CN1112410C - Method for extracting solapurpurin - Google Patents
Method for extracting solapurpurin Download PDFInfo
- Publication number
- CN1112410C CN1112410C CN00129943A CN00129943A CN1112410C CN 1112410 C CN1112410 C CN 1112410C CN 00129943 A CN00129943 A CN 00129943A CN 00129943 A CN00129943 A CN 00129943A CN 1112410 C CN1112410 C CN 1112410C
- Authority
- CN
- China
- Prior art keywords
- lycopene
- drip washing
- acetone
- tomato
- present
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a method for extracting lycopene, which belongs to the field of food processing. The method for extracting lycopene is mainly characterized in that raw materials to be extracted are used as filling agents, and the raw materials are washed by solvents so as to extract lycopene by using natural gravity or a pressurization method. The present invention provides a new way for processing tomatoes, expanding planting areas and the deep processing of the tomatoes.
Description
The present invention relates to a kind of extracting method of Lycopene.
Lycopene is the fat-soluble natural pigment of a class, and the very strong anti-oxidation ability that it had and the preventive and therapeutic effect of some tumour confirmed by kinds of experiments now has been used to the production of healthcare products, is in great demand on the world market.Lyeopene mainly is present in the middle of tomato and the goods thereof, though the tomato product of China occupies very big ratio in the international market, but, a large amount of extractions of Lyeopene have been limited because that China accounts in the tomato of production dominant position Lycopene content at present is very not high.
Japanese patent laid-open 9-183914, spy open the extracting method that flat 9-313167 discloses a kind of Lycopene in the prior art, because this method relates to high speed centrifugation, solid-liquid separation and liquid is carried out membrane filtration, step such as concentrates, therefore complicated operation is unsuitable for batch production production.The patent CN1176577 of Markert Sim Chemical Factory Co., Ltd discloses a kind of technology of preparing of Lyeopene, the tomato that is about to contain the 100ppm Lyeopene is processed, with 50 ℃ of hot ethyl acetates, twice extraction, after the solvent evaporation, obtain the oleoresin of about 5% Lycopene.And the data of grasping according to us, the Lycopene content of the most of tomato varieties of China does not also reach this level at present, uses method of extraction twice, can not get content at all and be 5% crude product; In addition, the organic solvent ethyl acetate of heat is volatilized in air seriously, has also brought atmospheric pollution and unsafe factor.
The objective of the invention is at the problems referred to above, propose a kind of not high raw material of existing Lycopene content that utilizes and carry out the extraction of Lycopene and the method for purifying.
What the present invention adopted is that chromatography or conventional pot process extract Lyeopene, the column type of column chromatography and filler a multitude of names in general, and manufacturer constantly puts out a new product, the birth of undoubted every kind of new column type and new carrier, bring new vitality with separating all for stratographic analysis, this is the basis of chromatogram widespread use, will seldom state at this.This law is different from above-mentioned chromatographic process, but with the starting material that are extracted as weighting agent, make eluent with solvent such as ethanol, acetone and similar reagents thereof etc. then and extract Lycopene.The used solvent of the present invention all refers to allow in the food food grade reagent of use.
Chromatography concrete operations of the present invention are as follows:
1. got tomato slurries or the direct upper prop of tomato-sauce after the raw material dry powder of 50 mesh sieves or bright tomato are squeezed the juice.The present invention also can add an amount of dispersion agent, mixing upper prop according to circumstances.Dispersion agent of the present invention is meant and does not cause that extract physics and chemical property change, the eluent generation chemical reaction of also getting along well, and help that raw material disperses and the material of solvent elution, and as: quartz sand, silica gel and other material well known to those skilled in the art thereof.
2. use earlier adequate amount of ethanol, the method drip washing pillar of employing natural gravity or pressurization is to remove impurity such as soluble sugar in the raw material and pure dissolubility pigment.
