CN102698466B - Remove the method for natural extract Pesticide Residues - Google Patents
Remove the method for natural extract Pesticide Residues Download PDFInfo
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Abstract
The invention discloses a kind of method removing natural extract Pesticide Residues, the steps include: the liquid natural extract containing residues of pesticides, or the liquid natural extract mixed with edible oil joins in extraction kettle; Irregular loose heap metal packing is provided with in described extraction kettle; Then quiet dynamic bind supercritical CO is adopted
2fluids extraction extracts the residues of pesticides in liquid natural extract, then resolves CO
2solvent, can obtain the natural extract removing residues of pesticides.This method does not use any organic solvent and poisonous and harmful substance to do remover, has the advantages that to remove process safety, non-secondary pollution.This method by adding irregular loose heap metal packing, thus effectively improving residues of pesticides removal effect, avoiding producing the phenomenon such as bias current or channel; Have the advantages that clearance is higher, simple for process, production cost is low, be particularly useful for the organic phosphates in partially fat-soluble natural extract, carbamates and pyrethroid pesticide remained removal.
Description
Technical field
The present invention relates to a kind of method of purification of natural extract, especially a kind of method removing natural extract Pesticide Residues.
Background technology
Current uphold nature, back to nature have become international irresistible historical trend, along with improving constantly of people's living standard, people more and more do not grudge and spending for safety, for health, more and more do not looked at by people institute parent containing residues of pesticides product, countries in the world, particularly developed country are paid much attention to Pesticide Residue, all define more and more stricter limit standard to various agricultural byproducts Pesticide Residues.Many countries are all technology barriers with Pesticide Residue, and the import of restriction agricultural byproducts, protecting agriculture is produced.Therefore produce not containing residues of pesticides or residues of pesticides product up to standard for people healthy, increase products export and earn foreign exchange all significant.
Report according to domestic and international publication, residues of pesticides minimizing technology is more, and to utilize supercritical extraction technique to remove residues of pesticides are a kind of more recent technology: a kind of 1, method (publication number CN101156881A) removing ginseng Pesticide Residues, mainly utilizes propane to do solvent to solid ginseng pulverate Pesticide Residues and remove; In the method, propane critical-temperature compare Gao ﹝ 97 DEG C ﹞ is not easy to reach, and propane is inflammable and explosive, causes its use dangerous.2, a kind of removal methods (publication number CN101810658A) of residual pesticide from ginseng, mainly utilize 1,1,1,2-tetrafluoro hexane does solvent and removes to solid ginseng pulverate Pesticide Residues, 1 in the method, 1,1,2-tetrafluoro hexane has larger harm to atmospheric environment, has and uses unsafe deficiency.3, from tealeaves, extract the method (publication number CN1837201A) of Tea Polyphenols, theanine, tea polysaccharide, Tea Pigment, mainly utilize CO
2do solvent to ethyl acetate mutually in caffeine, residues of pesticides and dissolvent residual remove, its raw material is the comparatively large water-soluble products partially of polarity; At present also not about supercritical CO
2remove partially fat-soluble natural extract Pesticide Residues system process report.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method that is safe, removal natural extract Pesticide Residues effectively.
For solving the problems of the technologies described above, the technical solution used in the present invention is: by the liquid natural extract containing residues of pesticides, or the liquid natural extract mixed with edible oil joins in extraction kettle; Irregular loose heap metal packing is provided with in described extraction kettle; Then quiet dynamic bind supercritical CO is adopted
2fluids extraction extracts the residues of pesticides in liquid natural extract, then resolves CO
2solvent, can obtain the natural extract removing residues of pesticides.
The weight ratio of edible oil of the present invention and liquid natural extract is 0 ~ 1:1; Described edible oil is salad oil, sunflower oil, rapeseed oil or peanut oil.
Irregular loose heap metal packing of the present invention is Intalox metal tower packing, and amount of filler is 1/2 ~ 2/3 of extraction kettle volume; The material of described irregular loose heap metal packing is stainless steel.
Static extracting pressure of the present invention is 10 ~ 15MPa, and extraction time is 20 ~ 30min; Described dynamic extraction pressure is 20 ~ 35MPa, and extraction time is 2 ~ 10h; The extraction temperature of quiet dynamic extraction is 40 ~ 75 DEG C.
