CN102698466A - Method for removing pesticide residues in natural extract - Google Patents
Method for removing pesticide residues in natural extract Download PDFInfo
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- CN102698466A CN102698466A CN2012101939357A CN201210193935A CN102698466A CN 102698466 A CN102698466 A CN 102698466A CN 2012101939357 A CN2012101939357 A CN 2012101939357A CN 201210193935 A CN201210193935 A CN 201210193935A CN 102698466 A CN102698466 A CN 102698466A
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Abstract
The invention discloses a method for removing pesticide residues in a natural extract. The method comprises the following steps of adding a liquid natural extract containing the pesticide residues or a liquid natural extract mixed with edible oil into an extraction kettle; causing irregular random metal packing to be arranged in the extraction kettle; and extracting the pesticide residues in the liquid natural extract with a static and dynamic combined supercritical CO2 fluid extraction method, and then resolving a CO2 solvent to finally obtain the natural extract without the pesticide residues. According to the method, any organic solvent and toxic and harmful substances are not used as a remover. The method has the characteristics that the removing process is safe, and no secondary pollution exists. According to the method, the irregular random metal packing is added, so that the removing effect of the pesticide residues is effectively increased, and the phenomena of bias current, channeling and the like are avoided. The method has the characteristics of higher removal rate, simple and easy process and low production cost and is particularly suitable for removing organophosphorus, carbamates and pyrethroid pesticide residues in partial-fat soluble natural extracts.
Description
Technical field
The present invention relates to a kind of method of purification of natural extract, especially a kind of method of removing residues of pesticides in the natural extract.
Background technology
Current uphold nature, the back to nature irresistible historical trend that become international; Improving constantly of Along with people's living standard; People more and more is not grudged for safety, for health and being spent; Do not contain the residues of pesticides product and more and more looked at by the parent of people institute, countries in the world, particularly developed country pay much attention to the residues of pesticides problem, and residues of pesticides in the various agricultural byproducts have all been stipulated more and more stricter limit standard.Many countries all are technology barriers with the Pesticide Residue, the import of restriction agricultural byproducts, protection agricultural production.So production does not contain residues of pesticides or residues of pesticides product up to standard is earned foreign exchange all significant for people's healthy, increase products export.
According to domestic and international publication report; Residues of pesticides removal method is more; And utilize supercritical extraction technique to remove residues of pesticides are a kind of more recent technology: 1, a kind of method (publication number CN101156881A) that removes residues of pesticides in the genseng mainly is to utilize propane to do solvent residues of pesticides among the solid ginseng pulverate are removed; Propane critical-temperature Jiao Gao ﹝ 97 ℃ ﹞ are not easy to reach in this method, and propane is inflammable and explosive, cause its use dangerous.2, the removal methods of remains of pesticide (publication number CN101810658A) in a kind of genseng mainly is to utilize 1,1; 1,2-tetrafluoro hexane is done solvent to residues of pesticides among the solid ginseng pulverate being removed 1 in this method; 1; 1,2-tetrafluoro hexane has bigger harm to atmospheric environment, has unsafe deficiency of use.3, from tealeaves, extracting the method (publication number CN1837201A) of Tea Polyphenols, theanine, tea polysaccharide, Tea Pigment, mainly is to utilize CO
2Do solvent the middle mutually caffeine of ethyl acetate, residues of pesticides and dissolvent residual are removed, its raw material is the big water-soluble products partially of polarity; At present also not about supercritical CO
2Remove residues of pesticides system process report in the fat-soluble partially natural extract.
Summary of the invention
The technical problem that the present invention will solve provide a kind of safe, remove the method for residues of pesticides in the natural extract effectively.
For solving the problems of the technologies described above, the technical scheme that the present invention taked is: will contain the liquid natural extract of residues of pesticides, or the liquid natural extract that mixes with edible oil joins in the extraction kettle; Be provided with irregular diffusing heap metal packing in the described extraction kettle; Adopt quiet dynamic combination supercritical CO then
2The fluid extraction method extracts the residues of pesticides in the liquid natural extract, resolves CO then
2Solvent can obtain removing the natural extract of residues of pesticides.
The weight ratio of edible oil according to the invention and liquid natural extract is 0～1:1; Described edible oil is salad oil, sunflower oil, rapeseed oil or peanut oil.
