CN1334328A - Process for extracting prolycopene oil resin with supercritical fluid - Google Patents
Process for extracting prolycopene oil resin with supercritical fluid Download PDFInfo
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- CN1334328A CN1334328A CN 01123601 CN01123601A CN1334328A CN 1334328 A CN1334328 A CN 1334328A CN 01123601 CN01123601 CN 01123601 CN 01123601 A CN01123601 A CN 01123601A CN 1334328 A CN1334328 A CN 1334328A
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- raw material
- resinous
- supercritical fluid
- extraction
- lycopene oleo
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Abstract
A process for extracting lycopene oil resin from tomato or water melon by supercritical fluid (CO2, propane, ethane, or ethene) includes pre-treating for removing sugar, gum and water from raw material, extracting with said supercritical fluid to obtain lycopene oil resin, packing it under protection of inertial gas in dark position or vacuum packing, and low-temp storage. Its advantages are simple process, high efficiency, low energy consumption, no pollution and low cost.
Description
Technical field
The present invention relates to tomato, watermelon etc. is the extracting method that raw material extracts lycopene oleo-resinous, refers to adopt supercritical co, propane, ethane, the method for ethene fluid extraction lycopene oleo-resinous especially.
Background technology
The country of scale operation lycopene oleo-resinous mainly contains Israel in the world today, the U.S., and Germany, Japan and other countries, employed method are solvent extraction method [WO97/48287, WO96/13178 (CN1176577A)].The shortcoming of solvent extraction method is to consume a large amount of valuable organic solvents, the energy consumption height, and the loss of leaching process Lyeopene is big, and dissolvent residual is arranged, extraction yield lower (only being about 80%) etc.
Summary of the invention
For solving the deficiency that above-mentioned existing solvent extraction method extracts the Lyeopene technology, it is raw material with tomato, watermelon etc. that spy of the present invention provides a kind of, adopt supercritical co, propane, ethane, the method of ethene fluid extraction lycopene oleo-resinous uses this method to obtain higher productive rate with the step of more simplifying.
Method of the present invention is made up of following two steps: the pre-treatment of a. raw material: fresh tomato, watermelon and goods thereof need pass through cleaning, fragmentation, separation, desugar, come unstuck, drying and other steps, obtain the raw material of drying, sugar-free, no glue.Add or do not add greases such as an amount of Semen Flos Carthami or linseed oil for step extraction down; B. supercritical fluid extraction lycopene oleo-resinous;
After obtaining lycopene oleo-resinous, need with vacuum-packed mode or lucifuge, fill CO
2Or N
2Gas shiled, low tempertaure storage.
Describe each step of the present invention below in detail:
1. the specific operation process of the pre-treatment of raw material is: extracting used raw material can be fresh tomato, fresh watermelon, also can be its goods, as: tomato-sauce, tomato powder and the waste residue when producing tomato-sauce, produces the filter residue of tomato juice etc.The method of different its pre-treatments of raw material is also different, but the raw material that is used to extract must be the solid material of drying, sugar-free, no glue.With the fresh tomato is example, and the method for pre-treatment is: selected, to clean, and fragmentation is crossed and is filtered out seed and waste material (first kind of raw material).Filtrate is passed through centrifugation again, be separated into two kinds of materials flows: tomato slurries and tomato clear liquid, or obtain slurries (second kind of raw material) and clear liquid (clear liquid generally contains about 90% the separated material that falls, concentrated then be a kind of new tomato product) through plate-and-frame filter press.Slurries (containing solid insoluble) promptly can be used for extracting lycopene oleo-resinous after super-dry.Filtering the first kind of raw material that obtains for the first time also needs drying, then with the isolated tomato skin of whirlwind vibration centrifuging, and also can be as the raw material of extraction lycopene oleo-resinous.As being raw material with tomato-sauce, tomato dry powder etc., also need be through similarly handling.Raw material after the processing adds oil plants such as an amount of Semen Flos Carthami or linseed oil for the step extracted with (also can not add Semen Flos Carthami or linseed oil as required) down.
