• Analytical Science and Technology
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• v.26 no.2
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• pp.142-153
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• 2013

A new, rapid, and simple analytical method was developed and validated using high performance liquid chromatograph-photodiode array detector (HPLC-PAD) for the determination of lepimectin residues in agricultural commodities. The lepimectin residues in samples were extracted with methanol, partitioned with dichloromethane, and then purified with glass column filled with subsequently to aminopropyl ($NH_2$) solid phase extraction (SPE) cartridge. The purified samples were detected using HPLC-PAD. Correlation coefficient ($R^2$) of both lepimectin $A_3$ and $A_4$ solutions were 0.9999. The method was validated using cucumber spiked with lepimectin at 0.02 and 0.2 mg/kg and pepper, mandarin, hulled rice, potato, soybean at 0.02 and 0.5 mg/kg. Average recoveries were 76.0~114.8% with relative standard deviation less than 10%, and limit of detection (LOD) and limit of quantification (LOQ) were 0.005 and 0.01 mg/kg, respectively. The result of recoveries and overall coefficient of variation of a laboratory results in Gwangju regional KFDA and Daejeon regional KFDA was followed with Codex guideline (CAC/GL 40). Therefore, developed method in this study is accurate, rapid, and appropriate for lepimectin determination and will be used to keep safety of lepimectin residues in agricultural products.

• Korean Journal of Environmental Agriculture
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• v.31 no.3
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• pp.277-285
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• 2012

BACKGROUND: For safety evaluation of imported agri-food in Korea, the multiresidue analysis method was establised for unregistered organophosphorus pesticides, aspon, chlorthion, chlorthiophos, crotoxyphos, demeton-O, demeton-S, demeton-S-methyl, dioxathion, heptenophos, iodofenphos, leptophos, methyl-trithion, propetamphos and sulfotep. METHODS AND RESULTS: The used method for multiresidue analysis in brown rice and orange used as representative samples of imported agri-food was the official method of Korean Food and Drug Administration. The results of validation test of 13 organophosphorus pesticides except crotoxyphos for multiresidue analysis method are compared to the criteria such as specificity, linearity, accuracy, precision and limit of quantification. CONCLUSION: The used method for multiresidue analysis of unregistered 13 organophosphorus pesticides except crotoxyphos in Korea can surely be used as an official method for routine analysis of imported agri-food.

• Korean Journal of Environmental Agriculture
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• v.28 no.2
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• pp.209-220
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• 2009

Octachlorostyrene(OCS) has been persisted in environment because it has not been decomposed easily. And, it has been known as highly toxic compounds to the environment and human as well as accumulated as high concentrations in a biota through a food chain. Therefore, OCS was monitored for water, soil and fish sampled from the areas where were able to be contaminated with OCS. The recoveries of octachlorostyrene were 93.1${\sim}$98.6% in water, 90.4${\sim}$94.8% in soil and 81.5${\sim}$90.2% in fish and detection limits were 0.0004 mg $L^{-1}$ for water, and 0.002 mg $kg^{-1}$ for soil and fish, respectively. OCS was not detected in water, sediment, soil and fish samples from Ulsan, Yeosu, Daejeon and Sihwa industrial complex and in soil sampled nearby incineration plants in all parts of the country. Accordingly, we estimated that there is no risk from exposure of OCS.

• Journal of Applied Biological Chemistry
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• v.65 no.1
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• pp.17-21
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• 2022

A new rapid and simple method for metalaxyl in Atractylodes macrocephala Koidzumi and Achyranthes japonica Nakai has been developed and validated. This study was conducted to develop a method for analyzing metalaxyl by a method based on QuEChERS using liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Samples were extracted with acetonitrile and purified using amino-propyl (NH₂) Solid Phase Extraction cartridge. The method limit of quantitation (MLOQ) was 0.01 mg/kg. The linearity of matrix-matched calibration curve (r²) was ≥0.99 at the calibration range of 0.001-0.05 mg/kg. For recovery test, Atractylodes macrocephala Koidzumi or Achyranthes japonica Nakai was treated with standard solutions at MLOQ and 10MLOQ levels. Recovery rates were in the range of 88.1-109.1% with <5.5% coefficient of variation. This established analytical method was fully validated. Based on these results, it can contribute to improving the safety of residual pesticides in Atractylodes macrocephala Koidzumi and Achyranthes japonica Nakai.