Irregular diffusing heap metal packing of the present invention is the rectangular saddle ring filler, and amount of filler is 1/2～2/3 of an extraction kettle volume; The material of said irregular diffusing heap metal packing is a stainless steel.
Static extracting pressure according to the invention is 10～15MPa, and the extraction time is 20～30min; Said dynamic extraction pressure is 20～35MPa, and the extraction time is 2～10h; The extraction temperature of quiet dynamic extraction is 40～75 ℃.
The secondary that resolves to of the present invention is resolved: it is 7.5～10MPa that one-level is resolved pressure, and it is 4～6MPa that secondary is resolved pressure, and resolution temperature is 30～50 ℃.
Gaseous state CO after the parsing according to the invention
2After adsorbents adsorb, be used for extraction once more; Described adsorbent is active carbon, discolour silica gel or aluminium oxide.
Natural extract of the present invention is fat-soluble partially natural extract, described residues of pesticides be organic phosphates, carbamates and pyrethroid pesticide remained in one or more.
Adopt the beneficial effect that technique scheme produced to be: the present invention does not use any organic solvent and poisonous and harmful substance to do remover in the process of removing residues of pesticides, so the present invention has the characteristics of removal process safety, non-secondary pollution.It is residual and in extraction process, come together and remove the residual effect of farming with the grease constituents that dilution farming is played in the adding of edible oil of the present invention; The adding of irregular diffusing heap metal packing can be played the effect of balanced air-flow, strengthens the contact area of material and supercritical fluid, thereby improves the residues of pesticides removal effect effectively, avoid producing phenomenons such as bias current or channel; The employing of static extracting mainly is that supercritical fluid is fully contacted with the material middle peasant is residual, is convenient to fully extract when dynamic that to remove farming residual.The present invention utilizes supercritical CO
2Fluid extraction method and irregular diffusing heap metal packing; Make it to have the advantages that clearance is higher, simple for process, production cost is low, be particularly useful for organic phosphates, carbamates and pyrethroid pesticide remained removal in the fat-soluble partially natural extract.
Gaseous state CO after the present invention will resolve
2With utilizing again again after the adsorbents adsorb, avoided not resolving the influence of residues of pesticides to extracting completely, thereby can effectively improve extraction yield.
The specific embodiment
Below in conjunction with specific embodiment the present invention is done further detailed explanation.
Embodiment 1: residues of pesticides are example to the method for residues of pesticides in the capsicum red pigment to remove in this removal natural extract, and concrete processing step is described below.
At supercritical CO
2Put into the metal packing of the diffusing heap of rectangular saddle ring stainless steel in the extraction kettle (Guangzhou high-new Separation Technologies, Inc. in U.S. morning produces the overcritical device of 300L*2), addition is 1/2 of an extraction kettle volume.Get the 100kg capsicum red pigment and add 30kg rapeseed oil (10:3), squeeze in the extraction kettle; Adopt static earlier, dynamic quiet dynamic combination supercritical CO again
2The extraction of boosting of fluid extraction method, static extracting pressure is 12MPa, the time is 25min; Dynamic extraction pressure is 25MPa, extracts 50 ℃ of extraction temperature, CO 5.0 hours
2Flow is 1250L/h.CO after the extraction
2Solvent is resolved, and it is that 10MPa, one-level resolution temperature are 40 ℃ that one-level is resolved pressure, and it is 5MPa that secondary is resolved pressure, and the secondary resolution temperature is 35 ℃.Gaseous state CO after the parsing
2In absorber,, remain in gaseous state CO fully to remove not resolve with active carbon and discolour silica gel absorption
2In residues of pesticides, through absorption after gaseous state CO
2Be used for supercritical CO once more
2Fluid extraction.
Through to Rogor, carbendazim, metrifonate, phoxim, Permanone, flucythrinate in raw material and the product, kill residues of pesticides content such as chrysanthemum ester, chlopyrifos and measure; Rogor clearance 97.8%, carbendazim clearance 91.7%, metrifonate clearance 95.8%; Phoxim clearance 88.7%; Permanone clearance 98.5%, flucythrinate clearance 90.1% is killed chrysanthemum ester clearance 92.1%; Chlopyrifos clearance 93.1% all reaches ideal pesticide residue removal effect.
Embodiment 2: residues of pesticides are example to the method for residues of pesticides in the safflower seed oil to remove in this removal natural extract, and concrete processing step is described below.
