• The Korean Journal of Pesticide Science
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• v.17 no.4
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• pp.264-270
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• 2013

Imidacloprid is a systemic insecticide which act as an insect neurotoxin. It used for control of pest such as aphids and other sucking insects in fruits and vegetables. Systemic pesticides move inside a crop following absorption by the plant, and these were converted into a variety of metabolites. Sometimes these metabolites make a problem about safety of agricultural products. So a simultaneous determination method of pesticide and its metabolites is needed, to monitor their presence in agricultural product and study on the fate of pesticide in a plant. This study's aim is to investigate simultaneous analysis method of imidacloprid and its metabolites, imidacloprid guanidine, imidacloprid olefin, imidacloprid urea, and 6-chloronicotinic acid in red pepper using QuEChERS method and LC-MS/MS systems. QuEChERS method was modifed beacuase $MgSO_4$ salts decreased the recoveries of 6-chloronicotinic acid in extraction procedure. Imidacloprid and its metabolites were extracted by acetonitrile with 1% glacial acetic acid and the extracts were purified through QuEChERS with primary secondary amine (PSA) and $C_{18}$ and analyzed with LC-MS/MS in ESI positive mode. Standard calibration curves were made by matrix matched standards and their correlation coefficients were higher than 0.999. Recovery studies were carried out on spiked pepper blank sample at four concentration levels (0.01, 0.04 and 0.1, 0.4 mg/kg). The average recoveries of imidacloprid and its metabolites were in the range of 70~120% with < 20% RSD. This result indicated that the method using QuEChERS and LC-MS/MS was suitable for the simultaneous determination of imidacloprid and its metabolites in red pepper.

• Applied Biological Chemistry
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• v.36 no.6
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• pp.463-468
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• 1993

In order to elucidate the translocation of the systemic insecticide, phosphamidon (2-chloro-2-diethylcarbamoyl-1-methylvinyl dimethyl phosphate), treated to pine trees against pine leaf gall midges (Thecodiplosis japonensis Uchida et Inouye), $[vinyl,\;carbonyl-^{14}C]$ phosphamidon was implanted into the trunks of 10-year-old Korean red pine (Pinus densiflora Sieb. et Zucc.) and Japanese black pine (Pinus thunbergii Parl.), respectively. The upward movement rates of the chemical within Korean red pine in July and Japanese black pine in December were ca. 10 cm/hr and 2 cm/hr, respectively. The original radioactivity level persisted up to 75 days after treatment throughout the whole tree in Korean red pine in July, whereas it did up to 150 days in Japanese black pine in December. The chemical was translocated up to the top at the insecticidal level within 3 days after treatment in July, whereas in December it was within 15 days. The translocation of the chemical was much dependent upon pine tree species and the treated season. Methanol was suitable for the extraction of phosphamidon and its metabolites from pine needles. Autoradiography of the methanol extracts of pine needles collected from the treated pine trees proved that phosphamidon broke down very quickly within pine trees (ca. 80% metabolized within 7 days).

• Korean Journal of Environmental Agriculture
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• v.5 no.2
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• pp.85-94
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• 1986

To study fate of carbofuran in paddy system, C-14 labelled carbofuran was applied to paddy water containing rice seedlings and time course study was made on the distribution, metabolism and chemical transformation of the systemic insecticide. Carbofuran was readily absorbed by plant root and translocated to shoots where most of the radioactivities were confined to leaf tips. The fact that gradual increases in radioactivities of both aqueous phase extracts and non-extractable fractions of plants (shoots and root) increased with incubation is taken as an evidence that reactions (phase I and II) proceed in rice plants. Carbofuran and its five metabolites were all detected by TLC in organic phase extracts of paddy plants or soil. Evidence was put forward that carbofuran and its five metabolites were all identified as aglycones of conjugates. 7-benzofuranol and 3-hydroxycarbofuran were the most abundant aglycones. Soil microbes appears to have little effects on the metabolism of carbofuran. They increased radioactivity of non-extractable fraction and reduced that of organic phase extracts of paddy soil.

• The Korean Journal of Pesticide Science
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• v.18 no.4
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• pp.228-235
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• 2014

The residue levels of flonicamid and its metabolites, 4-(trifluoromethyl)nicotinic acid (TFNA) and N-4-(trifluoromethyl)nicotinoyl glycine (TFNG) in sweer pepper were investigated to examine the residual characteristics of analytes for 87 days after pesticide application. The pesticide was applied once at recommended dosage and double dosage by foliar sprays and the samples of fruits and leaves of sweet pepper were collected for each treatment. The residues of flonicamid in all of fruits and leaves decreased gradually over time, while the residue levels of TFNG metabolite exhibited tendency that increased for long periods and thereafter decreased. Total flonicamid residual concentrations containing metabolites residues in fruit samples increased consistently until 30 days post-application and higher residue levels than residues at 1 day post-application were detected from 30 day to 87 day after treatment. The residue pattern observed in fruit could be explained by the movement of TFNG from leaves to fruits of plant. Such residual characteristic was similarly found in samples treated both recommended dosage and double dosage.