3. use acetone class reagent instead and continue the drip washing pillar, thin out until color, collect this elutriant, concentrate, can obtain the Lycopene raw product.Acetone class reagent of the present invention comprises: acetone, ethyl acetate etc. well known to a person skilled in the art material.
The operating process that conventional can of the present invention is extracted is as follows:
After drying contained the Lycopene raw material pulverizing, add an amount of ethanol, stirred 30--120 minute, centrifugal again or filter (this process can be carried out 2--3 time according to circumstances), abandoning supernatant; Press 1 in precipitating partly: 9-11 (volume ratio) adds acetone class reagent, stirs extraction 60--120 minute, centrifugal or filtration (this process can be carried out 2-3 time), and collection solution concentrates and promptly gets the Lycopene crude product.
More highly purified if desired Lycopene product, can be extracting resulting Lycopene raw product through resulting Lycopene raw product of column chromatography or conventional can, in 1: the ratio of 4-6 is adorned post after sneaking into dispersion agent, earlier with an amount of alcohol solvent drip washing, continue to remove impurity, and then use the solution that the drip washing of acetone kind solvent obtains containing the higher degree Lycopene instead, concentrate this solution and can obtain highly purified Lycopene product.
Alcoholic acid usage quantity of the present invention directly influences the purity and the productive rate of Lycopene in the finished product, must adjust at the raw material and the product desired degree of purity of different Lycopene content.In general: the purity that Lycopene content height, finished product require in the starting material is low, and then the alcoholic acid usage quantity is few; Otherwise then the alcoholic acid usage quantity is many.For example: when Lycopene content is 1g/kg dry powder in raw material, extract after adopting the ethanol drip washing of 1: 10 (w/v), can obtain Lycopene content and be about 5% thick product.
The present invention also is applicable to from other are rich in the vegetable material of Lycopene and extracts Lycopene, for example: Radix Dauci Sativae etc.
The present invention compares than prior art has following typical advantages:
1. of the present invention simple to operate, be suitable for batch production production.
2. the wash-out of organic solvent of the present invention all is to carry out at normal temperatures, and process system easily seals, and is applicable to the different raw materials that is rich in Lycopene, extracts the Lycopene crude product the residue of the present invention behind catsup processing, and purity can reach 8%.No atmospheric pollution and unsafe factor.
3. the present invention uses ethanol drip washing after raw material is adorned post, can partly remove the carotenoid of soluble sugar, a small amount of protein and some pure dissolubilities etc., this method enrichment Lycopene, improved product purity.Use ethanol simultaneously, also can make extract avoid the destruction of microorganism in process of production,, yeast, mould, bacterium etc. are all had restraining effect because ethanol is a kind of solvent with antimicrobial acivity character.
4. according to product requirement, increase or minimizing alcoholic acid wash out amount, can obtain the Lycopene product of different purity, this has just simplified production process.
Below narrate embodiments of the invention:
Embodiment 1: directly extract Lyeopene with tomato dry powder:
1, material: vegetable or flower institute of the Chinese Academy of Agricultural Sciences processing tomato, after squeezing the juice,, pulverize standby then with the dry residue of normal temperature and pressure dehydrating drier.
2, equipment: packed column;
The middle constant flow pump of pressing;
Rotary Evaporators;
High performance liquid chromatography;
Ultraviolet-visible spectrophotometer.
Get 280 gram exsiccant tomato powders, the dress post; With 2500 milliliters of edible ethanol flushing pillars, flow velocity 4.5 ml/min are changed acetone kind solvent drip washing pillar afterwards, and totally 4500 milliliters, collect acetone kind solvent elutriant, use the Rotary Evaporators evaporate to dryness, obtain 13 gram Lycopene crude products, content is about 4%.