At supercritical CO
2Put into the metal packing of the diffusing heap of rectangular saddle ring stainless steel in the extraction kettle (Guangzhou high-new Separation Technologies, Inc. in U.S. morning produces the overcritical device of 300L*2), addition is 2/3 of an extraction kettle volume.Get the 120kg safflower seed oil and add 10kg salad oil (12:1), squeeze in the extraction kettle; Adopt supercritical CO
2The fluid extraction of boosting, static extracting pressure is 10MPa, and the time is 30min, and dynamic extraction pressure is 30MPa, extracts 65 ℃ of extraction temperature, CO 8.0 hours
2Flow is 1350L/h.CO after the extraction
2Solvent is resolved, and it is that 9MPa, one-level resolution temperature are 45 ℃ that one-level is resolved pressure, and it is 5.5MPa that secondary is resolved pressure, and the secondary resolution temperature is 35 ℃.Gaseous state CO after the parsing
2In absorber,, remain in gaseous state CO fully to remove not resolve with active carbon and discolour silica gel absorption
2In residues of pesticides, through absorption after gaseous state CO
2Be used for supercritical CO once more
2Fluid extraction.
Through residues of pesticides content such as Rogor, carbendazim, phoxim, Aphox, Hostathion, Azodrin, cypermethrin in raw material and the product are measured Rogor clearance 97.8%, carbendazim clearance 91.7%; Phoxim clearance 95.8%; Aphox clearance 98.5%, Hostathion clearance 90.1%, Azodrin clearance 92.1%; Cypermethrin clearance 93.1%, the residues of pesticides removal effect is remarkable.
Embodiment 3: residues of pesticides are example to the method for residues of pesticides in the tomato red oleoresin to remove in this removal natural extract, and concrete processing step is described below.
At supercritical CO
2Put into the metal packing of the diffusing heap of rectangular saddle ring stainless steel in the extraction kettle (Guangzhou high-new Separation Technologies, Inc. in U.S. morning produces the overcritical device of 300L*2), addition is 3/5 of an extraction kettle volume.Get 95kg tomato red oleoresin and add 35kg peanut oil (19:7), squeeze in the extraction kettle; Adopt supercritical CO
2The fluid extraction of boosting, static extracting pressure is 15MPa, and the time is 20min, and dynamic extraction pressure is 27MPa, extracts 55 ℃ of extraction temperature, CO 5.5 hours
2Flow is 1410L/h.CO after the extraction
2Solvent is resolved, and it is that 8MPa, one-level resolution temperature are 45 ℃ that one-level is resolved pressure, and it is 6MPa that secondary is resolved pressure, and the secondary resolution temperature is 35 ℃.Gaseous state CO after the parsing
2In absorber,, remain in gaseous state CO fully to remove not resolve with active carbon and alumina adsorption
2In residues of pesticides, through absorption after gaseous state CO
2Be used for supercritical CO once more
2Fluid extraction.
Through residues of pesticides content such as carbendazim, Ethodan, cypermethrin, fenvalerate, phoxim, Rogor, malathion in raw material and the product are measured carbendazim clearance 97.1%, Ethodan clearance 92.3%; Cypermethrin clearance 90.7%; Fenvalerate clearance 95.4%, phoxim clearance 87.5%, Rogor clearance 92.1%; Malathion clearance 96.8% all reaches ideal pesticide residue removal effect.
Embodiment 4: residues of pesticides are example to the method for residues of pesticides in the lutein oleoresin to remove in this removal natural extract, and concrete processing step is described below.
At supercritical CO
2Put into the metal packing of the diffusing heap of rectangular saddle ring stainless steel in the extraction kettle (Guangzhou high-new Separation Technologies, Inc. in U.S. morning produces the overcritical device of 300L*2), addition is 1/2 of an extraction kettle volume.Get the 65kg lutein oleoresin and add 65kg sunflower oil (1:1), squeeze in the extraction kettle; Adopt supercritical CO
2The fluid extraction of boosting, static extracting pressure is 13MPa, and the time is 25min, and dynamic extraction pressure is 35MPa, extracts 75 ℃ of extraction temperature, CO 10.0 hours
2Flow is 1310L/h.CO after the extraction
2Solvent is resolved, and it is that 8.5MPa, one-level resolution temperature are 50 ℃ that one-level is resolved pressure, and it is 6MPa that secondary is resolved pressure, and the secondary resolution temperature is 50 ℃.Gaseous state CO after the parsing
2In absorber,, remain in gaseous state CO fully to remove not resolve with active carbon and alumina adsorption
2In residues of pesticides, through absorption after gaseous state CO
2Be used for supercritical CO once more
2Fluid extraction.