• Journal of The Korean Society of Clinical Toxicology
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• v.5 no.2
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• pp.99-105
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• 2007

Purpose: Pyrethroid is an insecticide that produces moderate intoxication in mammals, with neither exposure to skin nor inhalation resulting in severe systemic manifestations. In 2005 we made a nationwide survey of agrichemical human intoxication. The object of this study is to analyze pyrethroid intoxications based on the 2005 survey. Methods: We prospectively collected data from 1 August 2005 to 31 July 2006 by a standard investigation protocol. We analyzed demographic data, exposure data (cause, amount, ingredients), clinical features, and courses. Results: A total of 125 cases of pyrethroid intoxication were surveyed. The mean patient age was $56.78{\pm}16.158$ years old, and the mean amount ingested was $121.85{\pm}110.732ml$. Patients were classified into four severity groups according to symptoms and mental status: the asymptomatic group (27 patients, 21.6%), the mild symptom group (48, 38.4%), the moderate symptom group (21, 16.8%), and the severe symptom group (7, 5.6%). There were statistically significant differences in mental status, severity, and mean ICU days between two groups. Admission days by severity grade for the asymptomatic, mild, moderate, and severe symptom groups were $5.49{\pm}16.051,\;3.65{\pm}4.143,\;4.59{\pm}3.335,\;and\;8.14{\pm}7.199days$, respectively (p=0.047). Conclusion: Nationwide surveillance was extremely telling in uncovering a high frequency of agrichemical intoxication in Korea. In pyrethroid intoxication, severity grading can be a useful prognostic tool.

• Korean journal of applied entomology
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• v.56 no.4
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• pp.351-356
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• 2017

For determining the insecticidal effect of Carbofuran on the Brown planthopper, Nilaparvata lugens, sucking toxicity by drenching application, sucking and contact toxicity by leaf dipping application, and contact toxicity by topical application were examined. Drenching caused two types of mortality patterns. One was logarithmic curve at a relatively high concentration (8~30 ppm) with over 40% mortality in 24 h, and the other was an S-shaped curve at low concentrations (1~4 ppm) with over 60% mortality on the fifth day after Carbofuran treatment. Leaf dipping application caused a rapid increase in mortality in a day, and this effect decreased steadily with time. Topical application showed steep increase in mortality in a day, and hardly increased thereafter. The best mortality evaluation time for the drenching application was the second day (42 h), and that for the leaf dipping and topical applications was the first or second day after Carbofuran application. When the insecticide has systemic effects, drench application provides the best efficacy and its insecticidal effects persist for a longer time than any other application method.

• Korean Journal of Environmental Agriculture
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• v.40 no.4
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• pp.335-344
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• 2021

BACKGROUND: Cyantraniliprole is a systemic diamide insecticide that has been used to control lepidopteran pests in agriculture. Cyantraniliprole has become an issue due to its potentiality of unexpectable contamination in rotational crop cultivation. Thus, studies on the evaluation of cyantraniliprole translocated from soil into rotational crops are required. METHODS AND RESULTS: Cyantraniliprole was treated at a yearly maximum application level onto bare soil under greenhouse conditions in two geographically different regions. Lettuce was transplanted and spinach and radish were sown onto the soil 30 and 60 days-plant back intervals (PBIs) after cyantraniliprole treatment. The QuEChERS method was modified and coupled with LC/MS/MS analysis to determine the residues of cyantraniliprole in soil and plant samples. The methods for sample preparation and instrumental conditions were validated to meet the criteria of Codex guidelines and were successful to determine cyantraniliprole quantitatively and qualitatively in the samples. Cyantraniliprole residues in lettuce samples were 0.01 mg/kg for PBI 60 and 0.02 mg/kg for PBI 30, respectively. The residues in spinach samples were 0.01 mg/kg for PBI 60 and 0.01~0.02 mg/kg for PBI 30, respectively. Less than limit of the quantitation (LOQ) level (0.01 mg/kg) of cyantraniliprole was observed in radish samples. The residues in the plant samples were found as the levels less than maximum residue limit (MRL) for leafy and root vegetables. CONCLUSION(S): This study suggests PBI 30~60 days for rotational cultivation of lettuce, spinach and radish in greenhouse soil treated with cyantraniliprole at a yearly maximum application level.

• Korean Journal of Environmental Agriculture
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• v.31 no.3
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• pp.248-254
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• 2012

