• Korean Journal of Environmental Agriculture
• /
• v.34 no.2
• /
• pp.120-127
• /
• 2015

BACKGROUND: Supervised residue trials were conducted to establish pre-harvest residue limit(PHRL), a criterion to ensure the safety of the pesticide residue in the crop harvest, of amisulbrom for winter-grown cabbage in two fields. Following to application of amisulbrom on the crop, time-course study was carried out to obtain the amisulbrom dissipation of statistical significance which enabled to calculate the predicted values of PHRL. METHOD AND RESULTS: During cultivation under greenhouse condition, samples of winter-grown cabbage were collected at 0, 1, 3, 5, 7 and 10 days after amisulbrom application, and subjected to residue analysis. Analytical method was validated by recoveries ranging 93.7~100.0% as well as limit of quantitation(LOQ) of 0.04 mg/kg. Amisulbrom residues in winter-grown cabbage gradually decreased as time elapsed. The dissipation rate of the residue would be affected by intrinsic degradation along with dilution by the cabbage growth. The decay pattern was well fitted by the simple first-order kinetics. CONCLUSION: Biological half-lives of amisulbrom in winter-grown cabbage ranged 3.7~4.1 days in two field conditions. Based on the regression of amisulbrom dissipation, PHRLs of amisulbrom in winter-grown cabbage were recommended as 8.86~9.47 and 4.21~4.35 mg/kg for 10 and 5 days before harvest, respectively.

• Horticultural Science & Technology
• /
• v.34 no.4
• /
• pp.644-654
• /
• 2016

Supervised residue trials for mandipropamid in Korean cabbage(Brassica campestris L.) were conducted to establish its pre-harvest residue limit (PHRL), a criterion to ensure the safety of the terminal pesticide residue during cabbage production. Tissues of Korean cabbage were collected at 0, 1, 3, 5, 7, and 10 days after mandipropamid application and subjected to residue analysis. The analytical method was validated by recoveries ranging from 88.2-92.2% at two levels (0.4 and $2.0mg{\cdot}kg^{-1}$), and a limit of quantitation (LOQ) of $0.04mg{\cdot}kg^{-1}$. Mandipropamid residues in Korean cabbage gradually decreased over time. The dissipation rate of the residue would be affected by intrinsic degradation of the compound along with dilution resulting from the fast growth of Korean cabbage. The decay pattern was well fitted by simple first-order kinetics. Biological half-lives of mandipropamid in Korean cabbage ranged from 3.9-4.0 days in two field conditions. Calculated by the regression curve of mandipropamid dissipation, the PHRLs of mandipropamid in Korean cabbage were recommended as 11.07-12.19 and $5.76-6.05mg{\cdot}kg^{-1}$ for 10 and 5 days prior to harvest, respectively.

• The Korean Journal of Pesticide Science
• /
• v.16 no.3
• /
• pp.230-235
• /
• 2012

This study was carried out to clarify effects of field location and sprayer on the level of pesticide residue in chilli peppers. As confirmed by statistical analysis, the residue levels in green pepper among three greenhouses did not show significant difference at the first day after spraying with the same engine sprayer and nozzle. But the residue levels in green peppers collected from the exposed outside of crop were 2 times higher than those from the hidden inside. The sampling site was one of variation elements of pesticide residue. The residue levels after application by knapsack engine powered sprayer were 1.7 times higher than those by manual compressed sprayer. As the spraying pressure of the engine power sprayer is 2 times higher than the commonly used pressure of the manual compressed sprayer, the pressure of the sprayer and nozzles were considered to affect on the residue levels in peppers.

• Journal of the Korean Chemical Society
• /
• v.63 no.5
• /
• pp.335-341
• /
• 2019

Spirulina was cultured in Selenium solution and the total concentration was determined with isotope dilution technique. Low-molecular-weight-Selenium species for the water extract of Spirulina were separated and quantified with HPLC ICP/MS. Water extraction was used first and then protein enzyme (protease XIV) was used to digest and extract for the Se species in both water extract and residue. The total Se was $414.9{\pm}4.0{\mu}g\;g^{-1}$ and 77% existed in water extract while 22% remained in residue. Se species in supernatant was mostly inorganic selenate ($222.7{\mu}g\;g^{-1}$). After hydrolysis of protein, SeCys ($15.20{\mu}g\;g^{-1}$) and SeMet ($12.13{\mu}g\;g^{-1}$) were found. In residue, SeCys and SeMet were found with little inorganic Se. After protein hydrolysis of residue, more of Selenoamino acids SeCys ($9.35{\mu}g\;g^{-1}$) and SeMet ($18.23{\mu}g\;g^{-1}$) in addition to MeSeCys ($1.5{\mu}g\;g^{-1}$) were found. It is thought that inorganic selenium is mostly adsorbed on the surface of spirulina and can be easily removed by a simple distilled water extraction while most of organo-seleniums are remained in residue.

