CN105623857A - Preparation method of raisin extract and application of raisin extract in cigarettes - Google Patents
Preparation method of raisin extract and application of raisin extract in cigarettes Download PDFInfo
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- CN105623857A CN105623857A CN201510993232.6A CN201510993232A CN105623857A CN 105623857 A CN105623857 A CN 105623857A CN 201510993232 A CN201510993232 A CN 201510993232A CN 105623857 A CN105623857 A CN 105623857A
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- raisin
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/0003—Compounds of unspecified constitution defined by the chemical reaction for their preparation
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
- A24B15/302—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
- A24B15/303—Plant extracts other than tobacco
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Botany (AREA)
- Agronomy & Crop Science (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
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- Health & Medical Sciences (AREA)
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Abstract
The invention relates to a preparation method of raisin extract. The method comprises the steps of crushing treatment, supercritical extraction and ethanol precipitation treatment. The invention further relates to application of the raisin extract in cigarettes. By means of the preparation method, aroma ingredients of raisin itself cannot be destroyed, and the original flavor of raisin is greatly reserved. The preparation method is simple in technology and convenient to operate. When the raisin extract prepared through the preparation method is added to cigarette tobacco shreds, the smoking quality of the cigarettes can be significantly improved.
Description
[technical field]
The invention belongs to flavouring essence for tobacco field. In particular, it relates to the preparation method of a kind of raisin extract, also relate to the application of described raisin extract in cigarette.
[background technology]
Along with people are to the continuous concern of " smoking is with healthy ", reducing tar and reducing harm progressively becomes the main trend of whole world tobacco industry, and low-coke tar cigarette increases in the ratio of whole cigarette market. But while reducing tar, the flavor matter in tobacco also loses, so compensating aroma technology seems particularly important in perfuming cigarette feeding technique thereupon. Therefore, utilize flavouring essence for tobacco to add effective way that fragrance compensation for low-coke tar cigarette is a significant by fragrant technology.
By adding the flavouring essence for tobacco containing natural product extract in cigarette, it is possible on the basis not changing tobacco this fragrant breeze lattice, promote cigarette flavor matter and perfume quantity, make flue gas exquisiteness soft, cover assorted gas, it is to increase cigarette quality.
Raisin are the fruits of the grape drying in the sunlight or drying under shade, have another name called grass dragon pearl, Portugal. Recording according to China's Chinese materia medica works " Shennong Bencaojing " the earliest, grape, taste is sweet flat, main muscles and bones arthritis with fixed pain caused by dampness, benefit gas, times power, Qiang Zhi, makes us fertile strong, and resistance to famine bears chill, and food is made light of one's life by commiting suicide for a long time, does not always prolong life, can make wine. Modern Chinese medicine is thought, the sweet micro-acid of grape flavor, property are put down, and has invigorating the liver and kidney, replenishing QI and blood, appetizing are promoted the production of body fluid, effect of diuresis. Raisin made by grape, and moisture content is low, rich in nutrition content, are rich in carbohydrate, protein, VITAMIN, amino acid and various lipid acid. The process of raisin made by grape so that raisin are rich in abundant aroma component, such as terpenes, ester class, fatty alcohol, alkanoic, pyrazine, furans etc.
At present, preparation method about raisin extract roughly has following several. CN201110342923.1 " a kind of endophyte of plant bioconversion raisin extract and preparation and the application in tobacco flavoring " thereof, disclose the preparation method of a kind of endophyte of plant bioconversion raisin extract, comprise the cultivation of endophyte of plant, utilize alcohol that raisin carry out reflux extraction and prepare raisin extract, the endophyte of plant cultivated is inoculated in the raisin extract after sterilizing and carries out bioconversion etc. Multiple complex reaction can form various perfume compound, thus changes original local flavor of raisin. It is raw material taking raisin extract that CN201010600441.7 " a kind of tobacco aromatics using and its preparation method " discloses a kind of, add one or more amino acid and solvent, stir into the reaction system of equal, carrying out mailland reaction under oil bath heating condition, its mailland reaction product is as tobacco aromatics using. CN201410629963.8 " preparation method of raisin sub critical extraction thing and the application in cigarette ", discloses one propane, butane or dme as subcritical abstraction solvent, prepares the method for raisin sub critical extraction thing. This method utilizes the flavor matter of raisin self as tobacco aromatics using, does not change original local flavor of raisin.
