CN105011357B - Method for preparing cigarette-used smoked plum extract - Google Patents
Method for preparing cigarette-used smoked plum extract Download PDFInfo
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- CN105011357B CN105011357B CN201510390201.1A CN201510390201A CN105011357B CN 105011357 B CN105011357 B CN 105011357B CN 201510390201 A CN201510390201 A CN 201510390201A CN 105011357 B CN105011357 B CN 105011357B
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- extractum
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- 239000000284 extract Substances 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 72
- 238000000605 extraction Methods 0.000 claims abstract description 33
- 235000019504 cigarettes Nutrition 0.000 claims abstract description 22
- 239000012528 membrane Substances 0.000 claims abstract description 19
- 239000012535 impurity Substances 0.000 claims abstract description 14
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 239000006228 supernatant Substances 0.000 claims abstract description 9
- 239000002244 precipitate Substances 0.000 claims description 17
- 239000000706 filtrate Substances 0.000 claims description 14
- 238000000108 ultra-filtration Methods 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 12
- 239000012510 hollow fiber Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- 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
- 239000012141 concentrate Substances 0.000 claims description 7
- 238000005374 membrane filtration Methods 0.000 claims description 7
- 239000012467 final product Substances 0.000 claims description 5
- 102000011759 adducin Human genes 0.000 claims description 4
- 108010076723 adducin Proteins 0.000 claims description 4
- 230000002411 adverse Effects 0.000 claims description 2
- 239000003205 fragrance Substances 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract 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 8
- 238000012360 testing method Methods 0.000 description 7
- 238000000703 high-speed centrifugation Methods 0.000 description 5
- 239000004615 ingredient Substances 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 235000011158 Prunus mume Nutrition 0.000 description 2
- 244000018795 Prunus mume Species 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
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011156 evaluation 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
- 241000208125 Nicotiana Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 235000001014 amino acid Nutrition 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 150000001720 carbohydrates Chemical class 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
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000007850 degeneration 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
- 238000001471 micro-filtration Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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 cigarette dark plum extractum
Preparation method.
Background technology
Dark plum is also Armeniaca mume Sieb., containing substantial amounts of protein, fat, carbohydrate and multiple organic acid
Deng composition, dark plum extract is a kind of additive conventional in Medicated cigarette.CN104188089A discloses one
Planting plum extract application in Medicated cigarette, Armeniaca mume Sieb. jowar wine soak extraction is obtained by it, should
Extract can be effectively improved the quality of Medicated cigarette, improves the aroma quality of Medicated cigarette.
Mostly existing dark plum extract is to use water, ethanol to carry out decocting or reflux, extract, this preparation
The extraction efficiency of mode not only effective ingredient is the lowest, and impurity component is a lot, have impact on commenting of Medicated cigarette
Analysis effect.
Membrane separation technique is a kind of emerging high efficient separation technology, and hyperfiltration technique is one therein, its
Ultimate principle is to utilize fenestra selectivity sieve performance, to separate, to purify and condensed matter.In ultrafiltration
During, owing to impurity such as aminoacid, albumen, polysaccharide and the macromole inorganic matter being trapped is at film table
Constantly accumulate on face, concentration polarization phenomenon can be produced, when face impurity concentration reaches a certain limit
Generating gel layer, make the permeability of film drastically decline, this makes the application of ultrafiltration by dramatically
Limit.