• Analytical Science and Technology
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• v.21 no.6
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• pp.535-542
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• 2008

A liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) method was developed for the determination and confirmation of clenbuterol in bovine muscle and milk. Clenbuterol and clenbuterol-D9 using as an internal standard in samples were extracted with ethyl acetate after hydrolysis and evaporated to dryness. The extracts were dissolved in 20% methanol and cleaned using HLB solid-phase extraction cartridge. The analytes were detected by LC-ESI/MS/MS on a $C_{18}$ column. Mass spectral acquisition was done in selected reaction monitoring (SRM) in positive ion mode to provide a high degree of sensitivity. Using MS/MS with SRM mode, the transitions (precursor to product) monitored were m/z 277${\rightarrow}$203 for clenbuterol, and m/z 286${\rightarrow}$204 for internal standard. The limits of quantitation (LOQ) and mean recoveries of clenbuterol in bovine muscle were $0.2{\mu}g/kg$ and 84.3~91.1%, respectively. The LOQ and mean recoveries in milk were $0.05{\mu}g/kg$ and 87.7~98.3%, respectively.

• Journal of Food Hygiene and Safety
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• v.35 no.3
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• pp.225-233
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• 2020

By the standards and specifications for hygiene products, three test methods for formaldehyde are specified for each item type of hygiene product. After derivatization using acetylacetone and 2,4-dinitrophenylhydrazine (2,4-DNPH), formaldehyde is analyzed by spectrophotometer and high-performance liquid chromatography (HPLC). Validation of the three test methods was performed on tissue, diaper lining and waterproof layer, and panty liner products. The results of linearity (R²), limit of detection (LOD), limit of quantification (LOQ), recovery rate (%) and reproducibility (%), showed that all three methods are suitable for analyzing formaldehyde in hygiene products. After derivatization with 2,4-DNPH and cetylacetone, formaldehyde was analyzed at 0, 3, 6, 9, 24 and 48 hours by HPLC. Formaldehyde derivatized with 2,4-DNPH showed no statistically significant change in formaldehyde peak area over time (P>0.05). But, acetylacetone-derivatizated formaldehyde showed a negative correlation coefficient (r) over time (P<0.01). We investigated the residual amounts of formaldehyde in 205 hygiene products distributed in Busan. Among 74 disposable diaper products tested, 73 had low concentrations of formaldehyde (0.13-29.87 mg/kg). Moreover, formaldehyde was not detected in any of 78 tissue, 27 disposable paper towel, 12 disposable dishcloth, 7 paper cup, one brand of paper straw and 6 disposable napkin products.

• Current Research on Agriculture and Life Sciences
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• v.11
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• pp.101-110
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• 1993

The residues of combined insecticide of polynactin complex(tetranactin) and BPMC were determined to establish an index for the safety use to apple. Evaluation was made on residual concentration of tetranactin and BPMC in apple as a function of application frequency and date when the combined insecticide of tetranactin and BPMC was sprayed into apple. Their persistence in soil were also studied under the field and laboratory conditions. Recovery percentage from apple was ranged from 74.0 to 77.5 in tetranactin, 87.1 to 83.6 in BPMC, those from soil was 82.3 to 88.4 in tetranactin, 83.6 to 887.1 in BPMC. The minimum detectable limits of tetranactin and BPMC were 0.01ppm in apple pulp and 0.03ppm in apple peel and soil. The residue percentage of tetranactin and BPMC in the peel and pulp part of apple was about 96 in peel part by five sprays up to 3th day before harvest. The residues of tetranactin and BPMC in apple are proved to 0.39ppm and 0.75ppm by five sprays up to 30days before harvest. Maximum residue limit(MRL) of BPMC for fruits was established of 0.3ppm in Environment Protection Agency of Korea, and thus it is suggested that the preharvest intervals of combined insecticide for apple could be 30 days with twice spray. The half life of tetranactin in soil under field and laboratory conditions was 6.9 and 24.4 days, and in case of BPMC was 6.3 and 23.2 days, respectively.

• The Korean Journal of Pesticide Science
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• v.19 no.4
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• pp.361-369
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• 2015

This study investigated residual characteristics of bistrifluron and fluopicolide in Korean cabbage, and suggested the pre-harvest residue limits (PHRLs) based on their dissipation patterns and biological half-lives. The pesticides were sprayed on Korean cabbage in two different region under greenhouse conditions at the recommended dose, respectively. The samples for residue analysis were harvested at 0 (2 hr), 1, 2, 4, 6, 8 and 10 days after treatment, and analyzed by HPLC after clean-up with Florisil SPE. The limit of quantification (LOQ) was $0.03mg\;kg^{-1}$ for bistrifluron and fluopicolide, and the recoveries ranged from 87.2-110.6% with below 5% of RSD. The biological half-lives of field I and field II were 3.9 and 4.2 days for bistrifluron and 4.9 and 4.2 days for fluopicolide, respectively. The PHRL of bistrifluron and fluopicolide were recommended as 3.83 and $3.23mg\;kg^{-1}$ for 10 days before harvest, respectively.

• The Korean Journal of Pesticide Science
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• v.20 no.3
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• pp.221-227
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• 2016

This study was conducted to investigate residual organochlorine pesticides in green house soil and green perilla leaves. Extraction and clean-up method were developed using the modified QuEChERS method for residual organochlorine pesticides (ROCPs) in soil and green perilla leaves. Recovery and limit of quantitation (LOQ) of ROCPs in greenhouse soil and green perilla leaves were 76.3-113.4 and 79.4-107.3%, 0.03-0.24 and $0.33-0.50{\mu}g/kg$, respectively. Detected ROCPs in greenhouse soil were dieldrin and endosulfan sulfate, the residue were 1.6-9.2 and $22.0-87.8{\mu}g/kg$, respectively. But two pesticides in all green perilla leaf samples were not detected. These results showed that ROCPs residue in greenhouse soil was lower than the level of bioaccumulation occurring.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.19 no.6
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• pp.375-381
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• 2018

This study was performed to investigate the residual characteristics of the insecticide dinotefuran in asparagus under greenhouse conditions from July to August and consequentially to obtain basic data for guidelines on the safe use of this pesticide in asparagus. Residues of dinotefuran in young stem of asparagus before and after growing mother stem were analyzed from samples collected at 0, 1, 3, 5, and 7 days after single application of a commercial formulation of dinotefuran (wettable powder, 10%) at the recommended dose (2,000 times dilution). The residue of dinotefuran in young stem of asparagus was analyzed by HPLC-UVD, and recovery of dinotefuran in young stem was tested at 0.5 and 1.0 mg/kg concentrations. As a result, the limit of quantitation (LOQ) of dinotefuran was 0.01 mg/kg, and the recovery of dinotefuran was in the range of 83.3-94.0% with a coefficient of variation less than 10%. Residues of dinotefuran in young stem of asparagus before and after growing the mother stem were lower than the tentative limit (0.05 mg/kg) from 5 and 3 days after single application, respectively. Based on these results, single application of dinotefuran (wettable powder, 10%) at the recommended dose at 7 days before harvest would have no deleterious effects on safety issues concerning pesticide residue. This result might provide basic information to construct guidelines for the safe use of dinotefuran in asparagus.