration Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 235000020098 plum wine Nutrition 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Landscapes
- Preparation Of Fruits And Vegetables (AREA)
- Extraction Or Liquid Replacement (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for preparing cigarette-used smoked plum extract. The method includes the steps of ultrasonic countercurrent extraction of smoked plums, alcohol precipitation of condensed extract, membrane separation of supernatant after alcohol precipitation and condensation. The extraction efficiency of the smoked plum extract and smoking effect of the smoked plum extract in cigarettes are improved. Compared with common smoked plum extract, the extract prepared with the method is excellent in smoke compatibility, rich in fragrance and quality, low in irritation, less in impurities, and clean in aftertaste.
Description
Technical field
The invention belongs to cigarette additive preparing technical field, be specifically related to a kind of preparation method of cigarette smoked plum medicinal extract.
Background technology
Smoked plum is also green plum, and containing compositions such as a large amount of protein, fat, carbohydrate and multiple organic acids, smoked plum extract is a kind of additive conventional in cigarette.CN104188089A discloses the application of a kind of plum extract in cigarette, and green plum liquor made from sorghum soak extraction obtains by it, and this extract effectively can improve the quality of cigarette, improves the aroma quality of cigarette.
Mostly existing smoked plum extract is to adopt water, alcohol to carry out decocting or refluxing extraction, and the extraction efficiency of this preparation method not only active ingredient is very low, and impurity component is a lot, have impact on the evaluation and analysis effect of cigarette.
Membrane separation technique is a kind of emerging high efficient separation technology, and hyperfiltration technique is one wherein, and its general principle utilizes the selective sieve performance of fenestra, to be separated, to purify and condensed matter.In ultra-filtration process, because the impurity such as amino acid, albumen, polysaccharide and the large molecular inorganics that are trapped constantly accumulate on the surface of the film, concentration polarization phenomenon can be produced, gel layer is generated when face impurity concentration reaches a certain limit, the permeability of film is sharply declined, and this makes the application of ultrafiltration be limited dramatically.
Summary of the invention
The object of the invention is to the deficiency existed for existing smoked plum medicinal extract preparation method, provide a kind of extraction efficiency high, the preparation method of the cigarette smoked plum medicinal extract that impurity component is few.The present invention is achieved through the following technical solutions:
For achieving the above object, cigarette smoked plum medicinal extract preparation method provided by the invention, it comprises the following steps:
(1) ultrasonic counter-flow extraction: fresh smoked plum is cleaned up, 50 ~ 80% ethanol of 5 ~ 10 times are added by weight in smoked plum, 1 ~ 3h is soaked under temperature 30 ~ 50 DEG C of conditions, then ultrasonic counter-flow extraction is carried out, the supersonic frequency of described ultrasonic counter-flow extraction is 50 ~ 100KHz, temperature is 30 ~ 50 DEG C, and extraction time is 30 ~ 90min;
(2) alcohol precipitation: by gained extracting liquid filtering, collect filtrate reduced pressure concentration become relative density be 1.15 ~ 1.25 medicinal extract, in medicinal extract, then add 85 ~ 95% ethanol of 3 ~ 5 times by weight, fully stir and leave standstill 8 ~ 12 hours;
(3) UF membrane: get the supernatant after alcohol precipitation, high speed centrifugation removing insoluble impurities, be first the ceramic micro filter membrane filtration of 0.1-2 μm with aperture by centrifugate, then in filtrate, add the nano silicon of 0.05-0.1% by weight, the Tween 80 of 0.01-0.05%, stir 10-30 minute, be that the daltonian hollow fiber ultrafiltration membrane of 15000-20000 carries out separations with molecular cut off concentrated;
(4) concentrated: further for concentrate reduced pressure concentration is become relative density be 1.3 ~ 1.4 medicinal extract, to obtain final product.