Summary of the invention
Present invention aims to the deficiency that existing dark plum extractum preparation method exists, it is provided that a kind of
Extraction efficiency is high, the preparation method of the cigarette dark plum extractum that impurity component is few.The present invention is by following
Technical scheme realizes:
For achieving the above object, the cigarette dark plum extractum preparation method that the present invention provides, it includes following
Step:
(1) ultrasonic countercurrent extraction: cleaned up by fresh dark plum, adds 5～10 in dark plum by weight
Times 50～80% ethanol, under the conditions of temperature 30～50 DEG C, soak 1～3h, then carry out ultrasonic adverse current and carry
Taking, the supersonic frequency of described ultrasonic countercurrent extraction is 50～100KHz, and temperature is 30～50 DEG C, extracts
Time is 30～90min；
(2) precipitate with ethanol: filtered by gained extracting solution, collects filtrate concentrating under reduced pressure and becomes the relative density to be
The extractum of 1.15～1.25, then adds 85～95% ethanol of 3～5 times, fully in extractum by weight
Stir and stand 8～12 hours；
(3) membrance separation: take the supernatant after precipitate with ethanol, high speed centrifugation removes insoluble impurities, will be centrifugal
Liquid first with the ceramic micro filter membrane filtration that aperture is 0.1-2 μm, then adds in filtrate by weight
The nano silicon of 0.05-0.1%, the Tween 80 of 0.01-0.05%, stirs 10-30 minute, with retaining
Molecular weight is that the daltonian hollow fiber ultrafiltration membrane of 15000-20000 carries out separating concentration；
(4) concentrate: the extractum becoming relative density to be 1.3～1.4 further for concentrated solution concentrating under reduced pressure,
Obtain.
Preferably, the preparation method of described cigarette dark plum extractum comprises the following steps:
(1) ultrasonic countercurrent extraction: cleaned up by fresh dark plum, adds 8 in dark plum by weight
60% ethanol again, soaks 2h under the conditions of temperature 40 DEG C, then carries out ultrasonic countercurrent extraction, described
The supersonic frequency of ultrasonic countercurrent extraction is 60KHz, and temperature is 40 DEG C, and extraction time is 60min；
(2) precipitate with ethanol: filtered by gained extracting solution, collects filtrate and concentrating under reduced pressure becomes relative density to be 1.2
Extractum, in extractum, then add 95% ethanol of 4 times by weight, be sufficiently stirred for and to stand 10 little
Time；
(3) membrance separation: take the supernatant after precipitate with ethanol, high speed centrifugation removes insoluble impurities, will be centrifugal
Liquid first with the ceramic micro filter membrane filtration that aperture is 0.45 μm, then adds 0.06% in filtrate by weight
Nano silicon, the Tween 80 of 0.04%, stir 20 minutes, be 16000 with molecular cut off
Daltonian hollow fiber ultrafiltration membrane carries out separating concentration；
(4) concentrate: the extractum becoming relative density to be 1.35 further for concentrated solution concentrating under reduced pressure, to obtain final product.
It is further preferred that described ultracentrifugal rotating speed is 5000-10000 rev/min.
It is further preferred that described hollow fiber ultrafiltration membrane carries out separating the inlet pressure concentrated it is
0.2～0.8MPa, liquid outlet pressure is 0.2～0.5MPa, and flow velocity is 0.1～0.5m/s.
Owing to the grain diameter of nano silicon is between 7-40 nanometer, there is the most fluffy structure,
Having huge space between molecule, its specific surface area, between 70-400m/g, has extremely strong anti-current
Degeneration and thixotropy function, in the present invention for adsorbing contaminant, prevent the impurity such as amino being trapped
Acid, albumen, polysaccharide and macromole inorganic matter are at the accumulation of film surface and blocking fenestra.
Tween 80 is for improving the rheological characteristic of solution so that it is more easily by ultrafilter membrane.
Concentration of alcohol involved in the present invention, each means weight concentration, such as 60% ethanol, refers to
In every 100g ethanol water, containing ethanol 60g.
It is an advantage of the current invention that:
1, the present invention uses ultrasonic countercurrent extraction to dark plum, and this extracting method makes active ingredient extraction ratio more
Height, solvent load are less, and extraction time is shorter, thus improves extraction efficiency.And be extracted in relatively
Carry out at a temperature of low, it is possible to avoid effective ingredient by heat damage, thus improve extractum in Medicated cigarette
Evaluation and analysis effect.