2. the detailed process of supercritical fluid extraction is: the granularity after the raw material pulverizing＞20 orders are put into extraction kettle, when adopting supercritical carbon dioxide extraction: extracting pressure 25～40MPa, 40～80 ℃ of extraction temperature, extracted under the condition of flow 25～250kg/h 2～3 hours, collect lycopene oleo-resinous in separator, percentage extraction is about 90% under the optimum process condition.Adopt propane be solvent when extracting extraction conditions be: extracting pressure 5.0～15.0MPa, 20～90 ℃ of extraction temperature, flow 5～100kg/h, 2～3 hours extraction time.
Product (lycopene oleo-resinous) with a collection of raw material is put into clarifixator, and behind the homogeneous, CO is filled in can
2Or N
2Gas, stored refrigerated.Whole process need lucifuge.
With WO97/48287, the disclosed technology of WO96/13178 (hereinafter to be referred as prior art) is compared, and the present invention has own exclusive characteristics:
1. the present invention's carbonic acid gas, propane, ethane, the solvent of supercritical fluid extraction is accepted and be applicable to food such as ethene, extracts under supercritical state or liquid condition, and solvent recycles in same system, solvent consumption is little, and extraction agent is cheap, so solvent cost is low.
2. extraction cycle of the present invention is short, and only 2～3 hours, and prior art needs 6～7 hours.
3. it is good that the prepared product of method of the present invention has quality, purity height, free from extraneous odour, no solvent residue, characteristics such as non-environmental-pollution.
4. technology of the present invention is simple, and energy consumption is low.
5. as adopting CO
2Be supercutical fluid, then CO
2Have nontoxicly, do not fire, advantages of cheap price, but the extracting pressure height is arranged, solubleness is low, shortcomings such as equipment manufacturing cost height.If low molecular hydrocarbon classes such as employing propane are supercutical fluid, then the shortcoming of low molecular hydrocarbon class is inflammable, the price height.Advantage is a high-dissolvability, low extracting pressure, and equipment manufacturing cost is low, and the extraction time is short, and energy consumption is low.
6. add in the raw material and contain the high Semen Flos Carthami of unsaturated fatty acid ester, linseed oil, both helped extracting and separating, play the effect of protection lycopene oleo-resinous again.
Employed CO among the present invention
2Cut both ways with two kinds of supercutical fluids of low molecular hydrocarbon class, for macromole and the stronger molecule of polarity, with low molecular hydrocarbon better as extraction agent, for carotenoid, with low molecular hydrocarbon as supercutical fluid ratio CO
2Good.
The specific embodiment
Further describe operating procedure of the present invention with the following specific embodiment that exemplifies. Among the following embodiment Alleged raw material all is the dried powders that make as follows:
Waste residue etc. is when getting fresh tomato, watermelon, catsup, tomato meal and producing catsup, tomato juice Raw material (need to stay skin except seed with making the waste residue of producing catsup, extract lycopene from skin) is beaten earlier Broken pulping, the water that need add several times to raw material moisture, sugared, glue dilutes (warm water is better), and is molten Wherein sugar of solution, glue etc., and by centrifugation are separated into two ones in the slurries of clearly juice and insoluble solid Divide, will contain again the slurries press filtration of insoluble solid by flame filter press, remove most of moisture content wherein, And obtain dry powder (end) shape raw material by vacuum dehydrating at lower temperature and carry out extracting operation of lower step.＜embodiment 1 〉
Extraction conditions: pressure: 35MPa temperature: 70 ℃ of CO2Flow: 25kg/hr raw material granularity: 60～80 order extraction times: equipment used extraction kettle (model HA121-50-02, Haian County, Jiangsu oil scientific research instrument plant) in 2 hours