Preferably, the preparation method of described cigarette smoked plum medicinal extract comprises the following steps:
(1) ultrasonic counter-flow extraction: fresh smoked plum is cleaned up, 60% ethanol of 8 times is added by weight in smoked plum, 2h is soaked under temperature 40 DEG C of conditions, then ultrasonic counter-flow extraction is carried out, the supersonic frequency of described ultrasonic counter-flow extraction is 60KHz, temperature is 40 DEG C, and extraction time is 60min;
(2) alcohol precipitation: by gained extracting liquid filtering, collect filtrate reduced pressure concentration become relative density be 1.2 medicinal extract, in medicinal extract, then add 95% ethanol of 4 times by weight, fully stir and leave standstill 10 hours;
(3) UF membrane: get the supernatant after alcohol precipitation, high speed centrifugation removing insoluble impurities, be first the ceramic micro filter membrane filtration of 0.45 μm with aperture by centrifugate, then in filtrate, add the nano silicon of 0.06% by weight, the Tween 80 of 0.04%, stir 20 minutes, with molecular cut off be 16000 daltonian hollow fiber ultrafiltration membrane carry out separation concentrate;
(4) concentrated: further for concentrate reduced pressure concentration is become relative density be 1.35 medicinal extract, to obtain final product.
Further preferably, described ultracentrifugal rotating speed is 5000-10000 rev/min.
Further preferably, it is 0.2 ~ 0.8MPa that described hollow fiber ultrafiltration membrane carries out being separated concentrated inlet pressure, and liquid outlet pressure is 0.2 ~ 0.5MPa, and flow velocity is 0.1 ~ 0.5m/s.
Because the grain diameter of nano silicon is between 7-40 nanometer, there is extremely fluffy structure, there is between molecule huge space, its specific area is between 70-400m/g, there is extremely strong rheopexy and thixotropy function, in the present invention for adsorbing contaminant, prevent the impurity be trapped if amino acid, albumen, polysaccharide and large molecular inorganics are at the accumulation of film surface and blocking fenestra.
Tween 80, for improving the rheological characteristic of solution, makes it more easily by milipore filter.
Concentration of alcohol involved in the present invention, all refers to weight concentration, as 60% ethanol, refers in every 100g ethanol water, containing ethanol 60g.
The invention has the advantages that:
1, the present invention adopts ultrasonic counter-flow extraction to smoked plum, and this extracting method makes that effective ingredient recovery rate is higher, solvent load is less, and extraction time is shorter, thus improves extraction efficiency.And carry out under being extracted in lower temperature, active ingredient can be avoided to be subject to heat damage, thus to improve the evaluation and analysis effect of medicinal extract in cigarette.
2, the present invention eliminates the most of impurity in medicinal extract by alcohol precipitation and UF membrane, thus further increases the evaluation and analysis effect of cigarette.
3, the present invention selects the daltonian hollow fiber ultrafiltration membrane of 15000-20000 by lot of experiments, the impurity affecting effect of smokeing panel test in smoked plum extract can be removed to greatest extent by the milipore filter in this aperture, remain easy firing, volatile, and the active ingredient of tobacco aroma can be coordinated.The defects such as the present invention also by first carrying out micro-filtration before ultrafiltration, and adds auxiliary agent and overcomes milipore filter in prior art and easily block and cause ultrafiltration efficiency low, and milipore filter service life is short, the ultrafiltration membrance filter speed in the present invention is fast, and service time is long.
Detailed description of the invention
Below by way of specific embodiment, further Detailed Description is done to the present invention.
Embodiment 1
A preparation method for cigarette smoked plum medicinal extract, it comprises the following steps:
(1) ultrasonic counter-flow extraction: fresh smoked plum is cleaned up, 60% ethanol of 8 times is added by weight in smoked plum, 2h is soaked under temperature 40 DEG C of conditions, then ultrasonic counter-flow extraction is carried out, the supersonic frequency of described ultrasonic counter-flow extraction is 60KHz, temperature is 40 DEG C, and extraction time is 60min;
(2) alcohol precipitation: by gained extracting liquid filtering, collect filtrate reduced pressure concentration become relative density be 1.2 medicinal extract, in medicinal extract, then add 95% ethanol of 4 times by weight, fully stir and leave standstill 10 hours;
(3) UF membrane: get the supernatant after alcohol precipitation, 6000 revs/min of high speed centrifugation removing insoluble impurities, be first the ceramic micro filter membrane filtration of 0.45 μm with aperture by centrifugate, then in filtrate, add the nano silicon of 0.06% by weight, the Tween 80 of 0.04%, stir 20 minutes, with molecular cut off be 16000 daltonian hollow fiber ultrafiltration membrane carry out separation concentrate, the inlet pressure of milipore filter is 0.5MPa, and liquid outlet pressure is 0.3MPa, and flow velocity is 0.2m/s.