Through to Rogor, carbendazim, metrifonate, phoxim, Permanone, flucythrinate in raw material and the product, kill residues of pesticides content such as chrysanthemum ester, chlopyrifos and measure; Rogor clearance 97.6%, carbendazim clearance 91.8%, metrifonate clearance 95.8%; Phoxim clearance 88.8%; Permanone clearance 98.2%, flucythrinate clearance 89.7% is killed chrysanthemum ester clearance 92.0%; Chlopyrifos clearance 92.9% all reaches ideal pesticide residue removal effect.
Embodiment 5: residues of pesticides are example to the method for residues of pesticides in the linseed oil to remove in this removal natural extract, and concrete processing step is described below.
At supercritical CO
2Put into the metal packing of the diffusing heap of rectangular saddle ring stainless steel in the extraction kettle (Guangzhou high-new Separation Technologies, Inc. in U.S. morning produces the overcritical device of 300L*2), addition is 1/2 of an extraction kettle volume.Get 130kg linseed oil (not adding edible oil), squeeze in the extraction kettle; Adopt supercritical CO
2The fluid extraction of boosting, static extracting pressure is 14MPa, and the time is 20min, and dynamic extraction pressure is 20MPa, extracts 40 ℃ of extraction temperature, CO 2.0 hours
2Flow is 1450L/h.CO after the extraction
2Solvent is resolved, and it is that 7.5MPa, one-level resolution temperature are 30 ℃ that one-level is resolved pressure, and it is 4MPa that secondary is resolved pressure, and the secondary resolution temperature is 30 ℃.Gaseous state CO after the parsing
2In absorber,, remain in gaseous state CO fully to remove not resolve with active carbon and alumina adsorption
2In residues of pesticides, through absorption after gaseous state CO
2Be used for supercritical CO once more
2Fluid extraction.
Through residues of pesticides content such as Rogor, carbendazim, phoxim, Aphox, Hostathion, Azodrin, cypermethrin in raw material and the product are measured Rogor clearance 97.8%, carbendazim clearance 92.0%; Phoxim clearance 95.7%; Aphox clearance 98.1%, Hostathion clearance 90.7%, Azodrin clearance 92.0%; Cypermethrin clearance 92.6%, the residues of pesticides removal effect is remarkable.
Claims (10)
1. a method of removing residues of pesticides in the natural extract is characterized in that, this method step is: will contain the liquid natural extract of residues of pesticides, or the liquid natural extract that mixes with edible oil joins in the extraction kettle; Be provided with irregular diffusing heap metal packing in the described extraction kettle; Adopt quiet dynamic combination supercritical CO then
2The fluid extraction method extracts the residues of pesticides in the liquid natural extract, resolves CO then
2Solvent can obtain removing the natural extract of residues of pesticides.
2. the method for residues of pesticides in the removal natural extract according to claim 1 is characterized in that: the weight ratio of said edible oil and liquid natural extract is 0～1:1.
3. the method for residues of pesticides in the removal natural extract according to claim 1 is characterized in that: described edible oil is salad oil, sunflower oil, rapeseed oil or peanut oil.
4. the method for residues of pesticides in the removal natural extract according to claim 1 is characterized in that: described irregular diffusing heap metal packing is the rectangular saddle ring filler, and amount of filler is 1/2～2/3 of an extraction kettle volume.
5. the method for residues of pesticides in the removal natural extract according to claim 4 is characterized in that: the material of said irregular diffusing heap metal packing is a stainless steel.
6. the method for residues of pesticides in the removal natural extract according to claim 1 is characterized in that: said static extracting pressure is 10～15MPa, and the extraction time is 20～30min; Said dynamic extraction pressure is 20～35MPa, and the extraction time is 2～10h; The extraction temperature of quiet dynamic extraction is 40～75 ℃.
7. the method for residues of pesticides is characterized in that in the removal natural extract according to claim 1, and the described secondary that resolves to is resolved: it is 7.5～10MPa that one-level is resolved pressure, and it is 4～6MPa that secondary is resolved pressure, and resolution temperature is 30～50 ℃.