| Title | Weight (g) | Haematochrome content (mg/100g) | Haematochrome total amount (mg) | Oleoresin productive rate (%) | Haematochrome extraction yield (%) |
| Raw material | 640 | 38.5 | 246.4 | ||
| Extract remainder | 630 | 1.74 | 10.96 | ||
| Oleoresin | 10 | 2344 | 234.4 | 1.56 | 95.13 |
| Title | Weight (Kg) | Haematochrome content (mg/100g) | Haematochrome total amount (g) | Oleoresin productive rate (%) | Haematochrome extraction yield (%) |
| Raw material | 65 | 200 | 130 | ||
| Extract remainder | 64 | 2.5 | 1.6 | ||
| Oleoresin | 0.95 | 12657.89 | 120.25 | 1.46 | 92.5 |
| Title | Weight (g) | Haematochrome content (mg/100g) | Haematochrome total amount (mg) | Oleoresin productive rate (%) | Haematochrome extraction yield (%) |
| Raw material | 400 | 111 | 444 | ||
| Extract remainder | 393 | 20 | 78.6 | ||
| Oleoresin | 6.8 | 5440 | 360 | 1.7 | 83％ |
＜embodiment 4 〉 Extraction conditions: pressure: 12MPa temperature: 100 ℃ of propane flows: 5kg/hr raw material granularity: 60～80 order extraction times: device therefor was with embodiment 1 in 3 hours
| Title | Weight (g) | Haematochrome content (mg/100g) | Haematochrome total amount (mg) | Oleoresin productive rate (%) | Haematochrome extraction yield (%) |
| Raw material | 250 | 128 | 320 | ||
| Extract remainder | 247 | 22 | 54.34 | ||
| Oleoresin | 3.5 | 7650 | 267.8 | 1.4 | 83.7 |
Claims (10)
1, a kind of method with the supercritical fluid extraction lycopene oleo-resinous is characterized in that this method comprises the steps: successively
A. raw material moisture, sugared, glue is carried out the pre-treatment of desugar, glue, water, obtain the exsiccant raw material;
B. use CO
2Or the supercutical fluid of low molecular hydrocarbon class extracts raw material and obtains lycopene oleo-resinous.
2, the method with the supercritical fluid extraction lycopene oleo-resinous according to claim 1, it is characterized in that the waste residue when said raw material is meant fresh tomato, watermelon, tomato-sauce, tomato powder and produces tomato-sauce, tomato juice among the step a, low molecular hydrocarbon class supercutical fluid used among the step b can be selected from propane, ethane, ethene.
3, the method with the supercritical fluid extraction lycopene oleo-resinous according to claim 2, it is characterized in that the specific operation process among the step a is: raw material is carried out that fragmentation, warm water are soaked, desugar, comes unstuck, filters, carry out processed then and get dried feed, dehydration temperaturre is below 100 ℃, then need remove seed, stay skin as raw material with making the waste residue of producing tomato-sauce, from skin, extract Lyeopene.
4, the method with the supercritical fluid extraction lycopene oleo-resinous according to claim 3 is characterized in that the dehydration temperaturre among the step a is below 50 ℃.
5, the method with the supercritical fluid extraction lycopene oleo-resinous according to claim 2 is carried out step b after it is characterized in that adding an amount of Semen Flos Carthami or linseed oil in the step a dried raw material again.
6, the method with the supercritical fluid extraction lycopene oleo-resinous according to claim 2, it is characterized in that the specific operation process among the step b is: the operational condition during with supercritical carbon dioxide extraction: extracting pressure 25～40MPa, 40～80 ℃ of extraction temperature, flow 25～250Kg/h, 2～3 hours extraction time, raw material granularity 60～80 orders.
7, the method with the supercritical fluid extraction lycopene oleo-resinous according to claim 2, it is characterized in that in the specific operation process among the step b operational condition when extracting: extracting pressure 5.0～15.0MPa with supercritical propane, 20～90 ℃ of extraction temperature, flow 5～100Kg/h, 2～3 hours extraction time.
8,, it is characterized in that increasing step c lucifuge packing under the filling protection of inert gas behind the step b according to each described method of claim 1 to 7 with the supercritical fluid extraction lycopene oleo-resinous; Or adopt vacuum-packed back in low temperature storage.
