CN101987809A - Production technology for extracting purified lycopene from tomato waste residue - Google Patents
Production technology for extracting purified lycopene from tomato waste residue Download PDFInfo
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Abstract
The invention discloses production technology for extracting purified lycopene from tomato waste residue serving as a raw material, which comprises the following steps of: firstly, separating tomato skin from tomato seeds; secondly, extracting lycopene extract from the tomato skin by subcritical extraction technology; and finally, separating and purifying the lycopene in the lycopene extract by using a silica gel short column. The extraction ratio of the lycopene is 80 to 90 percent, and the lycopene content of extracted lycopene oleoresin can reach 6 to 50 percent.
Description
Technical field
The present invention relates to a kind of production technology of from the tomato waste residue, extracting the purifying Lyeopene, belong to food, healthcare products and pharmaceutical production and prepare industry.
Background technology
Lyeopene (Lycopene) has multiple important physical activity by 11 conjugation and 2 non-annularity planar conjugate polyunsaturated fat hydro carbons carotene compounds that unconjugated carbon-to-carbon double bond is formed, as quencher singlet oxygen and removing free radical; The generation of prevention coronary heart disease; Anticancer and activating immune cell effect etc.In recent years, Lyeopene is as the foodstuff additive of natural food colour, nutrient substance and the painted dual function of nutrition and be widely used in protective foods, and medicine and cosmetic industry have become the research focus of subjects such as domestic and international trophology, medical science, bromatology.Lyeopene is mainly derived from the natural product, and certain micro-organisms such as rhodobacterium also produce Lyeopene.Lyeopene is distributed widely in the various plants at nature, all contain Lyeopene as tomato, Radix Dauci Sativae, watermelon, oranges and tangerines, red natsudaidai etc., wherein content of lycopene is the highest in the tomato, Lyeopene is about 30-200mg/Kg in the fresh tomato, is about 430-2950mg/Kg in dry product.Lyeopene mainly is distributed in the water-insoluble part and skin of tomato in the tomato, accounts for the 72-92% of Lyeopene in the tomato, and wherein the content of Lyeopene is the highest in the tomato skin, and the Lyeopene that human body absorbed is mainly from tomato and goods thereof.
Lyeopene mainly is to extract gained from tomato-sauce, the patent application of extracting Lyeopene from tomato skin is also arranged, as: 200810043576.0 disclose under the neutral meta-alkalescence condition, utilize in three kinds, alkaline biological enzyme is combined with each other, allow the abundant enzymolysis of tomato peel, make Lyeopene fully dissociate out, the extraction process technology that combines in conjunction with the CO2 supercritical technology is extracted the patent application of Lyeopene in the tomato peel again; 00710150585.5 disclosing with tomato peel is raw material, adopts the technology of organic solvent extraction Lyeopene;
Lyeopene extracts the purifying patented technology have been had a variety of, mainly contain solvent-extraction process, is raw material as 02146559.2 with tomato-sauce, adopt organic solvent extractionprocess to extract Lyeopene, carry out the patent of separation and purification Lyeopene again with reverse-phase chromatography, the patent that enzyme process and saponification secondary solvent extract, the patent documentation that also useful supercritical liquid extraction technique (03146821.7), macroporous adsorbent resin and microwave-assisted extract.
But the patent industrial manufacture process technology of existing Lyeopene all has defective in various degree, and as the outward appearance and the inferior quality of lycopene oleo-resinous, the content of Lyeopene is lower in the lycopene oleo-resinous, and the production run cost is than problems such as height.
Summary of the invention
The object of the present invention is to provide a kind of production technology of from the tomato waste residue, extracting the purifying Lyeopene.
The present invention realizes by following measure:
The present invention is with the by product of tomato-sauce processing industry, promptly utilize the tomato waste residue to be raw material, separate tomato skin and seed earlier, adopt the sub critical extraction technology from tomato skin, to extract the Lyeopene extract then, adopt Lyeopene in the silica gel short column separation and purification tomato skin extract at last.
