As increasing the use of pesticides both in number and amount to boost crop production, consumer concerns over food quality and safety with respect to residual pesticides are also continuously increasing. However, there is still lacking of information that can effectively help to remove residual pesticides in foods. In recent years, contaminant removal by gas (or) glow discharge plasma (GDP) attracts great interests on environmental scientists because of its high removal efficiency and environmental compatibility. It was shown to be effective for the removal of some organophosphorus pesticides, phenols, benzoic acid, dyes, and nitrobenzene on solid substrate or in aqueous solution. This work mainly focuses on the removal of wide range of residual pesticides from fresh fruits and vegetables. As for preliminary study, the experiments were carried out to investigate whether GDP can be used as an effective tool for degrading target pesticides or not. With this objective, 60 selected pesticides drop wised onto glass slides were exposed to two types of GDP, dielectric barrier discharge plasma (DBDP) and low pressure discharge plasma (LPDP), for 5 min. Then, they were washed with 2 mL MeCN which were collected and used for determination of remaining concentration of pesticides using LC-MS/MS. Among selected pesticides, degradation of 18 pesticides (endosulfan-total was counted as one pesticide) by GDP could not be examined because control treatments, which were left in ambient environment, of those pesticides recovered less than 70% or even did not recover. However, majority of tested pesticides (42) were degraded by both types of GDP with satisfactory recovery (>80%) of control sample. Pesticides degradation ranged from 66.88% to 100% were achieved by both types of plasma except clothianidin which degradation in LPDP was 26.9%. The results clearly indicate that both types of gas discharge plasma are promising tools for degrading wide range of pesticides on glass substrate.
Ahn, Kyung-Geun;Kim, Gyeong-Ha;Kim, Gi-Ppeum;Hwang, Young-Sun;Hong, Seung-Beom;Lee, Young Deuk;Choung, Myoung-Gun
The Korean Journal of Pesticide Science
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v.19
no.3
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pp.195-203
/
2015
Quintozene, pentachloronitrobenzene (PCNB) is a contact fungicide for control of soilborne phytopathogenic fungi during cultivation of diverse crops. It was introduced to agricultural use around 1930's as a substitute for mercurial disinfectants. Although quintozene had been first registered in Korea on 1969. However, now it was banned to use due to its high residue levels in selected harvest products. Also, high possibility is expected that the residue may be contained in imported agricultural commodities as it is still used widely over the world. Therefore, this study was conducted to establish a determination method for quintozene residue in crops using GC/ECD/MS. Quintozene residue was extracted with acetonitrile from representative samples of five raw products which comprised hulled rice, soybean, Kimchi cabbage, green pepper, and apple. The extract was diluted with saline water, and n-hexane partition was followed to recover quintozene from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The quintozene was quantitated by GLC with ECD, using a DB-1 capillary column. The crops were fortified with quintozene at 3 levels per crop. Mean recoveries ranged from 79.9% to 102.7% in five representative agricultural commodities. The coefficients of variation were less than 4.3%. Quantitative limit of quintozene was 0.004 mg/kg in representative five crop samples. A GC/MS with selected-ion monitoring was also provided to confirm the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of quintozene in agricultural commodities.
Effect of the application time on the persistence of IBP and isoprothiolane in rice plant was studied in the field and effects of the water depth and soil texture on their persistence were also tested as a pot experiment. When granules were applied to the rice paddy water, two fungicides were readily absorbed through the root system and rapidly translocated to the upper parts of the plant. The concentrations of two fungicides in rice plant reached to the maximum within 24 hr regardless of the application time. When applied at the maximum tillering stage, the persistence pattern of two fungicides in plant showed similar trends; that is, residue levels of two compounds declined rapidly upto 7 days after application but more slowly thereafter. When applied at the heading stage, the persistence pattern of IBP in plant was similar to the maximum tillering stage while isoprothilane was quite different; 3 ppm reached on 3rd days after application was maintained almost constant for further 25 days. There was no effect of the water depth on the persistence of two compounds in plant and IBP concentration in plant was also not affected by soil texture. However, isoprothiolane in plant was higher in sandy loam than in loam and clay loam. Isoprothiolane residues in plant were much higher than those of IBP.