2, the present invention eliminates the most of impurity in extractum by precipitate with ethanol and membrance separation, thus further
Improve the evaluation and analysis effect of Medicated cigarette.
3, the present invention selects the daltonian hollow fiber ultrafiltration membrane of 15000-20000 by lot of experiments,
Can be removed to greatest extent by the ultrafilter membrane in this aperture and dark plum extracting solution affects the miscellaneous of effect of smokeing panel test
Matter, remains easy firing, volatile, and can coordinate the effective ingredient of tobacco aroma.The present invention is the most logical
Cross and the most first carry out microfiltration, and add auxiliary agent and overcome ultrafilter membrane in prior art easily to block to cause
The defects such as ultrafiltration efficiency is low, and ultrafilter membrane service life is short, the ultrafiltration membrance filter speed in the present invention is fast,
The use time is long.
Detailed description of the invention
Below by way of specific embodiment, the present invention made further Detailed Description.
Embodiment 1
A kind of preparation method of cigarette dark plum extractum, it comprises the following steps:
(1) ultrasonic countercurrent extraction: cleaned up by fresh dark plum, adds 8 in dark plum by weight
60% ethanol again, soaks 2h under the conditions of temperature 40 DEG C, then carries out ultrasonic countercurrent extraction, described
The supersonic frequency of ultrasonic countercurrent extraction is 60KHz, and temperature is 40 DEG C, and extraction time is 60min；
(2) precipitate with ethanol: filtered by gained extracting solution, collects filtrate and concentrating under reduced pressure becomes relative density to be 1.2
Extractum, in extractum, then add 95% ethanol of 4 times by weight, be sufficiently stirred for and to stand 10 little
Time；
(3) membrance separation: taking the supernatant after precipitate with ethanol, 6000 revs/min of high speed centrifugations remove insoluble
Impurity, by centrifugal liquid first with the ceramic micro filter membrane filtration that aperture is 0.45 μm, then by weight in filtrate
Amount adds the nano silicon of 0.06%, the Tween 80 of 0.04%, stirs 20 minutes, with retaining molecule
Amount is that 16000 daltonian hollow fiber ultrafiltration membrane carry out separating concentration, the inlet pressure of ultrafilter membrane
For 0.5MPa, liquid outlet pressure is 0.3MPa, and flow velocity is 0.2m/s.
(4) concentrate: the extractum becoming relative density to be 1.35 further for concentrated solution concentrating under reduced pressure, to obtain final product.
Embodiment 2
A kind of preparation method of cigarette dark plum extractum, it comprises the following steps:
(1) ultrasonic countercurrent extraction: cleaned up by fresh dark plum, adds 5 in dark plum by weight
80% ethanol again, soaks 3h under the conditions of temperature 30 DEG C, then carries out ultrasonic countercurrent extraction, described
Supersonic frequency 50KHz of ultrasonic countercurrent extraction, temperature is 50 DEG C, and extraction time is 30min；
(2) precipitate with ethanol: filtered by gained extracting solution, collects filtrate and concentrating under reduced pressure becomes relative density to be 1.15
Extractum, in extractum, then add 95% ethanol of 3 times by weight, be sufficiently stirred for and to stand 8 little
Time；
(3) membrance separation: taking the supernatant after precipitate with ethanol, 5000 revs/min of high speed centrifugations remove insoluble
Impurity, by centrifugal liquid first with the ceramic micro filter membrane filtration that aperture is 0.22 μm, then by weight in filtrate
Amount adds the nano silicon of 0.05%, the Tween 80 of 0.01%, stirs 10 minutes, with retaining molecule
Amount is that 15000 daltonian hollow fiber ultrafiltration membrane carry out separating concentration, the inlet pressure of ultrafilter membrane
For 0.2MPa, liquid outlet pressure is 0.2MPa, and flow velocity is 0.1m/s；
(4) concentrate: the extractum becoming relative density to be 1.3 further for concentrated solution concentrating under reduced pressure, to obtain final product.