The secondary that resolves to of the present invention is resolved: it is 7.5 ~ 10MPa that one-level resolves pressure, and it is 4 ~ 6MPa that secondary resolves pressure, and resolution temperature is 30 ~ 50 DEG C.
Gaseous state CO after parsing of the present invention
2after adsorbent, again for extraction; Described adsorbent is active carbon, discolour silica gel or aluminium oxide.
Natural extract of the present invention is partially fat-soluble natural extract, described residues of pesticides be organic phosphates, carbamates and pyrethroid pesticide remained in one or more.
The beneficial effect adopting technique scheme to produce is: the present invention does not use any organic solvent and poisonous and harmful substance to do remover in the process removing residues of pesticides, and therefore the present invention has the advantages that to remove process safety, non-secondary pollution.Play the adding of edible oil of the present invention dilution agriculture residual and extract and remove the residual effect of agriculture with grease constituents in extraction process; Irregular loose heap metal packing add the effect playing balanced air-flow, strengthen the contact area of material and supercritical fluid, thus effectively improve residues of pesticides removal effect, avoid phenomenon such as generation bias current or channel etc.; The employing of static extracting mainly makes supercritical fluid fully contact with material middle peasant is residual, fully extracts removal agriculture residual when being convenient to dynamic.The present invention utilizes supercritical CO
2fluids extraction and irregular loose heap metal packing, make it to have the advantages that clearance is higher, simple for process, production cost is low, be particularly useful for the organic phosphates in partially fat-soluble natural extract, carbamates and pyrethroid pesticide remained removal.
The present invention is by the gaseous state CO after parsing
2re-use again with after adsorbent, avoid and do not resolve the impact on extraction of residues of pesticides completely, thus effectively can improve extraction yield.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further detailed explanation.
Embodiment 1: the method for this removal natural extract Pesticide Residues is to remove capsicum red pigment Pesticide Residues, and concrete technology step is as described below.
At supercritical CO
2put into the metal packing of rectangular saddle ring stainless steel loose heap in extraction kettle (Guangzhou Mei Chen high and new separation technology company produces the overcritical device of 300L*2), addition is 1/2 of extraction kettle volume.Get 100kg capsicum red pigment and add 30kg rapeseed oil (10:3), squeeze in extraction kettle; Adopt first static state, more dynamic quiet dynamic bind supercritical CO
2fluids extraction carries out boosting extraction, and static extracting pressure is 12MPa, and the time is 25min; Dynamic extraction pressure is 25MPa, extracts 5.0 hours, extraction temperature 50 DEG C, CO
2flow is 1250L/h.CO after extraction
2solvent is resolved, and one-level parsing pressure is 10MPa, one-level resolution temperature is 40 DEG C, and it is 5MPa that secondary resolves pressure, and secondary resolution temperature is 35 DEG C.Gaseous state CO after parsing
2with active carbon and discolour silica gel absorption in absorber, remain in gaseous state CO completely to remove not resolve
2in residues of pesticides, through absorption after gaseous state CO
2again for supercritical CO
2fluid extraction.
By measuring residues of pesticides content such as Rogor, carbendazim, metrifonate, phoxim, Permanone, flucythrinate, killing logvalue, chlopyrifos in raw material and product, Rogor clearance 97.8%, carbendazim clearance 91.7%, metrifonate clearance 95.8%, phoxim clearance 88.7%, Permanone clearance 98.5%, flucythrinate clearance 90.1%, killing logvalue clearance 92.1%, chlopyrifos clearance 93.1%, all reaches desirable residues of pesticides removal effect.
Embodiment 2: the method for this removal natural extract Pesticide Residues is to remove safflower seed oil Pesticide Residues, and concrete technology step is as described below.
At supercritical CO
2put into the metal packing of rectangular saddle ring stainless steel loose heap in extraction kettle (Guangzhou Mei Chen high and new separation technology company produces the overcritical device of 300L*2), addition is 2/3 of extraction kettle volume.Get 120kg safflower seed oil and add 10kg salad oil (12:1), squeeze in extraction kettle; Adopt supercritical CO
2fluid carries out boosting extraction, and static extracting pressure is 10MPa, and the time is 30min, and dynamic extraction pressure is 30MPa, extracts 8.0 hours, extraction temperature 65 DEG C, CO
2flow is 1350L/h.CO after extraction
2solvent is resolved, and one-level parsing pressure is 9MPa, one-level resolution temperature is 45 DEG C, and it is 5.5MPa that secondary resolves pressure, and secondary resolution temperature is 35 DEG C.Gaseous state CO after parsing
2with active carbon and discolour silica gel absorption in absorber, remain in gaseous state CO completely to remove not resolve
2in residues of pesticides, through absorption after gaseous state CO
2again for supercritical CO
2fluid extraction.
By measuring residues of pesticides content such as Rogor, carbendazim, phoxim, Aphox, Hostathion, Azodrin, cypermethrins in raw material and product, 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%, residues of pesticides removal effect is remarkable.
Embodiment 3: the method for this removal natural extract Pesticide Residues is to remove tomato red oleoresin Pesticide Residues, and concrete technology step is as described below.
At supercritical CO
2put into the metal packing of rectangular saddle ring stainless steel loose heap in extraction kettle (Guangzhou Mei Chen high and new separation technology company produces the overcritical device of 300L*2), addition is 3/5 of extraction kettle volume.Get 95kg tomato red oleoresin and add 35kg peanut oil (19:7), squeeze in extraction kettle; Adopt supercritical CO
2fluid carries out boosting extraction, and static extracting pressure is 15MPa, and the time is 20min, and dynamic extraction pressure is 27MPa, extracts 5.5 hours, extraction temperature 55 DEG C, CO
2flow is 1410L/h.CO after extraction
2solvent is resolved, and one-level parsing pressure is 8MPa, one-level resolution temperature is 45 DEG C, and it is 6MPa that secondary resolves pressure, and secondary resolution temperature is 35 DEG C.Gaseous state CO after parsing
2by active carbon and alumina adsorption in absorber, remain in gaseous state CO completely to remove not resolve
2in residues of pesticides, through absorption after gaseous state CO
2again for supercritical CO
2fluid extraction.
By measuring residues of pesticides content such as carbendazim, Ethodan, cypermethrin, fenvalerate, phoxim, Rogor, malathions in raw material and product, 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 desirable residues of pesticides removal effect.
Embodiment 4: the method for this removal natural extract Pesticide Residues is to remove lutein oleoresin Pesticide Residues, and concrete technology step is as described below.
At supercritical CO
2put into the metal packing of rectangular saddle ring stainless steel loose heap in extraction kettle (Guangzhou Mei Chen high and new separation technology company produces the overcritical device of 300L*2), addition is 1/2 of extraction kettle volume.Get 65kg lutein oleoresin and add 65kg sunflower oil (1:1), squeeze in extraction kettle; Adopt supercritical CO
2fluid carries out boosting extraction, and static extracting pressure is 13MPa, and the time is 25min, and dynamic extraction pressure is 35MPa, extracts 10.0 hours, extraction temperature 75 DEG C, CO
2flow is 1310L/h.CO after extraction
2solvent is resolved, and one-level parsing pressure is 8.5MPa, one-level resolution temperature is 50 DEG C, and it is 6MPa that secondary resolves pressure, and secondary resolution temperature is 50 DEG C.Gaseous state CO after parsing
2by active carbon and alumina adsorption in absorber, remain in gaseous state CO completely to remove not resolve
2in residues of pesticides, through absorption after gaseous state CO
2again for supercritical CO
2fluid extraction.
By measuring residues of pesticides content such as Rogor, carbendazim, metrifonate, phoxim, Permanone, flucythrinate, killing logvalue, chlopyrifos in raw material and product, Rogor clearance 97.6%, carbendazim clearance 91.8%, metrifonate clearance 95.8%, phoxim clearance 88.8%, Permanone clearance 98.2%, flucythrinate clearance 89.7%, killing logvalue clearance 92.0%, chlopyrifos clearance 92.9%, all reaches desirable residues of pesticides removal effect.
Embodiment 5: the method for this removal natural extract Pesticide Residues is to remove linseed oil Pesticide Residues, and concrete technology step is as described below.
At supercritical CO
2put into the metal packing of rectangular saddle ring stainless steel loose heap in extraction kettle (Guangzhou Mei Chen high and new separation technology company produces the overcritical device of 300L*2), addition is 1/2 of extraction kettle volume.Get 130kg linseed oil (not adding edible oil), squeeze in extraction kettle; Adopt supercritical CO
2fluid carries out boosting extraction, and static extracting pressure is 14MPa, and the time is 20min, and dynamic extraction pressure is 20MPa, extracts 2.0 hours, extraction temperature 40 DEG C, CO
2flow is 1450L/h.CO after extraction
2solvent is resolved, and one-level parsing pressure is 7.5MPa, one-level resolution temperature is 30 DEG C, and it is 4MPa that secondary resolves pressure, and secondary resolution temperature is 30 DEG C.Gaseous state CO after parsing
2by active carbon and alumina adsorption in absorber, remain in gaseous state CO completely to remove not resolve
2in residues of pesticides, through absorption after gaseous state CO
2again for supercritical CO
2fluid extraction.
By measuring residues of pesticides content such as Rogor, carbendazim, phoxim, Aphox, Hostathion, Azodrin, cypermethrins in raw material and product, 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%, residues of pesticides removal effect is remarkable.
Claims (8)
1. remove a method for natural extract Pesticide Residues, it is characterized in that, the method step is: by the liquid natural extract containing residues of pesticides, or the liquid natural extract mixed with edible oil joins in extraction kettle; Irregular loose heap metal packing is provided with in described extraction kettle; Then adopt quiet dynamic bind Supercritical CO2 extraction to extract residues of pesticides in liquid natural extract, then resolve CO2 solvent, the natural extract removing residues of pesticides can be obtained;
Described static extracting pressure is 10 ~ 15MPa, and extraction time is 20 ~ 30min; Described dynamic extraction pressure is 20 ~ 35MPa, and extraction time is 2 ~ 10h; The extraction temperature of quiet dynamic extraction is 40 ~ 75 DEG C;
Described natural extract is partially fat-soluble natural extract, described residues of pesticides be organic phosphates, carbamates and pyrethroid pesticide remained in one or more.
2. the method for removal natural extract Pesticide Residues according to claim 1, is characterized in that: the weight ratio of described edible oil and liquid natural extract is 0 ~ 1:1.
3. the method for removal natural extract Pesticide Residues 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 removal natural extract Pesticide Residues according to claim 1, is characterized in that: described irregular loose heap metal packing is Intalox metal tower packing, and amount of filler is 1/2 ~ 2/3 of extraction kettle volume.
5. the method for removal natural extract Pesticide Residues according to claim 4, is characterized in that: the material of described irregular loose heap metal packing is stainless steel.
6. the method for removal natural extract Pesticide Residues according to claim 1, is characterized in that, the described secondary that resolves to is resolved: it is 7.5 ~ 10MPa that one-level resolves pressure, and it is 4 ~ 6MPa that secondary resolves pressure, and resolution temperature is 30 ~ 50 DEG C.
7. any one according to claim 1-6 removes the method for natural extract Pesticide Residues, it is characterized in that: the gaseous state CO2 after described parsing after adsorbent, again for extraction.
8. the method for any one removal natural extract Pesticide Residues according to claim 7, is characterized in that: described adsorbent is active carbon, discolour silica gel or aluminium oxide.
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CN103005005B (en) * | 2013-01-16 | 2014-01-22 | 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 |
CN103305343B (en) * | 2013-06-07 | 2015-02-18 | 佰香汇生物科技(厦门)有限公司 | Method for removing pesticide residue in citrus essential oil |
CN105838254B (en) * | 2016-03-17 | 2018-08-21 | 晨光生物科技集团股份有限公司 | It is a kind of to remove the remaining method of pesticide in capsicum oleoresin using molecular distillation |
CN105777699B (en) * | 2016-05-19 | 2017-11-17 | 湖北紫鑫生物科技有限公司 | A kind of preparation method of non agricultural chemical residuum black rice anthocyanin |
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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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CN1723969A (en) * | 2005-07-18 | 2006-01-25 | 天津大学 | Method for removing organic chlorine pesticide in ginseng by using supercritical carbon Co2 |
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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 |