The applicant, through test of many times, develops the inventive method, adopts supercritical extraction technique to prepare raisin extract. Thus obtained raisin extract can greatly retain the original local flavor of raisin, it can be used as a kind of tobacco aromatics using to add in cigarette, can improve aroma quality, enriching cigarette perfume (or spice), hamony is good, makes flue gas exquisiteness soft, increasing sweet sense, pleasant impression is clean, can significantly improve smoking property of cigarette quality.
[summary of the invention]
[technical problem to be solved]
It is an object of the invention to provide the preparation method of a kind of raisin extract.
It is a further object to provide the application of described raisin extract in cigarette.
[technical scheme]
The present invention is achieved through the following technical solutions.
The present invention relates to the preparation method of a kind of raisin extract, the step of described preparation method is as follows:
(1) pulverization process
Raisin raw material is carried out removal of impurities, then lyophilize 48 hours, carry out pulverization process subsequently, obtain unqualified shape raisin.
Raisin raw material is carried out removal of impurities process, removes in raisin the impurity carried secretly.
Raisin raw material after removal of impurities carries out lyophilize 48 hours in freeze drier. The freeze drier used in the inventive method is that the art is conventional and the product commercially sold, such as, by the serial vertical freeze drier of the FreeZone Freeze Drying Equipment of LABCONCO company of U.S. production and sales.
Owing to the inventive method (2) step is by sample is carried out supercritical extraction process, the state wherein extracting sample will affect the extraction recovery of described supercritical extraction method, generally, unqualified median size is more little, and extraction recovery can be more high. It is preferred, therefore, that the raisin after lyophilize to be carried out rapidly broken wall pulverization process further. But due to raisin sugar degree height, the raisin after pulverizing are unqualified can be gathered into bulk along with temperature rising, not easily calculates order number.
(2) supercritical extraction
Unqualified shape raisin step (1) obtained load supercritical CO2In the extraction kettle of device, adding 50-80wt% aqueous ethanolic solution as entrainment agent, its add-on is the weight 2-5 in unqualified shape raisin times. With supercritical CO2Fluid, as extraction solvent, extracts 3-6 hour under pressure 15-30MPa, temperature 45-55 DEG C of condition. After extraction terminates, decompression separation extract under pressure 10-20MPa, temperature 40-50 DEG C of condition.
Due to supercritical CO2Fluid critical temperature is 31.1 DEG C, and supercritical extraction can close to room temperature and CO2Carry out under atmosphere surrounding, effectively prevent oxidation and the loss of heat-sensitive substance. Therefore, supercritical CO2Abstraction technique can keep the effective constituent of natural phant, and the material of high boiling point, low volatility, easily pyrolysis can be extracted under its boiling temperature; Supercritical CO2Safety non-toxic, ensure that no solvent residue in extract, the pure natural property of product; Supercritical CO2Extraction can conveniently by adjustment temperature and pressure two parameter change CO2The solubility property of fluid, thus improve the receipts rate of product, reach extraction object, simple for process.
Utilize supercritical extraction method extraction essence to be possible not only to effectively extract aromatised fraction, but also product purity can be improved, and its natural flavor can be kept. Raisin itself are rich in the abundant aroma component same or similar with tobacco, such as terpenes, ester class, fatty alcohol, alkanoic, pyrazine, furans etc., its extract adds in cigarette shreds, it is possible to mutually coordinate with flue gas well, plays effect abundant, harmony cigarette perfume (or spice). Raisin contain abundant carbohydrate, protein, VITAMIN, amino acid and various lipid acid, cigarette burning process can well participate in Maillard reaction, produce abundant flavor matter, and the alkaline matter that can neutralize in tobacco, thus reduce assorted gas, making flue gas exquisiteness soft, increase sweet sense, pleasant impression is clean.
The influence factor of supercritical extraction method mainly contains extraction temperature, extracting pressure, entrainment agent etc. The applicant is through test of many times, it is determined that the most suitable parameter of the supercritical extraction used in the inventive method, thus obtains shorter extraction time, higher yield and lower processing cost. Wherein, extraction kettle pressure is 15-30MPa, and extraction temperature is 45-55 DEG C, extraction time 3-6h; Separating still pressure is 10-20MPa, and temperature is 40-50 DEG C. Entrainment agent is 50-80wt% aqueous ethanolic solution, and its add-on is the weight 2-5 in unqualified shape raisin times.
The supercritical extracting equipment used in the methods of the invention can be the common equipment of the art, and can commercially buy, such as, be by the HA221-50-01 type supercritical extraction unit of Huaan, Hai'an company of overcritical equipment company limited production and sales.