A kind of production technology of extracting the purifying Lyeopene from the tomato waste residue is characterized in that this production technology has the separation of skin seed, sub critical extraction and three steps of silica gel short column purifying:
A, skin seed separate: the tomato waste residue is added rinsing bath, add water, mechanical stirring, filter, filtrate is discarded, and filter residue adds rinsing bath again, adds water, mechanical stirring, suction filtration is removed the tomato seed that is suspended in fluid surface, and residuum filters, and filtrate is discarded, the filter residue that obtains is in dry below 50 ℃, pulverizing, the tomato skin that obtains pulverizing;
B, sub critical extraction: adopt general subcritical pressure boiler to extract equipment, the tomato skin of pulverizing is joined in the sub critical extraction still, 1-3MPa pressure in the time of 20-90 ℃, adds the sub critical extraction solvent, and mechanical stirring is extracted; Extract solvent pressurization 0.1-3MPa, change extraction-container over to, temperature is reduced to 25 ℃, resolves the degassing, changes gas over to the recovery still, and reclaim the still temperature and rise to 70-90 ℃, pressure 1-3MPa, compressed liquefied gas, stand-by; The tomato skin extract changes hold tank over to; Described extraction solvent is selected from one or both in alkane and the halogenated alkane;
C, silica gel short column purifying: with the Lyeopene extract, the organic solvent that adds 0.5-2 times of quality, mechanical stirring mixes, constant flow pump adds high 10-60cm, and diameter 10-200cm is equipped with on the short column of silica filler, the organic solvent that constant flow pump adds 10-20 times of Lyeopene extract weight carries out the short column separation, the preceding 2-4 times of weight of elutriant is first-class part, reclaims solvent, and enriched material discards; 5-10 times of weight of elutriant is second stream part, reclaims solvent and gets the Lyeopene purified product; 10-20 times of weight of elutriant is the 3rd stream part, reclaims solvent, and enriched material is discarded; Wherein organic solvent is selected from normal hexane, sherwood oil, acetone, ethyl acetate or ethanol.
The present invention is in the B step, and alkane is selected from one or both in propane, butane, third butane, cyclopropane and the oxyethane.
The present invention is in the B step, and halogenated alkane is selected from a fluoromethane, methylene fluoride, trifluoromethane, difluorochloromethane, methyl chlorofluoride, difluorobromomethane or difluorodibromomethane.
The invention has the advantages that the tomato skin that adopts in the tomato waste residue is a raw material, the extraction yield of Lyeopene is at 80-90%, and the content of Lyeopene can reach 6-50% in the lycopene oleo-resinous of extraction.
The characteristics that the present invention is different from prior art are can large-scale production, and the one-time process flow process can be handled more large batch of raw material, and industrial manufacture process is simple; technical process is short; cost is low, and organic solvent residual is low, and the outward appearance and the quality of lycopene oleo-resinous are preferable.
Embodiment
For a more clear understanding of the present invention, the present invention is further illustrated below in conjunction with embodiment, but the invention is not restricted to following examples.
Embodiment 1:
The separation of tomato skin in A, the tomato waste residue
1000kg tomato waste residue adds rinsing bath, adds 10000kg water, mechanical stirring 2h, filter, filtrate is discarded, and filter residue adds rinsing bath again, add 20000kg water, mechanical stirring 2h, suction filtration remove the tomato seed that is suspended in fluid surface, and residuum filters, filtrate is discarded, filter residue is dispersed in the forced air drying drying room, 50 ℃ of dry 8h, and pulverizer is pulverized.
Lyeopene in B, the sub critical extraction tomato skin
The tomato skin that 1000kg pulverizes adds in the sub critical extraction jar, under the 1MPa pressure, adds 3000kg third butane as extraction agent, 50 ℃ of mechanical stirring are extracted 2h, the extraction solvent is forced into the 1.2MPa filtration and squeezes into the parsing jar, and temperature is reduced to 25 ℃, and pressure is reduced to 0.6MPa, gas changes withdrawing can over to, treat that gas all shifts fully, the withdrawing can temperature rises to 90 ℃, pressure 1.2MPa, pressurized gas, stand-by; The Lyeopene extract changes hold tank over to, gets Lyeopene extract 100Kg, and productive rate is 1%, and HPLC carries out assay, and the content of Lyeopene is 1.0%.