Embodiment 2: directly extract with bright tomato:
Get 5 kilograms of bright tomatoes, squeeze the juice, get residue 900 grams.Get wherein 310 grams and dispersant dress post, after 2200 milliliters of drip washing of edible ethanol, use 2160 milliliters of acetone kind solvent drip washing instead, collect acetone kind solvent elutriant and evaporate to dryness, obtain 710 milligram 11.8% Lycopene crude product.
Embodiment 3: extract with tomato skin:
Tomato skin after the tomato processing of Hubei Province five canning factories of agriculture-countryside-farmer factory is dried after washing, is ground into powder.Get 75 gram dress posts, with 410 milliliters of drip washing of edible ethanol, change 640 milliliters of acetone kind solvent drip washing more earlier, collect acetone kind solvent elutriant, concentrate, obtain purity altogether and be 857 milligrams of 12.8% Lycopene products.
Embodiment 4: extract with the residue behind the catsup processing:
Residue behind the tomato catsup processing dries, and through pulverizing, gets 245 gram dry powder dress posts.
Earlier with after 6000 milliliters of drip washing of edible ethanol, with the drip washing of acetone kind solvent, totally 1500 milliliters, collect acetone kind solvent elutriant and evaporate to dryness, obtain content and be 8% Lycopene crude product 1.2 grams.
Embodiment 5: extract with commercially available tomato-sauce:
Beijing is auspicious that tomato product company limited uses the tomato-sauce 106 of Xinjiang high-quality tomato production to restrain, even with 40 gram dispersant, behind the dress post, with 325 milliliters of edible ethanol drip washing, use 1130 milliliters of acetone kind solvent drip washing again instead, collect acetone kind solvent elutriant, concentrate, obtain purity and be 927 milligrams of 5.38% Lycopene products.
Embodiment 6: being further purified of Lycopene raw product:
Get content and be 1% Lycopene crude product 12.4 grams (including 124 milligrams of Lycopenes), with 5 times of dispersant dress posts, use edible ethanol drip washing then, flow velocity is 8 ml/min, washes out 2000 milliliters of ethanol altogether, changes the drip washing of acetone kind solvent again, and substep is collected: V
1=100 milliliters, V
2=100 milliliters, V
3=170 milliliters, the collected samples contg of sampling analysis is respectively 15.8 milligrams, 39.6 milligrams, 43.7 milligrams, and rate of loss is less than 20%, and purity is respectively 40.0%, 76.7%, 86.7%.Therefore according to different requirements, appropriate change drip washing condition can obtain the product of different purity.
Experimental example 1: Lycopene Determination on content:
1. spectrography: adopt ultraviolet-visible spectrophotometer, 550--350nm scanning, Abs (absorbancy) value≤2 is that solvent is measured with acetone.Be calculated as follows:
V: overall solution volume.
Measure collection of illustrative plates and see Fig. 1, Fig. 2.
Fig. 1 is the scanning spectra of Lycopene standard model
Fig. 2 extracts the scanning spectra of sample for Lycopene
2. chromatography:
Instrument: Tianjin, island 10Avp high performance liquid chromatograph, Rotary Evaporators.
Method: chromatographic column: Nova-pak C
18(3.9mm * 300mm); Sample size: 10ul;
Moving phase: acetonitrile: trichloromethane (92: 8);
Detect wavelength: dual wavelength is measured, 470nm (0～8 minute) and 450nm (8～13 minutes);
Flow velocity: 1.0ml/min; Column temperature: 35 ℃.
Testing used standard reagent is all produced by Sigma company
Standard diagram is seen Fig. 3.
Fig. 3 is the HPLC collection of illustrative plates of 4 kinds of carotenoid standard specimens, and wherein 1 is xenthophylls, and 2 is Lycopene, and 3 is alpha-carotene, and 4 is β-Hu Luobusu
Claims (3)
1. the extracting method of a Lycopene, the starting material that it is characterized in that in column chromatography being extracted extract Lycopene as weighting agent with ethanol and the drip washing of acetone kind solvent.