(3) alcohol precipitation process
Adding 70-90wt% aqueous ethanolic solution in the extract that step (2) obtains, the add-on of aqueous ethanolic solution is in the weight 4 times of unqualified shape raisin. Stir 1 hour, then leave standstill 10 hours in temperature-10 DEG C of refrigerator-freezers, then incline and supernatant liquor, concentrated except desolventizing, obtain described raisin extract.
The present invention also relates to a kind of raisin extract prepared according to above-mentioned preparation method.
The present invention also relates to the application of described raisin extract in cigarette, described raisin extract 90wt% aqueous ethanolic solution dilutes, the raisin extract employing atomised form of dilution evenly sprays and is added in pipe tobacco, and described raisin extract consumption is the 0.001-0.01% of tobacco quality.
The pipe tobacco thus obtained balances 48 hours in constant temperature (22 DEG C �� 2 DEG C) constant humidity (RH60% �� 5%) case, make cigarette, then organize many perfumers to adopt and blind comment scoring system, the projects such as the gloss of cigarette, fragrance, harmony, assorted gas, pleasant impression and pungency are carried out sensory evaluating smoking's qualification. By smoking result it will be seen that this raisin extract is added in pipe tobacco, while retaining the cigarette perfume (or spice) of tobacco leaf itself, improving aroma quality, enrich cigarette perfume (or spice), hamony is good, makes flue gas exquisiteness soft, reduces assorted gas and pungency.
[useful effect]
The present invention compared with prior art, mainly has following useful effect:
Present invention employs alcohol precipitation preparation method after supercritical extraction, lower extraction temperature can not destroy the aroma component of raisin itself, thus greatly remains the original odour characteristics of raisin. Preparation method's technique of the present invention is simple, and easy to operate, the raisin extract obtained prepared according to the methods of the invention adds in cigarette shreds, can significantly improve smoking property of cigarette quality.
[embodiment]
Non-limiting example is used for illustrating in greater detail the present invention below.
Embodiment 1
(1) pulverization process
Raisin raw material is carried out removal of impurities, then lyophilize 48 hours in freeze drier, carry out pulverization process subsequently, obtain unqualified shape raisin.
(2) supercritical extraction
Get the unqualified shape raisin loading supercritical CO that 500g step (1) obtains2In the extraction kettle of device, add using the 50wt% aqueous ethanolic solution of unqualified shape raisin weight 2 times as entrainment agent, with supercritical CO2Fluid, as extraction solvent, extracts 4.5 hours under pressure 25MPa, temperature 50 DEG C of conditions. After extraction terminates, decompression separation extract under pressure 15MPa, temperature 45 DEG C of conditions.
(3) alcohol precipitation process
Add in the extract obtained in step (2) in the 70wt% aqueous ethanolic solution of unqualified shape raisin weight 4 times, stir 1 hour, then leave standstill 10 hours in temperature-10 DEG C of refrigerator-freezers, then incline and supernatant liquor, concentrated except desolventizing, obtain described raisin extract.
The raisin extract 90wt% aqueous ethanolic solution dilution that will prepare according to above method, evenly it is sprayed onto in pipe tobacco with atomised form by the 0.003% of tobacco quality, constant temperature (22 DEG C �� 2 DEG C) constant humidity (RH60% �� 5%) case balances 48 hours, make cigarette, then allow perfumer adopt the blind method commented to carry out sensory evaluating smoking's qualification.
Its smoking result is: this raisin extract is added in pipe tobacco, while retaining the cigarette perfume (or spice) of tobacco leaf itself, can improve aroma quality, enrich cigarette perfume (or spice), and hamony is good, makes flue gas exquisiteness soft, reduces assorted gas and pungency.
Embodiment 2
(1) pulverization process
Raisin raw material is carried out removal of impurities, then lyophilize 48 hours in freeze drier, carry out pulverization process subsequently, obtain unqualified shape raisin.
(2) supercritical extraction
Get the unqualified shape raisin loading supercritical CO that 500g step (1) obtains2In the extraction kettle of device, add using the 60wt% aqueous ethanolic solution of unqualified shape raisin weight 3 times as entrainment agent, with supercritical CO2Fluid, as extraction solvent, extracts 3.5 hours under pressure 18MPa, temperature 45 DEG C of conditions. After extraction terminates, decompression separation extract under pressure 10MPa, temperature 40 DEG C of conditions.
(3) alcohol precipitation process
Add in the extract obtained in step (2) in the 80wt% aqueous ethanolic solution of unqualified shape raisin weight 4 times, stir 1 hour, then leave standstill 10 hours in temperature-10 DEG C of refrigerator-freezers, then incline and supernatant liquor, concentrated except desolventizing, obtain described raisin extract.