BACKGROUND: In order to elucidate residual characteristics of difenoconazole and thiamethoxam by treatment to sweet persimmons for one year and to generate the data for the maximum residue limit (MRL) establishment for those pesticides in or on sweet persimmon. METHODS AND RESULTS: Systemic fungicide difenoconazole WP (10% a.i.) and systemic insecticide thiamethoxam WG (10% a.i.) were sprayed onto 12~25-years-old sweet persimmons according to its preharvest interval (PHI), respectively, and then fresh sweet persimmons were harvested at 0, 1, 3, 7, 14, 21 days after treatment from pesticide-sprayed plots at each 3 sites. The analytical methods were evaluated to limit of quantification, linearity, specificity, reproducibility and recoveries. The crop samples were extracted with acetone and performed dichloromethane partition process. The extracted samples of difenoconazole were analyzed by GC-ECD and the thiamethoxam extracted samples were analyzed by HPLC with good sensitivity and selectivity of the method. The average recoveries of difenoconazole ranged from 87.5 to 99.5% with the percentage of coefficient variation in the range 4.1~7.6% at three different spiking levels(0.02, 0.2 and 2.0 mg/kg). And the average recoveries of thiamethoxam and clothianidin ranged from 88.8 to 98.9% and 83.2 to 96.6% with the percentage of coefficient variation in the range 3.6~5.0% and 3.8~9.4% at three different spiking levels(0.02, 0.2 and 2.0 mg/kg), respectively. The residue amounts ranges of difenoconazole were 0.2~0.56 mg/kg and the residue amount was decreased below the MRL level, 1.0 mg/kg, after 1 day harvest. The residue amounts ranges of thiamethoxam were 0.08~0.28 mg/kg and the residue amount was decreased below the MRL level, 0.5 mg/kg, after 1 day harvest. And the residue amount of clothianidin was below then 0.03 mg/kg for only one test site of 14 and 28 day samples. CONCLUSION: As a result, the residual amounts of difenoconazole and thiamethoxam were not exceeded the MRL of established criteria for sweet persimmon. The biological half-lives of difenoconazole and thiamethoxam were 13.6, 19.4, 16.3 and 10.0, 15.3, 14.0 days at each three test sites, respectively.

• The Korean Journal of Pesticide Science
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• v.17 no.3
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• pp.145-154
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• 2013

Flonicamid was a water-soluble and systemic insecticide. It was applied to control neonicotinod pesticide-resistant cotton aphid in sweet peppers. However, the residue levels of total flonicamid in sweet pepper exported to Japan in 2009 were exceeded the maximum residue limit (MRL). This study was conducted to elucidate residual properties of flonicamid parent compound and its metabolites in sweet peppers. It was carried out to compare the variation of residues in sweet pepper in three different greenhouses for 21 days after 3 times application with 7 days interval. The mean residues were 0.176, 0.152 and 0.108 mg $kg^{-1}$ and the residue levels in sweet pepper among three greenhouses show significant difference. The maximum residue levels were detected 10 days later after last treatments. The overall residue levels were lower than MRL 2.0 mg $kg^{-1}$ (by Korea) and 0.4 mg $kg^{-1}$ (by Japan in 2009 but now revised MRL is 2.0 mg $kg^{-1}$). But the residue level of total flonicamid at the 21th day after 3 times treatment with 7 days interval was 0.429 mg $kg^{-1}$ restricted by the application of double rate than recommended rate. The amounts of metabolites, TFNA, 4-Trifluoro methyl nicotinic acid and TFNG, N-(4-trifluoro methyl nicotinoyl) glycine were increased while flonicamid parent compound was decreased over time. Therefore the longer trial period should be needed for flonicamid in sweet peppers.

• Korean Journal of Environmental Agriculture
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• v.8 no.2
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• pp.103-118
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• 1989

In order to investigate the uptake of the systemic insecticide, carbofuran, 2,3-dihydro-2,2-dimethyl-7-benzofuranyl-N-methyl(arbamate) residues, fresh and aged, by rice plants, they were grown for 42 days in soils containing freshly treated (T-1), 3-month-aged (T-2), and 6-month-aged residues (T-3). The amounts of $^{14}CO_2$ evolved from $^{14}C-carbofuran$ during the 3-and 6-month aging in soil (temp. $22{\pm}1^{\circ}C$ ; moisture, 50% of the maximum water-holding capacity) were 8.9 and 26.7% of the original radioactivity applied, respectively. Mineralization of $^{14}C-carbofuran$ in soil to $^{14}CO_2$ during 42 days of rice growing was 4.4% (T-1), 11.0% (T-2), and 15.7 (T-3). The methanol extract of the 3-and 6-month-aged soils revealed that 3-keto carbofuran phenol (2,3-dihydro-2,2-dimethyl-3-oxo-7-benzofuranol) was the major metabolite, where as 3-hydroxy carbofuran (2,3-dihydro-2,2-dimethyl-3-hydroxy-7-benzofuranyl-N-methylcarbamate) turned out to be the major metabolite in the shoots by the enzymatic cleavage of the possible conjugate present in the methanol extract. Volatilization of $^{14}C-carbofuran$ in soil during 3-and 6-month-aging, and 42 days of rice growing was 0.026, 0.05, and 0.012-0.018% of the applied radioactivity, respectively. The $^{14}C-radioactivity$ which was absorbed from the soils by rice plants during 42 days of the growing period and persisted in rice plant tissues was 26.8, 21.4, and 10.3% in T-1, T-2, and T-3, respectively. The non-extractable bound residues were 8.3, 37.9, and 54.6% of the originally applied carbofuran in T-1. T-2, and T-3, respectively. The small translocation of $^{14}C-radioactivity$ in T-3 upwards suggests that major metabolite 3-keto carbofuran phenol is conjugated in roots and the low recovery in T-1 indicates the loss of carbofuran from the shoots.