C, silica gel short column separate the Lyeopene in the tomato skin extract
Lyeopene extract 40kg adds the 20Kg sherwood oil, and the mechanical stirring mixing is all used, constant flow pump adds high 40cm, and diameter 120cm is equipped with on the silica gel short column of 80-100 order silica gel, constant current pumps into the 400Kg sherwood oil, and 100Kg is first-class part before the elutriant, reclaims solvent, enriched material discards, elutriant second a stream part 100Kg reclaims solvent, the enriched material 5Kg that weighs, it is 7% that HPLC measures content, and the rate of transform of Lyeopene is 87.8%.All the other 200Kg sherwood oil stream parts are the 3rd stream part, reclaim solvent, and enriched material is discarded.
Embodiment 2:
The separation of tomato skin in A, the tomato waste residue
1000kg tomato waste residue adds rinsing bath, adds 15000kg water, mechanical stirring 1h, filter, filtrate is discarded, and filter residue adds rinsing bath again, add 15000kg water, mechanical stirring 2h, suction filtration remove the tomato seed, and the residuum press filtration is to doing, filtrate is discarded, filter residue is dispersed in the forced air drying drying room, 40 ℃ of dry 12h, and pulverizer is pulverized.
Lyeopene in B, the sub critical extraction tomato skin
The tomato skin that 1000kg pulverizes adds in the sub critical extraction jar, under the 1.5MPa pressure, adds the 3000kg methyl chlorofluoride, 50 ℃ of mechanical stirring are extracted 2h, the extraction solvent is forced into the 1.4MPa filtration and squeezes into the parsing jar, and temperature is reduced to 25 ℃, and pressure is reduced to 0.6MPa, gas changes withdrawing can over to, treat that gas all shifts fully, the withdrawing can temperature rises to 80 ℃, pressure 1.4MPa, pressurized gas, stand-by; The Lyeopene extract changes hold tank over to, gets Lyeopene extract 110Kg, and productive rate is 1.1%, and HPLC carries out assay, and the content of Lyeopene is 1.2%.
C, silica gel short column separate the Lyeopene in the tomato skin extract
Lyeopene extract 40kg adds the 20Kg normal hexane, and the mechanical stirring mixing is all used, constant flow pump adds high 20cm, and diameter 90cm is equipped with on the silica gel short column of 200-300 order silica gel, constant flow pump adds the 400Kg normal hexane, and 120Kg is first-class part before the elutriant, reclaims solvent, enriched material discards, a second stream part 120Kg connects in addition, reclaims solvent, the enriched material 2Kg that weighs, it is 20% that HPLC measures content, and the rate of transform of Lyeopene is 83.3%.All the other 160Kg normal hexanes are the 3rd stream part, reclaim solvent, and enriched material is discarded.
Embodiment 3:
The separation of tomato skin in A, the tomato waste residue
1000kg tomato waste residue adds rinsing bath, adds 10000kg water, mechanical stirring 3h, filter, filtrate is discarded, and filter residue adds rinsing bath again, add 20000kg water, mechanical stirring 2h, suction filtration remove the tomato seed that is suspended in fluid surface, and residuum filters, filtrate is discarded, filter residue is dispersed in the forced air drying drying room, 45 ℃ of dry 10h, and pulverizer is pulverized.
Lyeopene in B, the sub critical extraction tomato skin
The tomato skin that 1000kg pulverizes adds in the sub critical extraction jar, and under the 1.1MPa pressure, adding 3000kg third butane and methyl chlorofluoride is that the mixed gas of forming at 1: 0.1 is an extraction agent by volume, 40 ℃ of mechanical stirring are extracted 3h, the extraction solvent is forced into the 1.3MPa filtration and squeezes into the parsing jar, and temperature is reduced to 25 ℃, and pressure is reduced to 0.5MPa, gas changes withdrawing can over to, treat that gas all shifts fully, the withdrawing can temperature rises to 90 ℃, pressure 1.3MPa, pressurized gas, stand-by; The Lyeopene extract changes hold tank over to, gets Lyeopene extract 120Kg, and productive rate is 2.0%, and HPLC carries out assay, and the content of Lyeopene is 1.3%.