The raisin extract 90wt% aqueous ethanolic solution dilution that will prepare according to above method, evenly it is sprayed onto in pipe tobacco with atomised form by the 0.005% of tobacco quality, constant temperature (22 DEG C �� 2 DEG C) constant humidity (RH60% �� 5%) case balances 48 hours, make cigarette, then allow perfumer adopt the blind method commented to carry out sensory evaluating smoking's qualification.
Its smoking result is: this raisin extract is added in pipe tobacco, while retaining the cigarette perfume (or spice) of tobacco leaf itself, can increase perfume quantity, enrich cigarette perfume (or spice), and hamony is good, makes flue gas exquisiteness soft, reduces assorted gas and pungency, and promote the production of body fluid slightly Hui Tian.
Embodiment 3
(1) pulverization process
Raisin raw material is carried out removal of impurities, then lyophilize 48 hours in freeze drier, carry out pulverization process subsequently, obtain unqualified shape raisin.
(2) supercritical extraction
Get the unqualified shape raisin loading supercritical CO that 500g step (1) obtains2In the extraction kettle of device, add using the 70wt% aqueous ethanolic solution of unqualified shape raisin weight 5 times as entrainment agent, with supercritical CO2Fluid, as extraction solvent, extracts 5.5 hours under pressure 30MPa, temperature 55 DEG C of conditions. After extraction terminates, decompression separation extract under pressure 20MPa, temperature 50 DEG C of conditions.
(3) alcohol precipitation process
Add in the extract obtained in step (2) in the 90wt% aqueous ethanolic solution of unqualified shape raisin weight 4 times, stir 1 hour, then leave standstill 10 hours in temperature-10 DEG C of refrigerator-freezers, then incline and supernatant liquor, concentrated except desolventizing, obtain described raisin extract.
The raisin extract 90wt% aqueous ethanolic solution dilution that will prepare according to above method, evenly it is sprayed onto in pipe tobacco with atomised form by the 0.008% of tobacco quality, constant temperature (22 DEG C �� 2 DEG C) constant humidity (RH60% �� 5%) case balances 48 hours, make cigarette, then allow perfumer adopt the blind method commented to carry out sensory evaluating smoking's qualification.
Its smoking result is: this raisin extract is added in pipe tobacco, while retaining the cigarette perfume (or spice) of tobacco leaf itself, can improve aroma quality, enrich cigarette perfume (or spice), and hamony is good, makes flue gas exquisiteness soft, increases sweet sense, and pleasant impression is clean, can significantly improve smoking property of cigarette quality.
Embodiment 4
(1) pulverization process
Raisin raw material is carried out removal of impurities, then lyophilize 48 hours in freeze drier, carry out pulverization process subsequently, obtain unqualified shape raisin.
(2) supercritical extraction
Get the unqualified shape raisin loading supercritical CO that 500g step (1) obtains2In the extraction kettle of device, add using the 80wt% aqueous ethanolic solution of unqualified shape raisin weight 4 times as entrainment agent, with supercritical CO2Fluid, as extraction solvent, extracts 3 hours under pressure 15MPa, temperature 45 DEG C of conditions. After extraction terminates, decompression separation extract under pressure 10MPa, temperature 45 DEG C of conditions.
(3) alcohol precipitation process
Add in the extract obtained in step (2) in the 90wt% aqueous ethanolic solution of unqualified shape raisin weight 4 times, stir 1 hour, then leave standstill 10 hours in temperature-10 DEG C of refrigerator-freezers, then incline and supernatant liquor, concentrated except desolventizing, obtain described raisin extract.
The raisin extract 90wt% aqueous ethanolic solution dilution that will prepare according to above method, evenly it is sprayed onto in pipe tobacco with atomised form by the 0.001% of tobacco quality, constant temperature (22 DEG C �� 2 DEG C) constant humidity (RH60% �� 5%) case balances 48 hours, make cigarette, then allow perfumer adopt the blind method commented to carry out sensory evaluating smoking's qualification.
Its smoking result is: this raisin extract is added in pipe tobacco, while retaining the cigarette perfume (or spice) of tobacco leaf itself, can increase perfume quantity, enrich cigarette perfume (or spice), and hamony is good, makes flue gas exquisiteness soft, reduces assorted gas and pungency, and promote the production of body fluid slightly Hui Tian.
Embodiment 5
(1) pulverization process
Raisin raw material is carried out removal of impurities, then lyophilize 48 hours in freeze drier, carry out pulverization process subsequently, obtain unqualified shape raisin.