8. remove the method for residues of pesticides in the natural extract according to described any one of claim 1-7, it is characterized in that: the gaseous state CO after the said parsing
2After adsorbents adsorb, be used for extraction once more.
9. according to claim 8 any one removed the method for residues of pesticides in the natural extract, and it is characterized in that: described adsorbent is active carbon, discolour silica gel or aluminium oxide.
10. remove the method for residues of pesticides in the natural extract according to described any one of claim 1-7; It is characterized in that: described natural extract is fat-soluble partially natural extract, described residues of pesticides be organic phosphates, carbamates and pyrethroid pesticide remained in one or more.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103005005A (en) * | 2013-01-16 | 2013-04-03 | 福建仙芝楼生物科技有限公司 | Device and method for removing pesticide residue from plant by supercritical carbon dioxide |
| CN103305343A (en) * | 2013-06-07 | 2013-09-18 | 佰香汇生物科技（厦门）有限公司 | Method for removing pesticide residue in citrus essential oil |
| CN105777699A (en) * | 2016-05-19 | 2016-07-20 | 湖北紫鑫生物科技有限公司 | Preparation method of black rice anthocyanin without pesticide residue |
| CN105838254A (en) * | 2016-03-17 | 2016-08-10 | 晨光生物科技集团股份有限公司 | Method for removing pesticide residues in capsicum oleoresin through molecular distillation |
| CN106689980A (en) * | 2016-11-30 | 2017-05-24 | 西北大学 | Method for removing pesticide and antibiotic residues from honey |
| CN107445924A (en) * | 2017-07-31 | 2017-12-08 | 梅跃进 | A kind of method of subcritical abstraction pyrethrins |
| CN110813205A (en) * | 2019-08-01 | 2020-02-21 | 铜仁学院 | Mode for removing pesticide residues in natural product extract |
| CN111743932A (en) * | 2020-08-12 | 2020-10-09 | 陕西瑞沃生物科技有限公司 | Process for removing pesticide residue in ginseng plant extract |
| CN112544942A (en) * | 2020-11-23 | 2021-03-26 | 南通奥凯生物技术开发有限公司 | Method for preparing special powdered essence for pickled vegetables by deep processing and purification of natural extract |
| CN113698987A (en) * | 2021-08-30 | 2021-11-26 | 山东三星玉米产业科技有限公司 | Method for removing residual pesticide in corn oil |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103005005A (en) * | 2013-01-16 | 2013-04-03 | 福建仙芝楼生物科技有限公司 | Device and method for removing pesticide residue from plant by supercritical carbon dioxide |
| CN103305343A (en) * | 2013-06-07 | 2013-09-18 | 佰香汇生物科技（厦门）有限公司 | Method for removing pesticide residue in citrus essential oil |
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| CN106689980A (en) * | 2016-11-30 | 2017-05-24 | 西北大学 | Method for removing pesticide and antibiotic residues from honey |
| CN107445924A (en) * | 2017-07-31 | 2017-12-08 | 梅跃进 | A kind of method of subcritical abstraction pyrethrins |
| CN107445924B (en) * | 2017-07-31 | 2020-05-08 | 梅跃进 | Subcritical pyrethrin extraction method |
| CN110813205A (en) * | 2019-08-01 | 2020-02-21 | 铜仁学院 | Mode for removing pesticide residues in natural product extract |
| CN111743932A (en) * | 2020-08-12 | 2020-10-09 | 陕西瑞沃生物科技有限公司 | Process for removing pesticide residue in ginseng plant extract |
| CN112544942A (en) * | 2020-11-23 | 2021-03-26 | 南通奥凯生物技术开发有限公司 | Method for preparing special powdered essence for pickled vegetables by deep processing and purification of natural extract |
| CN113698987A (en) * | 2021-08-30 | 2021-11-26 | 山东三星玉米产业科技有限公司 | Method for removing residual pesticide in corn oil |
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Application publication date: 20121003 Assignee: Xinjiang Chenxi Pepper Industry Co.,Ltd. Assignor: Chengguang Natural Pigment Group Co., Ltd. Contract record no.: 2019990000135 Denomination of invention: Method for removing pesticide residues in natural extract Granted publication date: 20151125 License type: Common License Record date: 20190430 |