• Korean Journal of Agricultural Science
• /
• v.43 no.4
• /
• pp.634-640
• /
• 2016

The objective of this study was to evaluate the effectiveness of using HR-GC/MS for the rapid screening of dieldrin residues in soils. Persistent organic pollutants (POPs) of organochlorine pesticides such as dieldrin, were analyzed in sedimentary rock and granite rock collected from greenhouses, Niigata, Japan. Dieldrin remains in Japanese farming soils, more than 40 years after their use as insecticides was prohibited. The averages in soil moisture ranged from 2.79% to 7.20% in soils derived from sedimentary rock and from 25.59% to 31.40% in soils derived from granite rock. Mean concentrations of dieldrin residues in sedimentary rock and granite rock were $39.7ng\;g^{-1}$ and $40.51ng\;g^{-1}$, respectively. Dieldrin residue was detected at a slightly higher concentration in granite rock than sedimentary rock samples. There was no consistency between the two soils or between surface and subsurface soils. The coefficients of variation of the two soils were 10.6% and 8.7%, respectively. These results suggest that our high-resolution mass spectrometry detector (HR-GC/MS) is effective at analyzing residual organochlorine pesticides in soil. In order to increase the precision and sensitivity for chemical analysis of POPs, high-resolution gas chromatography coupled with a HR-GC/MS is highly recommended.

• Agribusiness and Information Management
• /
• v.3 no.1
• /
• pp.11-22
• /
• 2011

This study describes the development of a web-based system that collects all data generated in the research conducted to set pre-harvest residue limits (PHRLs) for agricultural product safety control. These data, including concentrations of pesticide residues, limit of detection, limit of quantitation, recoveries, weather charts, and growth rates, are incorporated into a database, a regression analysis of the data is performed using statistical techniques, and the PHRL for an agricultural product is automatically computed. The development and establishment of this system increased the efficiency and improved the reliability of the research in this area by standardizing the data and maintaining its accuracy without temporal or spatial limitations. The system permits automatic computation of the PHRL and a quick review of the goodness of fit of the regression model. By building and analyzing a database, it also allows data accumulated over the last 10 years to be utilized.

• Journal of Welding and Joining
• /
• v.35 no.3
• /
• pp.21-27
• /
• 2017

A soldering temperature of ($235{\pm}3$) $^{\circ}C$ is described in ISO 9455-15 for the copper corrosion test. However, this temperature is not suitable for performing lead-free solder pastes. We evaluated the compatibility of a lead-free solder paste in the experimental conditions of (Liquidus temperature + ($35{\pm}3$)) $^{\circ}C$. Based on the results after a Cu corrosion test, a proper temperature for Pb-free soldering was (melting point+($35{\pm}3$)) $^{\circ}C$. Criteria used to evaluate corrosion due to discoloration of flux residue is described in ISO 9455-15, but a more quantitative evaluation standard is needed. In this study, experimental error level was estimated by analyzing flux residue after a corrosion test for 72, 500 hours of specimens using EDS analysis with acceleration voltage. It was determined that the copper area at the flux residue boundary is suitable for the EDS analysis area.

• Mass Spectrometry Letters
• /
• v.10 no.2
• /
• pp.50-55
• /
• 2019

The fragmentation statistics of ion trap CID (Collision-Induced Dissociation) spectra using 87,661 tandem mass spectra of doubly charged tryptic peptides are analyzed here. In contrast to the usual method of using intensity information, the frequency of occurrence of fragment ions, with respect to the position of the cleavage site and the residues at these sites is studied in this paper. The analysis shows that the frequency of occurrence of fragment ion peaks is more towards the middle of the peptide than its ends. It was noted that amino acid with an aromatic and basic side chain at N- & C- terminal end of the peptide stimulates more peaks at the lower end of the spectrum. The residue pair effect was shown when the amide bond occurs between acidic and basic residues. The fragmentation at these sites (D/E-H/R/K) stimulates the generation of the y-ion peak. Also, the cleavage site H-H/R/K stimulates the generation of b-ions. K-P environment in the peptide sequence has more tendency to generate y-ions than b-ions. Statistical analysis helps in the visualization of the CID fragmentation pattern. Cleavage pattern along the length of the peptide and the residue pair effects, enhance the knowledge of fragmentation behavior, which is useful for the better interpretation of tandem mass spectra.

• Korean Journal of Environmental Agriculture
• /
• v.42 no.1
• /
• pp.71-81
• /
• 2023

An accurate and easy-to-use analytical method for determining isocycloseram and its metabolites (SYN549431 and SYN548569) residue is necessary in various food matrixes. Additionally, this method should satisfy domestic and international guidelines (Ministry of Food and Drug Safety and Codex Alimentarius Commission CAC/GL 40). Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) was used to determine the isocycloseram and its metabolites residue in foods. To determine the residue and its metabolites, a sample was extracted with 20 mL of 0.1% formic acid in acetonitrile, 4 g magnesium sulfate anhydrous and 1 g sodium chloride and centrifuged (4,700 G, 10 min, 4℃). To remove the interferences and moisture, d-SPE cartridge was performed before LC-MS/MS analysis with C₁₈ column. To verify the method, a total of five agricultural commodities (hulled rice, potato, soybean, mandarin, and red pepper) were used as a representative group. The matrix-matched calibration curves were confirmed with coefficients of determination (R²) ≥ 0.99 at a calibration range of 0.001-0.05 mg/kg. The limits of detection and quantification were 0.003 and 0.01 mg/kg, respectively. Mean average recoveries were 71.5-109.8% and precision was less than 10% for all five samples. In addition, inter-laboratory validation testing revealed that average recovery was 75.4-107.0% and the coefficient of variation (CV) was below 19.4%. The method is suitable for MFDS, CODEX, and EU guideline for residue analysis. Thus, this method can be useful for determining the residue in various food matrixes in routine analysis.

• Analytical Science and Technology
• /
• v.9 no.2
• /
• pp.1033-1060
• /
• 1996