C, silica gel short column separate the Lyeopene in the tomato skin extract
Lyeopene extract 40kg adds the 20Kg sherwood oil, and the mechanical stirring mixing is all used, constant flow pump adds high 30cm, and diameter 100cm is equipped with on the silica gel short column of 80-100 order silica gel, constant current pumps into the 500Kg sherwood oil, and 150Kg is first-class part before the elutriant, reclaims solvent, enriched material discards, elutriant second a stream part 80Kg reclaims solvent, the enriched material 4.68Kg that weighs, it is 30% that HPLC measures content, and the rate of transform of Lyeopene is 90%.All the other 270Kg sherwood oil stream parts are the 3rd stream part, reclaim solvent, and enriched material is discarded.
Embodiment 4:
The separation of tomato skin in A, the tomato waste residue
Undertaken by A step among the embodiment 3.
Lyeopene in B, the sub critical extraction tomato skin
The tomato skin that 1000kg pulverizes adds in the sub critical extraction jar, and under the 1.2MPa pressure, adding 3000kg difluorochloromethane and difluorodibromomethane is the mixed gas of forming at 1: 1 by volume, 40 ℃ of mechanical stirring are extracted 2h, the extraction solvent is forced into the 1.3MPa filtration and squeezes into the parsing jar, and temperature is reduced to 25 ℃, and pressure is reduced to 0.7MPa, gas changes withdrawing can over to, treat that gas all shifts fully, the withdrawing can temperature rises to 90 ℃, pressure 1.3MPa, pressurized gas, stand-by; The Lyeopene extract changes hold tank over to, gets Lyeopene extract 100Kg, and productive rate is 2.0%, and HPLC carries out assay, and the content of Lyeopene is 1.4%.
C, silica gel short column separate the Lyeopene in the tomato skin extract
Undertaken by C step among the embodiment 3, the Lyeopene purified product 6.3Kg that weighs, it is 20% that HPLC measures content, the rate of transform of Lyeopene is 90%.
Embodiment 5:
The separation of tomato skin in A, the tomato waste residue
Undertaken by A step among the embodiment 3.
Lyeopene in B, the sub critical extraction tomato skin
The tomato skin that 1000kg pulverizes adds in the sub critical extraction jar, and under the 1.2MPa pressure, adding the 3000kg butane and third butane is the mixed gas of forming at 1: 10 by volume, 40 ℃ of mechanical stirring are extracted 2h, the extraction solvent is forced into the 1.3MPa filtration and squeezes into the parsing jar, and temperature is reduced to 25 ℃, and pressure is reduced to 0.7MPa, gas changes withdrawing can over to, treat that gas all shifts fully, the withdrawing can temperature rises to 90 ℃, pressure 1.3MPa, pressurized gas, stand-by; The Lyeopene extract changes hold tank over to, gets Lyeopene extract 100Kg, and productive rate is 2.0%, and HPLC carries out assay, and the content of Lyeopene is 1.4%.
C, silica gel short column separate the Lyeopene in the tomato skin extract
Undertaken by C step among the embodiment 3, the Lyeopene purified product 6.3Kg that weighs, it is 20% that HPLC measures content, the rate of transform of Lyeopene is 90%.
Embodiment 6:
The separation of tomato skin in A, the tomato waste residue
Undertaken by A step among the embodiment 3.