(4) concentrated: further for concentrate reduced pressure concentration is become relative density be 1.35 medicinal extract, to obtain final product.
Embodiment 2
A preparation method for cigarette smoked plum medicinal extract, it comprises the following steps:
(1) ultrasonic counter-flow extraction: fresh smoked plum is cleaned up, 80% ethanol of 5 times is added by weight in smoked plum, 3h is soaked under temperature 30 DEG C of conditions, then ultrasonic counter-flow extraction is carried out, the supersonic frequency 50KHz of described ultrasonic counter-flow extraction, temperature is 50 DEG C, and extraction time is 30min;
(2) alcohol precipitation: by gained extracting liquid filtering, collect filtrate reduced pressure concentration become relative density be 1.15 medicinal extract, in medicinal extract, then add 95% ethanol of 3 times by weight, fully stir and leave standstill 8 hours;
(3) UF membrane: get the supernatant after alcohol precipitation, 5000 revs/min of high speed centrifugation removing insoluble impurities, be first the ceramic micro filter membrane filtration of 0.22 μm with aperture by centrifugate, then in filtrate, add the nano silicon of 0.05% by weight, the Tween 80 of 0.01%, stir 10 minutes, with molecular cut off be 15000 daltonian hollow fiber ultrafiltration membrane carry out separation concentrate, the inlet pressure of milipore filter is 0.2MPa, and liquid outlet pressure is 0.2MPa, and flow velocity is 0.1m/s;
(4) concentrated: further for concentrate reduced pressure concentration is become relative density be 1.3 medicinal extract, to obtain final product.
Embodiment 3
A preparation method for cigarette smoked plum medicinal extract, it comprises the following steps:
(1) ultrasonic counter-flow extraction: fresh smoked plum is cleaned up, 50% ethanol of 10 times is added by weight in smoked plum, 1h is soaked under temperature 50 C condition, then ultrasonic counter-flow extraction is carried out, the supersonic frequency 100KHz of described ultrasonic counter-flow extraction, temperature is 30 DEG C, and extraction time is 90min;
(2) alcohol precipitation: by gained extracting liquid filtering, collect filtrate reduced pressure concentration become relative density be 1.25 medicinal extract, in medicinal extract, then add 85% ethanol of 5 times by weight, fully stir and leave standstill 12 hours;
(3) UF membrane: get the supernatant after alcohol precipitation, 10000 revs/min of high speed centrifugation removing insoluble impurities, be first the ceramic micro filter membrane filtration of 1.5 μm with aperture by centrifugate, then in filtrate, add the nano silicon of 0.1% by weight, the Tween 80 of 0.05%, stir 30 minutes, with molecular cut off be 20000 daltonian hollow fiber ultrafiltration membrane carry out separation concentrate, the inlet pressure of milipore filter is 0.8MPa, and liquid outlet pressure is 0.5MPa, and flow velocity is 0.5m/s;
(4) concentrated: further for concentrate reduced pressure concentration is become relative density be 1.4 medicinal extract, to obtain final product.
Test example
The smoked plum medicinal extract obtained by embodiment 1-3 joins in cigarette shreds respectively in the ratio of 0.5 ‰, simultaneously with common smoked plum medicinal extract as a comparison case 1 and 2, wherein comparative example 1 is by smoked plum water boiling and extraction, carry out alcohol precipitation after extract is concentrated, and the supernatant after alcohol precipitation carries out concentrated obtaining again; Smoked plum alcohol reflux extracts and obtains after concentrating by comparative example 2, and effect of smokeing panel test is in table 1.
The effect test of smokeing panel test of table 1 embodiment and comparative example
Test finds, the smoked plum medicinal extract adopting method of the present invention to prepare can significantly improve the fragrance of cigarette, reduces the excitant of flue gas and assorted gas, and good with flue gas harmony, and aroma quality is good, and successful is better than the smoked plum medicinal extract adopting conventional method to prepare.The effect of comprehensively smokeing panel test of embodiment 1 is slightly better than embodiment 2 and 3.