Ahn, Kyung-Geun;Kim, Gyeong-Ha;Kim, Gi-Ppeum;Kim, Min-Ji;Hwang, Young-Sun;Hong, Seung-Beom;Lee, Young Deuk;Choung, Myoung-Gun
The Korean Journal of Pesticide Science
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v.18
no.4
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pp.321-329
/
2014
This experiment was conducted to establish an analytical method for residues of amisulbrom, as recently developed an oomycete-specific fungicide showing inhibition of fungal respiration, in crops using HPLC-UVD/MS. Amisulbrom residue was extracted with acetonitrile from representative samples of five raw products which comprised apple, green pepper, kimchi cabbage, potato and hulled rice. The extract was diluted with 50 mL of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. For the hulled rice sample, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. On an octadecylsilyl column in HPLC, amisulbrom was successfully separated from sample co-extractives and sensitively quantitated by ultraviolet absorption at 255 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery test on every crop samples fortified with amisulbrom at 3 concentration levels per crop in each triplication. Mean recoveries ranged from 85.3% to 105.6% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of amisulbrom was 0.04 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue. The proposed method was sensitive, reproducible and easy-to-operate enough to routinely determine the residue of amisulbrom in agricultural commodities.
In order to determine the removal efficiency of pesticide residues in fruits and vegetables by washing processes, samples of lettuce, young Chinese radish, Chinese cabbage, green red pepper, strawberry and grape were artificially contaminated with malathion and washed according to the household practices. After three times washings with water, the remaining ratios of malathion residues in grape, green red pepper, strawberry, young Chinese radish, lettuce and Chinese cabbage were 9.7%, 25.2%, 28.0%, 29.7%, 38.9% and 57.5%, respectively. After washing with detergent solution followed by two times rinsing with water, the remaining ratios of malathion residues in the same food samples were 1.6%, 8.3%, 15.8%, 24.8%, 27.2% and 45.9%, respectively. The removal efficiency of malathion by detergent washing was significantly higher than the water washings only. The removal ratio of malathion residues was the highest in the first washing and the ratio fell greatly in the following washings. The removal efficiency was not quite different in the temperature range of $5-35^{\circ}C$ of the washing solution, but the efficiency at $100^{\circ}C$ was 2-3 times higher than other temperature ranges.
Kim, Eun-Hee;Jang, Mi-Ra;Kim, Jin-A;Kim, Tae-Rang;Yook, Dong-Hyun;Hwang, In-Sook;Kim, Jung-Hun
Korean Journal of Food Science and Technology
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v.43
no.3
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pp.277-281
/
2011
A rapid and very sensitive high-performance liquid chromatography/atmospheric-pressure chemical-ionization mass spectrometry method to detect ethylenethiourea (ETU) fungicide residues in fruits was developed. Methylene chloride was used as the surface extraction solvent for the target component. Recovery rates improved when cysteine hydrochloride and sodium carbonate were added to product prior to fortification. The limits of detection and quantification were approximately 0.006 and 0.02 mg/kg, respectively, from mandarin oranges. Recoveries from mandarin oranges, oranges, bananas, and pears, spiked in the range of 0.05-0.5 mg/kg, averaged 80-100%. The proposed method was used to monitor the presence of ETU in commercial fruits purchased from different markets in Seoul, Korea. ETU was found in four orange peels and in three mandarin orange peel samples. The highest ETU residue levels were $73.6{\mu}g/kg$ and $29.8{\mu}g/kg$.
To get information on the behavior of phorate in vegetables under the subtropical conditions, phorate granule (10%) was applied to silt loam soil at the rate of 40㎏ a.i./ha and incorporated to 10㎝ soil depth just befere sowing. Insecticide residues in vegetables were determined with GLC and confirmed qualitatively with TLC. Phorate and its metabolites were absorbed by the radish and carrot roots and rapidly translocated into foliages. The compounds detected in vegetables were phorate, phorate sulfoxide, and phorate sulfone. Residue levels of compounds in radishes were higher in foliages than in roots and much more residues were present in leaf lamina than in midribs. The concentration of the total residues in vegetable roots was rapidly decreased with the time, while the amount of total residues in radish roots was increased with the time. Therefore, the rapid decline of residue levels in vegetables was mainly attributed to the dilution of insecticide residues by the rapid growth of these vegetables.