Embodiment 3
A kind of preparation method of cigarette dark plum extractum, it comprises the following steps:
(1) ultrasonic countercurrent extraction: cleaned up by fresh dark plum, adds 10 in dark plum by weight
50% ethanol again, soaks 1h under the conditions of temperature 50 C, then carries out ultrasonic countercurrent extraction, described
Supersonic frequency 100KHz of ultrasonic countercurrent extraction, temperature is 30 DEG C, and extraction time is 90min；
(2) precipitate with ethanol: filtered by gained extracting solution, collects filtrate and concentrating under reduced pressure becomes relative density to be 1.25
Extractum, in extractum, then add 85% ethanol of 5 times by weight, be sufficiently stirred for and to stand 12 little
Time；
(3) membrance separation: taking the supernatant after precipitate with ethanol, 10000 revs/min of high speed centrifugations remove insoluble
Impurity, by centrifugal liquid first with the ceramic micro filter membrane filtration that aperture is 1.5 μm, then by weight in filtrate
Amount adds the nano silicon of 0.1%, the Tween 80 of 0.05%, stirs 30 minutes, with retaining molecule
Amount is that 20000 daltonian hollow fiber ultrafiltration membrane carry out separating concentration, the inlet pressure of ultrafilter membrane
For 0.8MPa, liquid outlet pressure is 0.5MPa, and flow velocity is 0.5m/s；
(4) concentrate: the extractum becoming relative density to be 1.4 further for concentrated solution concentrating under reduced pressure, to obtain final product.
Test example
The dark plum extractum that embodiment 1-3 prepares is added separately in cigarette shreds in the ratio of 0.5 ‰,
Simultaneously with common dark plum extractum as a comparison case 1 and 2, wherein comparative example 1 is by dark plum soak by water
Extracting, extracting solution carries out precipitate with ethanol after concentrating, and the supernatant after precipitate with ethanol carries out being concentrated to give again；Contrast
Example 2 obtains after dark plum alcohol reflux concentration, and effect of smokeing panel test is shown in Table 1.
Table 1 embodiment and the effect test of smokeing panel test of comparative example
Test finds, the dark plum extractum using the method for the present invention to prepare can significantly improve the fragrance of Medicated cigarette,
Reduce zest and the miscellaneous QI of flue gas, and good with flue gas harmony, and aroma quality is good, and effect is the most excellent
In the dark plum extractum using conventional method to prepare.The effect of comprehensively smokeing panel test of embodiment 1 is slightly better than embodiment 2
With 3.
Claims (3)
1. the cigarette preparation method of dark plum extractum, it is characterised in that comprise the following steps:
(1) ultrasonic countercurrent extraction: cleaned up by fresh dark plum, adds 5～10 in dark plum by weight
Times 50～80% ethanol, under the conditions of temperature 30～50 DEG C, soak 1～3h, then carry out ultrasonic adverse current and carry
Taking, the supersonic frequency of described ultrasonic countercurrent extraction is 50～100KHz, and temperature is 30～50 DEG C, extracts
Time is 30～90min；
(2) precipitate with ethanol: filtered by gained extracting solution, collects filtrate concentrating under reduced pressure and becomes the relative density to be
The extractum of 1.15～1.25, then adds 85～95% ethanol of 3～5 times, fully in extractum by weight
Stir and stand 8～12 hours；
(3) membrance separation: take the supernatant after precipitate with ethanol, rotating speed is 5000-10000 rev/min and centrifugal removes
Remove insoluble impurities, by centrifugal liquid first with the ceramic micro filter membrane filtration that aperture is 0.1-2 μm, then to
Filtrate adds the nano silicon of 0.05-0.1%, the Tween 80 of 0.01-0.05%, stirring by weight
10-30 minute, be that the daltonian hollow fiber ultrafiltration membrane of 15000-20000 is carried out point with molecular cut off
From concentration；
(4) concentrate: the extractum becoming relative density to be 1.3～1.4 further for concentrated solution concentrating under reduced pressure,
Obtain.