Lyeopene in B, the sub critical extraction tomato skin
The tomato skin that 1000kg pulverizes adds in the sub critical extraction jar, and under the 1.2MPa pressure, adding the 3000kg butane and third butane is the mixed gas of forming at 1: 0.1 by volume, 40 ℃ of mechanical stirring are extracted 2h, the extraction solvent is forced into the 1.3MPa filtration and squeezes into the parsing jar, and temperature is reduced to 25 ℃, and pressure is reduced to 0.7MPa, gas changes withdrawing can over to, treat that gas all shifts fully, the withdrawing can temperature rises to 90 ℃, pressure 1.3MPa, pressurized gas, stand-by; The Lyeopene extract changes hold tank over to, gets Lyeopene extract 100Kg, and productive rate is 2.0%, and HPLC carries out assay, and the content of Lyeopene is 1.4%.
C, silica gel short column separate the Lyeopene in the tomato skin extract
Undertaken by C step among the embodiment 3, the Lyeopene purified product 6.3Kg that weighs, it is 20% that HPLC measures content, the rate of transform of Lyeopene is 90%.
Claims (3)
1. production technology of extracting the purifying Lyeopene from the tomato waste residue is characterized in that this production technology has the separation of skin seed, sub critical extraction and three steps of silica gel short column purifying:
A, skin seed separate: the tomato waste residue is added rinsing bath, add water, mechanical stirring, filter, filtrate is discarded, and filter residue adds rinsing bath again, adds water, mechanical stirring, suction filtration is removed the tomato seed that is suspended in fluid surface, and residuum filters, and filtrate is discarded, the filter residue that obtains is in dry below 50 ℃, pulverizing, the tomato skin that obtains pulverizing;
B, sub critical extraction: adopt general subcritical pressure boiler to extract equipment, the tomato skin of pulverizing is joined in the sub critical extraction still, 1-3MPa pressure in the time of 20-90 ℃, adds the sub critical extraction solvent, and mechanical stirring is extracted; Extract solvent pressurization 0.1-3MPa, change extraction-container over to, temperature is reduced to 25 ℃, resolves the degassing, changes gas over to the recovery still, and reclaim the still temperature and rise to 70-90 ℃, pressure 1-3MPa, compressed liquefied gas, stand-by; The tomato skin extract changes hold tank over to; Described extraction solvent is selected from one or both in alkane and the halogenated alkane;
C, silica gel short column purifying: with the Lyeopene extract, the organic solvent that adds 0.5-2 times of quality, mechanical stirring mixes, constant flow pump adds high 10-60cm, and diameter 10-200cm is equipped with on the short column of silica filler, the organic solvent that constant flow pump adds 10-20 times of Lyeopene extract weight carries out the short column separation, the preceding 2-4 times of weight of elutriant is first-class part, reclaims solvent, and enriched material discards; 5-10 times of weight of elutriant is second stream part, reclaims solvent and gets the Lyeopene purified product; 10-20 times of weight of elutriant is the 3rd stream part, reclaims solvent, and enriched material is discarded; Wherein organic solvent is selected from normal hexane, sherwood oil, acetone, ethyl acetate or ethanol.
2. the method for claim 1, it is characterized in that: in the B step, alkane is selected from one or both in propane, butane, third butane, cyclopropane and the oxyethane.
3. the method for claim 1, it is characterized in that: in the B step, halogenated alkane is selected from a fluoromethane, methylene fluoride, trifluoromethane, difluorochloromethane, methyl chlorofluoride, difluorobromomethane or difluorodibromomethane.