BACKGROUND: The analytical method was established for determination of fungicide chinomethionat in several animal commodities using gas chromatography (GC) coupled with electron capture detector (ECD). METHODS AND RESULTS: In order to verify the applicability, the method was optimized for determining chinomethonat in various livestock products including beef, pork, chicken, milk and egg. Chinomethionat residual was extracted using acetone/dichloromethane(9/1, v/v) with magnesium sulfate and sodium chloride (salting outassociated liquid-liquid extraction). The extract was diluted by direct partitioning into dichloromethane to remove polar co-extractives in the aqueous phase. The extract was finally purified with optimized silica gel 10 g. CONCLUSION: The method limit of quantitation (MLOQ) was 0.02 mg/kg, which was in accordance with the maximum residue level (MRL) of chinomathionate as 0.05 mg/kg in livestock product. Recovery tests were carried out at two levels of concentration (MLOQ, 10 MLOQ) and resulted in good recoveries (84.8~103.0%). Reproducibilities were obtained (Coefficient of variation <5.2%), and the linearity of calibration curves were reasonable (r2>0.995) in the range of 0.01-0.2 ㎍/mL. This established analytical method was fully validated and could be useful for quantification of chinomathionat in animal commodities as official analytical method.
Kim, Rina;Cho, Heechan;Jeong, Jinan;Kim, Jihye;Lee, Sugyeong
Resources Recycling
/
v.29
no.1
/
pp.17-24
/
2020
In this study, rare earth elements (REE) leaching from a refractory REE ore containing goethite as a major gangue mineral was conducted, introducing a two-stage method of chemical decomposition-acid leaching. At the chemical decomposition step, using one of alkaline agent, NaOH, the ore was decomposed, changing NaOH concentration from 20 to 50 wt% at 10% (w/w) of pulp density and the maximum temperature achieved without boiling at each NaOH concentration. With increasing NaOH concentration, light REE (Ce, La and Nd) and iron were concentrated in the solid phase which is the decomposed product, while aluminum (Al) and phosphorus (P) were removed to the liquid phase, and their concentrations in the solid phase were down to 0.96 and 0.17%, respectively. In addition, through XRD analysis, it was found that the crystallinity of goethite was considerably decreased. At the acid leaching step, the product decomposed by 50 wt% NaOH was leached at 3.0 M HCl and 80 ℃ for 3 hr, then the REE leaching efficiency was above 94% (Ce 80%), and the leaching efficiencies of Al and P were decreased to 12 and 0%, respectively. Therefore, in terms of both REE leaching efficiency and impurity removal, those decomposition and leaching conditions were chosen as optimum processing methods of the investigated material. In terms of REE leaching mechanism, because REE and iron leaching efficiencies showed the positive correlation each other, so it can be concluded that decreasing crystallinity of goethite affect the improvement of REE leaching.
Journal of the Korea Organic Resources Recycling Association
/
v.14
no.3
/
pp.148-156
/
2006
Potential hydrocarbon degrading bacteria were screened from the site artificially polluted with 20,000 ppm of diesel. Among the isolates, two strains, SJD2 and SJD4, showed higher activities to degrade diesel on the Bushnell-Hass broth medium containing 2% of diesel. 16S rDNA sequence analysis revealed that SJD2 and SJD4 were Bacillus fusifomis and B. cereus, respectively. Both strains were found to grow in a wide range of temperature between $20^{\circ}C-55^{\circ}C$, with the best at $30^{\circ}C-37^{\circ}C$. This is the first report, as far as we know, that B. fusifomis is capable of degrading diesel. We hope that a new isolate, B. fusifomis, will efficiently conduct bioremediation at the contaminated sites with petroleum hydrocarbons.
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