(2) supercritical extraction
Get the unqualified shape raisin loading supercritical CO that 500g step (1) obtains2In the extraction kettle of device, add using the 65wt% aqueous ethanolic solution of unqualified shape raisin weight 4 times as entrainment agent, with supercritical CO2Fluid, as extraction solvent, extracts 6 hours under pressure 20MPa, temperature 50 DEG C of conditions. After extraction terminates, decompression separation extract under pressure 15MPa temperature 40 DEG C of conditions.
(3) alcohol precipitation process
Add in the extract obtained in step (2) in the 85wt% aqueous ethanolic solution of unqualified shape raisin weight 4 times, stir 1 hour, then leave standstill 10 hours in temperature-10 DEG C of refrigerator-freezers, then incline and supernatant liquor, concentrated except desolventizing, obtain described raisin extract.
The raisin extract 90wt% aqueous ethanolic solution dilution that will prepare according to above method, evenly it is sprayed onto in pipe tobacco with atomised form by the 0.01% of tobacco quality, constant temperature (22 DEG C �� 2 DEG C) constant humidity (RH60% �� 5%) case balances 48 hours, make cigarette, then allow perfumer adopt the blind method commented to carry out sensory evaluating smoking's qualification.
Its smoking result is: this raisin extract is added in pipe tobacco, while retaining the cigarette perfume (or spice) of tobacco leaf itself, can improve aroma quality, enrich cigarette perfume (or spice), and hamony is good, makes flue gas exquisiteness soft, increases sweet sense, and pleasant impression is clean, can significantly improve smoking property of cigarette quality.
Claims (9)
1. the preparation method of a raisin extract, it is characterised in that the step of described preparation method is as follows:
(1) pulverization process
Raisin raw material is carried out removal of impurities, then lyophilize 48 hours, carry out pulverization process subsequently, obtain unqualified shape raisin;
(2) supercritical extraction
Unqualified shape raisin step (1) obtained load supercritical CO2In the extraction kettle of device, add aqueous ethanolic solution as entrainment agent, with supercritical CO2Fluid extracts as extraction solvent, after extraction terminates, and decompression separation extract;
(3) alcohol precipitation process
In the extract obtained in step (2), add aqueous ethanolic solution, stir 1 hour, then leave standstill 10 hours in temperature-10 DEG C of refrigerator-freezers, then incline and supernatant liquor, concentrated except desolventizing, obtain described raisin extract.
2. preparation method according to claim 1, it is characterised in that in step (2), described ethanol entrainment agent is 50-80wt% aqueous ethanolic solution, and its add-on is the weight 2-5 in unqualified shape raisin times.
3. extracting method according to claim 1, it is characterised in that in step (2), extraction kettle pressure is 15-30MPa, and temperature is 45-55 DEG C.
4. preparation method according to claim 1, it is characterised in that in step (2), separating still pressure is 10-20MPa, and temperature is 40-50 DEG C.
5. extracting method according to claim 1, it is characterised in that in step (2), the 3-6 hour time of extraction.
6. extracting method according to claim 1, it is characterised in that in step (3), described aqueous ethanolic solution is 70-90wt% aqueous ethanolic solution, and its add-on is in the weight 4 times of unqualified shape raisin.
7. the raisin extract that a preparation method described in claim any one of claim 1-6 prepares.
8. the application of raisin extract according to claim 7 in cigarette, it is characterised in that described raisin extract adds in pipe tobacco.
9. application according to claim 8, it is characterized in that raisin extract 90wt% aqueous ethanolic solution dilutes, the raisin extract employing atomised form of dilution evenly sprays and is added in pipe tobacco, and described raisin extract consumption is the 0.001-0.01% of tobacco quality.
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| CN108822964A (en) * | 2018-06-21 | 2018-11-16 | 湖北中烟工业有限责任公司 | A kind of preparation method of cigarette raisins distillation |
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Address after: 850000 Lhasa economic and Technological Development Zone, Tibet autonomous region, road, investment building, Applicant after: HUABAO FLAVOURS & FRAGRANCES CO.,LTD. Address before: 850000 Lhasa economic and Technological Development Zone, Tibet autonomous region, road, investment building, Applicant before: Huabao flavor Ltd. Address after: 850000 Lhasa economic and Technological Development Zone, Tibet autonomous region, road, investment building, Applicant after: Huabao flavor Ltd. Address before: 201821 Yecheng Road, Shanghai, No. 1299, No. Applicant before: Huabao Flavours & Fragrances Co.,Ltd |
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