9, the method with the supercritical fluid extraction lycopene oleo-resinous according to claim 8 is characterized in that said rare gas element is CO among the step c
2Or N
2
10, the method with the supercritical fluid extraction lycopene oleo-resinous according to claim 9, it is characterized in that step c specific operation process is: the lycopene oleo-resinous that extraction obtains is placed in the clarifixator, at CO
2Or N
2Homogeneous under the gas shiled, the lucifuge packing is filled CO in the pail pack
2Or N
2Gas, low tempertaure storage.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01123601 CN1334328A (en) | 2001-07-25 | 2001-07-25 | Process for extracting prolycopene oil resin with supercritical fluid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01123601 CN1334328A (en) | 2001-07-25 | 2001-07-25 | Process for extracting prolycopene oil resin with supercritical fluid |
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| CN1334328A true CN1334328A (en) | 2002-02-06 |
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| CN 01123601 Pending CN1334328A (en) | 2001-07-25 | 2001-07-25 | Process for extracting prolycopene oil resin with supercritical fluid |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1315953C (en) * | 2003-09-15 | 2007-05-16 | 广州优宝工业有限公司 | Preparation method of lycopene |
| CN100341950C (en) * | 2005-11-10 | 2007-10-10 | 南京工业大学 | Method for preparing lycopene oleoresin and lycopene |
| CN101505615A (en) * | 2006-08-02 | 2009-08-12 | 皮耶里有限责任公司 | Food supplement based on biological lycopene and process to obtain biological lycopene |
| CN101810225A (en) * | 2010-04-09 | 2010-08-25 | 新疆大学 | Method for producing lycopene oil resin and plant oil rich in lycopene |
| CN101928473A (en) * | 2009-06-22 | 2010-12-29 | 新疆大学 | Method for producing lycopene oleoresin |
| CN102115357A (en) * | 2010-11-17 | 2011-07-06 | 晨光生物科技集团天津有限公司 | Method for refining lycopene oleoresin |
| CN105521618A (en) * | 2016-01-28 | 2016-04-27 | 上海化工研究院 | Inert gas shielded high-pressure liquefied extraction device and extraction method thereof |
| US9434886B2 (en) | 2011-12-31 | 2016-09-06 | Chenguang Biotech Group Co. Ltd. | Process for extracting lycopene |
| CN107235881A (en) * | 2017-06-15 | 2017-10-10 | 中国科学院昆明植物研究所 | The supercritical carbon dioxide extraction method of astaxanthin in transgenic engineering tamato fruit |
| CN109452649A (en) * | 2018-12-29 | 2019-03-12 | 宁夏沃福百瑞枸杞产业股份有限公司 | A kind of fructus lycii zeaxanthin compound oil capsule and pill and preparation method thereof |
-
2001
- 2001-07-25 CN CN 01123601 patent/CN1334328A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1315953C (en) * | 2003-09-15 | 2007-05-16 | 广州优宝工业有限公司 | Preparation method of lycopene |
| CN100341950C (en) * | 2005-11-10 | 2007-10-10 | 南京工业大学 | Method for preparing lycopene oleoresin and lycopene |
| CN101505615A (en) * | 2006-08-02 | 2009-08-12 | 皮耶里有限责任公司 | Food supplement based on biological lycopene and process to obtain biological lycopene |
| CN101928473B (en) * | 2009-06-22 | 2013-09-25 | 新疆大学 | Method for producing lycopene oleoresin |
| CN101928473A (en) * | 2009-06-22 | 2010-12-29 | 新疆大学 | Method for producing lycopene oleoresin |
| CN101810225B (en) * | 2010-04-09 | 2013-01-23 | 新疆大学 | Method for producing lycopene oil resin and plant oil rich in lycopene |
| CN101810225A (en) * | 2010-04-09 | 2010-08-25 | 新疆大学 | Method for producing lycopene oil resin and plant oil rich in lycopene |
| CN102115357A (en) * | 2010-11-17 | 2011-07-06 | 晨光生物科技集团天津有限公司 | Method for refining lycopene oleoresin |
| US9434886B2 (en) | 2011-12-31 | 2016-09-06 | Chenguang Biotech Group Co. Ltd. | Process for extracting lycopene |
| CN105521618A (en) * | 2016-01-28 | 2016-04-27 | 上海化工研究院 | Inert gas shielded high-pressure liquefied extraction device and extraction method thereof |
| CN105521618B (en) * | 2016-01-28 | 2017-08-01 | 上海化工研究院有限公司 | A kind of inert gas shielding high-pressure liquefaction extraction element and its extracting method |
| CN107235881A (en) * | 2017-06-15 | 2017-10-10 | 中国科学院昆明植物研究所 | The supercritical carbon dioxide extraction method of astaxanthin in transgenic engineering tamato fruit |
| CN107235881B (en) * | 2017-06-15 | 2019-06-11 | 中国科学院昆明植物研究所 | The supercritical carbon dioxide extraction method of astaxanthin in transgenic engineering tamato fruit |
| CN109452649A (en) * | 2018-12-29 | 2019-03-12 | 宁夏沃福百瑞枸杞产业股份有限公司 | A kind of fructus lycii zeaxanthin compound oil capsule and pill and preparation method thereof |
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