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Cited By (10)
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| CN102526334A (en) * | 2011-12-09 | 2012-07-04 | 新疆晨曦椒业有限公司 | Industrial method for producing tomato red by using tomato peel residues |
| CN105038309A (en) * | 2015-08-11 | 2015-11-11 | 哈尔滨市工艺美术有限责任公司 | Dark red corn straw dye and production method thereof |
| CN105368573A (en) * | 2015-11-24 | 2016-03-02 | 郑州雪麦龙食品香料有限公司 | Method for preparing nutmeg oleoresin by using subcritical fluid |
| CN105400596A (en) * | 2015-11-24 | 2016-03-16 | 郑州雪麦龙食品香料有限公司 | Method for extracting green prickleyash oleoresin through subcritical dimethyl ether fluid |
| CN105462287A (en) * | 2016-01-26 | 2016-04-06 | 青岛百草纤维科技股份有限公司 | Method for extracting lavender dye and application of method to regenerated cellulose fiber dyeing |
| CN105566048A (en) * | 2014-10-17 | 2016-05-11 | 中粮营养健康研究院有限公司 | Method for extracting tomato skin residues by adopting subcritical fluid |
| CN107056574A (en) * | 2017-02-03 | 2017-08-18 | 深圳市江牧实业有限公司 | A kind of method for extracting lycopene |
| CN110256189A (en) * | 2019-07-19 | 2019-09-20 | 长沙卫一生物科技有限公司 | The technique of lycopene is extracted from tomato peel |
| CN110396305A (en) * | 2019-09-04 | 2019-11-01 | 淮南宜生生物科技有限公司 | A kind of extracting method of capsicum red pigment |
| CN113045377A (en) * | 2021-04-30 | 2021-06-29 | 中国药科大学 | Preparation method of lycopene particles based on combined process of subcritical extraction and supercritical granulation |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102526334A (en) * | 2011-12-09 | 2012-07-04 | 新疆晨曦椒业有限公司 | Industrial method for producing tomato red by using tomato peel residues |
| CN102526334B (en) * | 2011-12-09 | 2014-04-02 | 新疆晨曦椒业有限公司 | Industrial method for producing tomato red by using tomato peel residues |
| CN105566048B (en) * | 2014-10-17 | 2018-11-09 | 中粮营养健康研究院有限公司 | A method of tomato peel is extracted using subcritical fluids |
| CN105566048A (en) * | 2014-10-17 | 2016-05-11 | 中粮营养健康研究院有限公司 | Method for extracting tomato skin residues by adopting subcritical fluid |
| CN105038309A (en) * | 2015-08-11 | 2015-11-11 | 哈尔滨市工艺美术有限责任公司 | Dark red corn straw dye and production method thereof |
| CN105368573A (en) * | 2015-11-24 | 2016-03-02 | 郑州雪麦龙食品香料有限公司 | Method for preparing nutmeg oleoresin by using subcritical fluid |
| CN105400596A (en) * | 2015-11-24 | 2016-03-16 | 郑州雪麦龙食品香料有限公司 | Method for extracting green prickleyash oleoresin through subcritical dimethyl ether fluid |
| CN105462287B (en) * | 2016-01-26 | 2017-08-25 | 青岛百草新材料股份有限公司 | A kind of extracting method of lavender dyestuff and its application in regenerated celulose fibre dyeing |
| CN105462287A (en) * | 2016-01-26 | 2016-04-06 | 青岛百草纤维科技股份有限公司 | Method for extracting lavender dye and application of method to regenerated cellulose fiber dyeing |
| CN107056574A (en) * | 2017-02-03 | 2017-08-18 | 深圳市江牧实业有限公司 | A kind of method for extracting lycopene |
| CN110256189A (en) * | 2019-07-19 | 2019-09-20 | 长沙卫一生物科技有限公司 | The technique of lycopene is extracted from tomato peel |
| CN110256189B (en) * | 2019-07-19 | 2022-02-08 | 长沙卫一生物科技有限公司 | Process for extracting lycopene from tomato peel residue |
| CN110396305A (en) * | 2019-09-04 | 2019-11-01 | 淮南宜生生物科技有限公司 | A kind of extracting method of capsicum red pigment |
| CN110396305B (en) * | 2019-09-04 | 2021-04-20 | 淮南宜生生物科技有限公司 | Extraction method of capsanthin |
| CN113045377A (en) * | 2021-04-30 | 2021-06-29 | 中国药科大学 | Preparation method of lycopene particles based on combined process of subcritical extraction and supercritical granulation |
| CN113045377B (en) * | 2021-04-30 | 2023-02-28 | 中国药科大学 | Preparation method of lycopene particles based on combined process of subcritical extraction and supercritical granulation |
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Application publication date: 20110323 |