2. method according to claim 1 is characterized in that adopting earlier ethanolic soln drip washing, continues the drip washing pillar with acetone class reagent again, and is thin out until color, collects this elutriant, concentrates, and can obtain the Lycopene raw product.
3. method according to claim 1 is characterized in that the particle of upper prop raw material should be crossed 50 mesh sieves.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00129943A CN1112410C (en) | 2000-10-20 | 2000-10-20 | Method for extracting solapurpurin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00129943A CN1112410C (en) | 2000-10-20 | 2000-10-20 | Method for extracting solapurpurin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1296038A CN1296038A (en) | 2001-05-23 |
| CN1112410C true CN1112410C (en) | 2003-06-25 |
Family
ID=4593852
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN00129943A Expired - Fee Related CN1112410C (en) | 2000-10-20 | 2000-10-20 | Method for extracting solapurpurin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1112410C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1118521C (en) * | 2001-09-28 | 2003-08-20 | 新疆金企实业有限公司 | Preparation method of lycopene |
| CN105693583B (en) * | 2015-12-30 | 2018-02-09 | 晨光生物科技集团股份有限公司 | The method of composition is endangered in a kind of removal carotenoid |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1198661A (en) * | 1996-06-20 | 1998-11-11 | 利库德天然产品工业有限公司 | Industrial processing of tomatoes and lycopene extraction |
-
2000
- 2000-10-20 CN CN00129943A patent/CN1112410C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1198661A (en) * | 1996-06-20 | 1998-11-11 | 利库德天然产品工业有限公司 | Industrial processing of tomatoes and lycopene extraction |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1296038A (en) | 2001-05-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101314568B (en) | Novel method for adsorbing and separating high-purity chlorogenic acid | |
| CN106588616B (en) | A kind of preparation method of curcumin | |
| CN101260131A (en) | Method for extracting iridoid active site and monomer from eucommia bark | |
| CN110483599B (en) | Method for separating flavonoid components from sweetsop leaves | |
| CN108176079B (en) | A method for decolorizing Glycyrrhrizae radix extract | |
| CN108059628A (en) | A kind of fast preparation method of blueberry anthocyanin | |
| CN113773184B (en) | Method for extracting curcumin compounds | |
| US11981697B2 (en) | Method for preparing delphinium acylated anthocyanin | |
| CN110092772B (en) | Blueberry anthocyanin high-selectivity separation method and separation material | |
| CN109503373B (en) | Method for rapidly separating and purifying polyphenol compounds in sorbus pohuashanensis fruits | |
| CN1112410C (en) | Method for extracting solapurpurin | |
| CN107629140A (en) | A kind of method of ionic liquid double-aqueous phase system extraction Goods-Flow Plan | |
| CN112110886A (en) | Method for separating polyphenol compounds in phellinus igniarius by utilizing high-efficiency countercurrent chromatography | |
| CN1313460C (en) | Method for extracting anthocyanidin | |
| CN1226308C (en) | Wolfberry fruit polysaccharide separating and purifying technology | |
| CN112321658B (en) | Method for extracting anthocyanin in aronia melanocarpa fruit | |
| CN113173835A (en) | Method for preparing high-purity bakuchiol by high-speed counter-current chromatography separation | |
| CN1334267A (en) | Process for preparing total sanchinoside | |
| CN106518831B (en) | A kind of plant proanthocyanidin dimer, tripolymer quick separating preparation method | |
| CN1587266A (en) | Improved process for preparing podophyllotoxin from Chinese podophyllum root | |
| CN114380666B (en) | Industrial extraction method of cannabidiol | |
| CN111808066B (en) | Extraction method of schisandrin B extract | |
| CN112321655B (en) | Method for separating and preparing petunidin-3-O- (6-O-p-coumaroyl) glucoside | |
| CN114456138B (en) | Method for separating three coumarin compounds from fingered citron extract | |
| CN108329374B (en) | Method for separating high-purity tea seed saponin monomer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |