CN102406216A - Method for controlling organophosphorus pesticide residue in bayberry juice through irradiation degradation - Google Patents
Method for controlling organophosphorus pesticide residue in bayberry juice through irradiation degradation Download PDFInfo
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- CN102406216A CN102406216A CN2011103828443A CN201110382844A CN102406216A CN 102406216 A CN102406216 A CN 102406216A CN 2011103828443 A CN2011103828443 A CN 2011103828443A CN 201110382844 A CN201110382844 A CN 201110382844A CN 102406216 A CN102406216 A CN 102406216A
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Abstract
The invention discloses a method for controlling organophosphorus pesticide residue in bayberry juice through irradiation degradation. The method comprises the following steps of: 1) precooling the bayberry juice at the temperature of between 1 and 4DEG C for 100 to 140 minutes; and 2) putting the precooled into an enclosed container, irradiating by using 60Co-gamma rays as a radiation source, wherein the irradiation dose is 4.8-5.2kGy and the irradiation dose rate is 780-820cGy/min. By the method, the organophosphorus pesticide residue can be effectively, quickly and safely reduced or eliminated from the bayberry juice, so that the maximum organophosphorus pesticide residue in the bayberry juice reaches the national limit standard.
Description
Technical field
The present invention relates to a kind of pass through parathion, fenifrothion and Entex in the irradiance method degraded cranberry juice, realize the method for organophosphorus pesticide in the control cranberry juice.
Background technology
Organophosphorus pesticide (Organophosphates; Be called for short OPs) grow up for replacing organo-chlorine pesticide; Worldwide be widely used at present; Account for first of pesticide market, organophosphorus pesticide have the drug effect height, wide in variety, prevention and treatment range is wide and cost is low, than the easy degraded of organo-chlorine pesticide, the harm of the environmental pollution and the ecosystem and residual also advantage such as general and outstanding not as good as organo-chlorine pesticide; Be the primary categories in the agricultural chemicals, in agricultural production, play the important and pivotal role.The organophosphorus pesticide major part is the ester class or the amides compound of phosphoric acid.Can be divided into phosphate, thiophosphate, phosphonate ester and Thiophosphonate class, phosphamide and thiophosphoryl amine by structure.At present, comprise that in the world the organophosphorus pesticide of Insecticides (tech) & Herbicides (tech), bactericide has reached kind more than 150, kind surplus the organophosphorus pesticide that China uses at present also has 30.
Yet along with Agricultural Development, the use amount of organophosphorus pesticide is more and more big, causes not only surface water and groundwater resources being polluted in its a large amount of remaining rainwater and the soil, and causes a large amount of agricultural product persticide residues to exceed standard.And; Organophosphorus pesticide has very strong toxicity; For a long time, after a large amount of the use, poisonous agricultural chemicals gets into food chain through modes such as food are residual, produces cumulative effect in animal body; Thereby cause harm such as teratogenesis, carcinogenic, mutagenesis, the human beings'health that is in the food chain top has been caused serious threat.A large amount of toxicity research show that organophosphorus pesticide has alkylating, can combine with the cholinesterase in the body behind the entering organism; Form more stable phosphorylated cholinesterase, cholinesterase is lost activity, forfeiture is to the capacity of decomposition of acetylcholine; Cause accumulating of the interior acetylcholine of body; Cause the disorder of nerve conduction physiological function, make animal and human's body produce poisoning symptom, even cause death.According to national requirements; 2007 China have forbidden that acephatemet, parathion, parathion-methyl, Azodrin, 5 kinds high malicious organophosphorus pesticides of phosphamidon producing and selling and agricultural at home go up to use (only keep produced in small quantities ability for export with the emergent demand of agricultural production); Organophosphorus pesticide in the vegetable and fruit is all had strict limiting the quantity of, as residual value of limiting the quantity of of parathion-methyl, parathion, fenifrothion, Entex be 0.01,0.01,0.5,0.05mg/kg etc.Become the key factor that threatens the agricultural product security and the export of farm produce to a certain extent at China's organophosphorus pesticide.Therefore it is residual and cause the biodegrading process of minimum influence to seem particularly important to quality of agricultural product to seek a kind of effectively degrading organic phosphor pesticides at present.
Residues of pesticides are results after the comprehensive functions such as absorption, degraded and migration; Wherein degraded is the critical process of its residual quantity of restriction; How to control organophosphorus pesticide in the agricultural product; Essential method is source control, promptly in agricultural cultivation processes such as red bayberry banned pesticides with remove residual in soil, water body and biology of organophosphorus pesticide in the planting environment.The former accomplishes that easily the latter is difficult to realize fully that so inevitable organophosphorus pesticide gets in the agricultural product, comprises red bayberry, has influence on the food security of agricultural product.In the exit procedure, be prone to be detected and exceed standard and return goods, cause the tremendous economic loss by the importer port.Therefore, residues of pesticides are to ensure food safety and the key that exports smoothly in the control agricultural product, and correlative study has become scientific and technological circle's emphasis brainstorm subject.
Irradiation obtains the concern and the application of more and more countries and international organization as a kind of food security and new technology that prolongs shelf life of improving in recent years, is also manifesting its huge economic and social benefit day by day.The FAO/IAEA/WHO food irradiation safe and sanitary joint specialist committee points out, can not cause toxicologic harm at 10kGy dosage with any food of internal irradiation.Research shows
60The Co-gamma-rays on degradable organic pollutant, be a kind of highly effective method (Wu Minghong, Bao Bairong. the application of radiotechnology in environmental protection. Beijing: Chemical Industry Press, 2002:13-33.), big quantity research shows
60It is residual that the Co-gamma-rays can effectively be controlled in the waste water organic pollution.But to be reported in China less in the residual research of agricultural chemicals in the relevant irradiation technique control agricultural byproducts; Correlative study mainly concentrates in the residues of pesticides control to agricultural product such as tealeaves, honey, shrimp and edible mushrooms; And in the relevant irradiation technique control fruit juice class agricultural byproducts residues of pesticides research to be reported in China few; Particularly control in the fruit juice class agricultural byproducts organophosphorus pesticide research report and have only one piece, this is discovered
60The Co-gamma-ray irradiation is handled fenifrothion in the normal temperature cider, parathion, parathion-methyl, thimet, chlorpyrifos degrading effect remarkable; Degradation rate is all more than 85%; If adopt the irradiation dose of 5kGy can make the organophosphorus pesticide in the cider be reduced to a very low level fully; Again not can to cider export main physical and chemical index impact (Chen Dongmei, Yue Tianli, Yuan Yahong etc.
60Co-γ irradiation is to organic phosphorus pesticide degradation in the cider and quality influence. EI, 2008,24 (3): 270-274).It is thus clear that the radiation treatment technology has certain application prospect in the residues of pesticides field in control fruit juice class agricultural byproducts.
Waxberry fruit is nutritious; Be rich in glucose, fructose, citric acid, malic acid, Cobastab, vitamin C etc., be applicable to processing fruit juice, cranberry juice has become an important fruit drink on the market; Owing to might use organophosphorus pesticide in the red bayberry production process; Cause organophosphorus pesticide unavoidably to get in the red bayberry, have influence on the food security of agricultural product such as cranberry juice, and relevantly how to control that the research of organophosphorus pesticide does not appear in the newspapers in the cranberry juice.
Summary of the invention
The technical problem that the present invention will solve provides the method for organophosphorus pesticide in a kind of irradiation-induced degradation control cranberry juice; Adopt the reduction that this method can be effective, quick, safe or eliminate organophosphorus pesticide in the cranberry juice, make in the cranberry juice the high residue value of organophosphorus pesticide reach national limit standard.
In order to solve the problems of the technologies described above, the present invention provides the method for organophosphorus pesticide in a kind of irradiation-induced degradation control cranberry juice, comprises the steps:
1), with cranberry juice in 1～4 ℃ of precooling 100～140 minutes;
2), the cranberry juice after the above-mentioned precooling is put into closed container, with
60The Co-gamma-rays is that radiation source carries out irradiation, and irradiation dose is 4.8～5.2kGy, and radiation dose rate is 780～820cGy/min.
Improvement as the method for organophosphorus pesticide in the irradiation-induced degradation control cranberry juice of the present invention: irradiation dose is SkGy, and radiation dose rate is 796.36cGy/min.That is, exposure time is 628 minutes.
Dose of radiation is meant gross absorption (kGy)=radiation dose rate * exposure time.
Reflect this; The present invention utilizes the potentiality of residues of pesticides in the irradiation technique control fruit juice class agricultural byproducts; Invent out the method for organophosphorus pesticide in a kind of irradiation-induced degradation control cranberry juice; Adopt the reduction that this method can be effective, quick, safe or eliminate organophosphorus pesticide in the cranberry juice, make in the cranberry juice the high residue value of organophosphorus pesticide reach national limit standard.
Because temperature can raise in the fruit juice radiative process; Be unfavorable for keeping of fruit juice quality; The present invention carries out precooling earlier through the cranberry juice to radiation treatment, carry out radiation treatment again, has realized keeping of organophosphorus pesticide control and cranberry juice quality in the cranberry juice effectively.
The present invention produces aquation free electron (eaq), free radical (OH, H), H after can making hydrone in the cranberry juice receive gamma-ray irradiation according to radiation treatment
2O
2Etc. the very high material of reactivity, these materials can react with weak link in the organophosphorus pesticide molecular structure in the cranberry juice, and radiation chemical reactions such as scission of link also can take place, and organic phosphorus pesticide degradation and active function key were lost efficacy.Select the dosage in the safe dose scope that the FAO/IAEA/WHO food irradiation safe and sanitary joint specialist committee points out for use; Set up a kind of effective, quick, safe reduction or eliminated the method for organophosphorus pesticide in the cranberry juice; Obtained satisfied result; Make that the high residue value of organophosphorus pesticide reaches national limit standard in the cranberry juice, the correlative study achievement is not appeared in the newspapers at present.
The inventor had once carried out following demonstration test in the invention process:
1 medicament and reagent
The standard items of three kinds of agricultural chemicals of parathion, fenifrothion and Entex.
Methyl alcohol (chromatographically pure), acetonitrile, sodium chloride, it is pure to be analysis, heavily steams before acetonitrile uses.
Cranberry juice (market purchase).
2 key instruments
60Co-gamma-ray irradiation source; Gas chromatograph (band nitrogen phosphorous detector).
3 solution preparations, Pesticides Testing and radiation treatment
3.1 solution preparation
3.1.1 organophosphorus pesticide standard liquid: accurately take by weighing parathion, fenifrothion and Entex standard items and be equipped with 50mg, be dissolved in the standard reserving solution of processing 1g/L in the 50mL methyl alcohol (promptly with methanol constant volume to 50mL) respectively, sealing is stored in 4 ℃ of refrigerators.
3.1.2 cranberry juice sample preparation: (1) draw respectively accurately 50 μ L to parathion, fenifrothion or Entex standard reserving solution in different 50mL volumetric flasks; Use the cranberry juice constant volume, being contained parathion, fenifrothion or Entex concentration respectively is the residual appearance of single farming of 1mg/L.(2) accurately draw 50 μ L parathion, fenifrothion and Entex standard reserving solution respectively in same 50mL volumetric flask, use the cranberry juice constant volume, contained parathion, fenifrothion and Entex concentration simultaneously and respectively be the agricultural residual appearance of the mixing of 1mg/L; Other draws the blank cranberry juice of 50mL in the 50mL volumetric flask, the mensuration contrast of cranberry juice physical and chemical index after being used to degrade.
3.2 radiation treatment
With preparation contain the residual cranberry juice sample of organophosphorus pesticide earlier 1～4 ℃ of precooling of refrigerator 120 minutes, change in the tool plug triangular flask, afterwards with
60The Co-gamma-rays is a radiation source, and irradiation dose is 5.0kGy, and close rate 796.36cGy/min (being that exposure time is 628 minutes) carries out irradiation to sample.
3.3 the detection of organophosphorus pesticide
The mensuration of organophosphorus pesticide (with reference to NY/T 761-2004), specific as follows:
Accurately pipette 25mL radiation treatment cranberry juice and in the heart-shaped bottle of 100mL, add the 50mL acetonitrile, jolting 3min is transferred in the 100mL tool plug graduated cylinder that 7g NaCl is housed, jolting 1min up and down, and room temperature leaves standstill 1h, makes acetonitrile mutually and the water layering.Draw and be concentrated near doing under 10mL supernatant 65～C, acetone is settled to 5mL, behind the 0.22um membrane filtration, measures organophosphorus pesticide with gas chromatographic analysis.
The mensuration of 4 cranberry juice physical and chemical indexs:
Total reducing sugar, total acid, soluble solid content are measured with reference to SB/T 10203-1994 in the cranberry juice; Colour and light transmittance are measured with reference to GB/T 18963-2003.
The concrete experiment as follows:
Test the residual control of the single residual appearance of 1 parathion
With preparation contain the single cranberry juice sample of parathion earlier refrigerator 1-4 ℃ precooling 120 minutes, change in the tool plug triangular flask, afterwards with
60The Co-gamma-rays is a radiation source, and irradiation dose is 5.0kGy, and close rate 796.36cGy/min carries out irradiation (being irradiation 628 minutes) to sample.Measure the residual quantity of parathion.The result shows that the parathion degradation rate reaches 99.3% in the single residual appearance of parathion, and residual concentration is 0.007mg/L, and residual quantity is in national limit standard.
Test the residual control of the single residual appearance of 2 fenifrothions
With preparation contain the single cranberry juice sample of fenifrothion earlier refrigerator 1-4 ℃ precooling 120 minutes, change in the tool plug triangular flask, afterwards with
60The Co-gamma-rays is a radiation source, and irradiation dose is 5.0kGy, and close rate 796.36cGy/min carries out irradiation (being irradiation 628 minutes) to sample.Measure the residual quantity of fenifrothion.The result shows that the fenifrothion degradation rate reaches 90.6% in the single residual appearance of fenifrothion, and residual concentration is 0.094mg/L, and residual quantity is in national limit standard.
Test the residual control of the single residual appearance of 3 Entexs
With preparation contain the single cranberry juice sample of Entex earlier refrigerator 1-4 ℃ precooling 120 minutes, change in the tool plug triangular flask, afterwards with
60The Co-gamma-rays is a radiation source, and irradiation dose is 5.0kGy, and close rate 796.36cGy/min carries out irradiation (being irradiation 628 minutes) to sample.Measure the residual quantity of Entex.The result shows that the Entex degradation rate reaches 99.4% in the single residual appearance of Entex, and residual concentration is 0.006mg/L, and residual quantity is in national limit standard.
Test 4 parathion, fenifrothion and Entex and mix the residual control of residual appearance
With preparation contain parathion, fenifrothion and Entex mixes residual cranberry juice sample earlier refrigerator 1-4 ℃ precooling 120 minutes, change in the tool plug triangular flask, afterwards with
60The Co-gamma-rays is a radiation source, and irradiation dose is 5.0kGy, and close rate 796.36cGy/min carries out irradiation (being irradiation 628 minutes) to sample.Measure the residual quantity of parathion, fenifrothion and Entex.The result shows, parathion, fenifrothion and Entex mixing degradation rate reach 99.2%, 89.7% and 99.1% respectively in the residual appearance, and residual concentration is respectively 0.008,0.103 and 0.009mg/L, and residual quantity is in national limit standard.
Test of the influence of 5 irradiation to cranberry juice physical and chemical quality index
With cranberry juice sample determination total reducing sugar, total acid, soluble solid content, colour and the light transmittance behind the irradiation.The result shows; Compare with contrast, radiation treatment can cause that soluble solid and total sugar content descend slightly in the cranberry juice, and total acid content increases slightly; Light transmittance slightly increases, colour slightly raises, but These parameters is compared the significant difference (p＜0.01) on the not statistically significant with contrast.It is thus clear that under this dosage, do not influence the quality of cranberry juice when reaching the control organophosphorus pesticide.
The specific embodiment
Below in conjunction with specific embodiment the present invention is further described, but protection scope of the present invention is not limited to this:
The method of organophosphorus pesticide in embodiment 1, the irradiation-induced degradation control cranberry juice, carry out following steps successively:
1), with cranberry juice in 1～4 ℃ of precooling 120 minutes;
2), the cranberry juice after the above-mentioned precooling is changed in the tool plug triangular flask, with
60The Co-gamma-rays is that radiation source carries out irradiation, and irradiation dose is 5kGy, close rate 796.36cGy/min, and exposure time is 628 minutes.
According to the method described above, 3 kinds of prior known cranberry juices of organophosphorus pesticide residual quantity that contain are in various degree tested, and be provided with corresponding contrast groups; This contrast groups is specially:
Contrast groups 1, with cranberry juice in 120 minutes alternative steps 1 of 15 degree insulations, afterwards cranberry juice is changed in the tool plug triangular flask over to step 2) with embodiment 1.
Contrast groups 2, step 2) in radiation parameter make into: irradiation dose is 5kGy, close rate 1000cGy/min, promptly exposure time is 500 minutes.All the other are with embodiment 1.
Contrast groups 3, step 2) in radiation parameter make into: irradiation dose is 5kGy, close rate 500cGy/min, promptly exposure time is 1000 minutes.All the other are with embodiment 1.
The result is as shown in table 1 below:
Table 1
The result shows:
With three kinds compare discovery; The inventive method is to 3 kinds of organophosphorus insecticide good degrading effect of concentration in various degree in the cranberry juice; The high residue value of organophosphorus insecticide all is up to state standards, and the quality of cranberry juice changes very for a short time simultaneously, reaches quality and agricultural residual control doulbe-sides' victory.And control group 1; Though also better (but effect is lower than the present invention to the organophosphorus insecticide degradation effect slightly; The preliminary treatment that low temperature is described can further improve follow-up radiation to the degradation effect of high concentration to the Phosphorus agricultural chemicals of machine), cause the cranberry juice quality obviously to be affected but do not carry out irradiation through precooling; The quality of control group 2 and control group 3 keep with agricultural residual control effect all not as the present invention.
At last, it is also to be noted that what more than enumerate only is several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (2)
1. the method for organophosphorus pesticide in the irradiation-induced degradation control cranberry juice is characterized in that comprising the steps:
1), with cranberry juice in 1～4 ℃ of precooling 100～140 minutes;
2), the cranberry juice after the above-mentioned precooling is put into closed container, with
60The Co-gamma-rays is that radiation source carries out irradiation, and irradiation dose is 4.8～5.2kGy, and radiation dose rate is 780～820cGy/min.
2. the method for organophosphorus pesticide in the irradiation-induced degradation control cranberry juice according to claim 1, it is characterized in that: irradiation dose is 5kGy, radiation dose rate is 796.36cGy/min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105454981A (en) * | 2015-11-25 | 2016-04-06 | 广东省粮食科学研究所 | Method for reducing chlopyrifos and triazophos residues in rice |
| CN109608540A (en) * | 2019-01-29 | 2019-04-12 | 广州华大生物科技有限公司 | A method of extracting collagen from fish scale |
| CN109619384A (en) * | 2018-12-14 | 2019-04-16 | 河南省科学院同位素研究所有限责任公司 | A kind of method of calcium silicates collaboration irradiation-induced degradation orthene |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1565280A (en) * | 2003-07-08 | 2005-01-19 | 宁波超能科技股份有限公司 | Radiation degradation technology for reducing synthetic pyrethroid analogue agricultural chemicals residue in tea |
Non-Patent Citations (2)
| Title |
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| 《农业工程学报》 20080515 陈冬梅等 ~(60)Co-gamma辐照对苹果汁中有机磷农药降解及品质影响 , 第05期 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105454981A (en) * | 2015-11-25 | 2016-04-06 | 广东省粮食科学研究所 | Method for reducing chlopyrifos and triazophos residues in rice |
| CN105454981B (en) * | 2015-11-25 | 2019-02-22 | 广东省粮食科学研究所 | A method of cutting down paddy Chlorpyrifos and Triazophos residue |
| CN109619384A (en) * | 2018-12-14 | 2019-04-16 | 河南省科学院同位素研究所有限责任公司 | A kind of method of calcium silicates collaboration irradiation-induced degradation orthene |
| CN109608540A (en) * | 2019-01-29 | 2019-04-12 | 广州华大生物科技有限公司 | A method of extracting collagen from fish scale |
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