Claims (4)
1. a cigarette preparation method for smoked plum medicinal extract, is characterized in that comprising the following steps:
(1) ultrasonic counter-flow extraction: fresh smoked plum is cleaned up, 50 ~ 80% ethanol of 5 ~ 10 times are added by weight in smoked plum, 1 ~ 3h is soaked under temperature 30 ~ 50 DEG C of conditions, then ultrasonic counter-flow extraction is carried out, the supersonic frequency of described ultrasonic counter-flow extraction is 50 ~ 100KHz, temperature is 30 ~ 50 DEG C, and extraction time is 30 ~ 90min;
(2) alcohol precipitation: by gained extracting liquid filtering, collect filtrate reduced pressure concentration become relative density be 1.15 ~ 1.25 medicinal extract, in medicinal extract, then add 85 ~ 95% ethanol of 3 ~ 5 times by weight, fully stir and leave standstill 8 ~ 12 hours;
(3) UF membrane: get the supernatant after alcohol precipitation, high speed centrifugation removing insoluble impurities, be first the ceramic micro filter membrane filtration of 0.1-2 μm with aperture by centrifugate, then in filtrate, add the nano silicon of 0.05-0.1% by weight, the Tween 80 of 0.01-0.05%, stir 10-30 minute, be that the daltonian hollow fiber ultrafiltration membrane of 15000-20000 carries out separations with molecular cut off concentrated;
(4) concentrated: further for concentrate reduced pressure concentration is become relative density be 1.3 ~ 1.4 medicinal extract, to obtain final product.
2. the cigarette preparation method of smoked plum medicinal extract as claimed in claim 1, is characterized in that comprising the following steps:
(1) ultrasonic counter-flow extraction: fresh smoked plum is cleaned up, 60% ethanol of 8 times is added by weight in smoked plum, 2h is soaked under temperature 40 DEG C of conditions, then ultrasonic counter-flow extraction is carried out, the supersonic frequency of described ultrasonic counter-flow extraction is 60KHz, temperature is 40 DEG C, and extraction time is 60min;
(2) alcohol precipitation: by gained extracting liquid filtering, collect filtrate reduced pressure concentration become relative density be 1.2 medicinal extract, in medicinal extract, then add 95% ethanol of 4 times by weight, fully stir and leave standstill 10 hours;
(3) UF membrane: get the supernatant after alcohol precipitation, high speed centrifugation removing insoluble impurities, be first the ceramic micro filter membrane filtration of 0.45 μm with aperture by centrifugate, then in filtrate, add the nano silicon of 0.06% by weight, the Tween 80 of 0.04%, stir 20 minutes, with molecular cut off be 16000 daltonian hollow fiber ultrafiltration membrane carry out separation concentrate;
(4) concentrated: further for concentrate reduced pressure concentration is become relative density be 1.35 medicinal extract, to obtain final product.
3. the cigarette preparation method of smoked plum medicinal extract as claimed in claim 1 or 2, is characterized in that: described ultracentrifugal rotating speed is 5000-10000 rev/min.
4. the cigarette preparation method of smoked plum medicinal extract as claimed in claim 1 or 2, is characterized in that: it is 0.2 ~ 0.8MPa that described hollow fiber ultrafiltration membrane carries out being separated concentrated inlet pressure, and liquid outlet pressure is 0.2 ~ 0.5MPa, and flow velocity is 0.1 ~ 0.5m/s.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510390201.1A CN105011357B (en) | 2015-07-06 | 2015-07-06 | Method for preparing cigarette-used smoked plum extract |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510390201.1A CN105011357B (en) | 2015-07-06 | 2015-07-06 | Method for preparing cigarette-used smoked plum extract |
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| CN105011357B CN105011357B (en) | 2017-01-11 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107446704A (en) * | 2017-08-25 | 2017-12-08 | 湖北中烟工业有限责任公司 | A kind of preparation method of cigarette strawberry extract |
| CN109315824A (en) * | 2018-09-14 | 2019-02-12 | 横县南方茶厂 | A kind of jasmine tea cigarette and preparation method thereof |
| CN112971200A (en) * | 2021-02-07 | 2021-06-18 | 无锡华叶生物科技有限公司 | Preparation method of plum isolate for cigarettes |
| CN113907394A (en) * | 2021-09-28 | 2022-01-11 | 深圳市真味生物科技有限公司 | Preparation method of apple extract for cigarettes |
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| CN113907394A (en) * | 2021-09-28 | 2022-01-11 | 深圳市真味生物科技有限公司 | Preparation method of apple extract for cigarettes |
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