2. the cigarette preparation method of dark plum extractum as claimed in claim 1, it is characterised in that include following
Step:
(1) ultrasonic countercurrent extraction: cleaned up by fresh dark plum, adds 8 in dark plum by weight
60% ethanol again, soaks 2h under the conditions of temperature 40 DEG C, then carries out ultrasonic countercurrent extraction, described
The supersonic frequency of ultrasonic countercurrent extraction is 60KHz, and temperature is 40 DEG C, and extraction time is 60min；
(2) precipitate with ethanol: filtered by gained extracting solution, collects filtrate and concentrating under reduced pressure becomes relative density to be 1.2
Extractum, in extractum, then add 95% ethanol of 4 times by weight, be sufficiently stirred for and to stand 10 little
Time；
(3) membrance separation: take the supernatant after precipitate with ethanol, rotating speed is 6000 revs/min and is centrifuged off insoluble
Property impurity, by centrifugal liquid first with the ceramic micro filter membrane filtration that aperture is 0.45 μm, then presses in filtrate
Weight adds the nano silicon of 0.06%, the Tween 80 of 0.04%, stirs 20 minutes, with retaining point
Son amount is that 16000 daltonian hollow fiber ultrafiltration membrane carry out separating concentration；
(4) concentrate: the extractum becoming relative density to be 1.35 further for concentrated solution concentrating under reduced pressure, to obtain final product.
3. the cigarette preparation method of dark plum extractum as claimed in claim 1 or 2, it is characterised in that: institute
State hollow fiber ultrafiltration membrane carrying out separating the inlet pressure concentrated is 0.2～0.8MPa, liquid outlet pressure
Being 0.2～0.5MPa, flow velocity is 0.1～0.5m/s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510390201.1A CN105011357B (en) | 2015-07-06 | 2015-07-06 | Method for preparing cigarette-used smoked plum extract |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510390201.1A CN105011357B (en) | 2015-07-06 | 2015-07-06 | Method for preparing cigarette-used smoked plum extract |
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| Publication Number | Publication Date |
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| CN105011357A CN105011357A (en) | 2015-11-04 |
| CN105011357B true CN105011357B (en) | 2017-01-11 |
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| CN201510390201.1A Active CN105011357B (en) | 2015-07-06 | 2015-07-06 | Method for preparing cigarette-used smoked plum extract |
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| 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 |
| CN109315824B (en) * | 2018-09-14 | 2021-05-25 | 横县南方茶厂 | Jasmine tea cigarette and making method thereof |
| CN112971200B (en) * | 2021-02-07 | 2023-07-14 | 无锡华叶生物科技有限公司 | Preparation method of plum isolate for cigarettes |
| CN113907394B (en) * | 2021-09-28 | 2023-06-13 | 深圳市真味生物科技有限公司 | Preparation method of apple extract for cigarettes |
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| CN102851118B (en) * | 2011-06-27 | 2013-12-25 | 湖北中烟工业有限责任公司 | Extraction process of rose essence for cigarette |
| CN102754784B (en) * | 2012-08-08 | 2013-06-19 | 天宁香料（江苏）有限公司 | Method for preparing tamarind fruit extract and application of same in edible essence |
| CN104672188A (en) * | 2013-12-03 | 2015-06-03 | 刘群秀 | Compound used as food sweetening agent |
| CN104082846B (en) * | 2014-07-24 | 2016-02-24 | 中国烟草总公司郑州烟草研究院 | The application of a kind of hollyhock seed extract in cigarette |
| CN104257763B (en) * | 2014-10-17 | 2016-11-09 | 内蒙古中兴华冠生物工程股份有限公司 | A kind of saline cistanche water extract, preparation method and its usage |
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