• Korean Journal of Environmental Agriculture
• /
• v.38 no.4
• /
• pp.321-331
• /
• 2019

BACKGROUND: Pinoxaden is the phenylpyrazoline herbicide developed by Syngenta Crop Protection, Inc. and marketed on 2006. The maximum residue levels for wheat and barley were set by import tolerance. Thus, Ministry of Food and Drug Safety (MFDS) official analytical method determining Pinoxaden residue was necessary in various food matrixes. Satisfaction of international guideline of CODEX (Codex Alimentarius Commission CAC/GL 40) and National Institute of Food and Drug Safety Evaluation-MFDS (2017) are additional pre-requirements for analytical method. In this study, liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was investigated to analyze residue of Pinoxaden (M4), which is defined as pesticide residue in Korea, in foods. METHODS AND RESULTS: Pinoxaden (M4) was extracted followed by acid digestion (2hr reflux with 1N HCl) and pH adjusting (pH 4-5 with 3% ammonium solution). To remove oil, additional clean-up step with hexane saturated with acetonitrile was required to high oil contained sample before purification. HLB cartridge and nylon syringe filter were used for purification. Then, samples were analyzed by LC-MS/MS using reserve phase column C₁₈. Five agricultural group representative commodities (mandarin, potato, soybean, hulled rice, and red pepper) were used to verify the method in this study. The liner matrix-matched calibration curves were confirmed with coefficient of determination (r²) > 0.99 at calibration range 0.002-0.2 mg/kg. The limits of detection and quantitation were 0.004 and 0.01 mg/kg, respectively, which were suitable to apply Positive List System (PLS). Mean average accuracies of pinoxaden (M4) were shown to be 74.0-105.7%. The precision of pinoxaden and its metabolites were also shown less than 14.5% for all five samples. CONCLUSION: The method investigated in this study was suitable to CODEX (CAC/GL 40) and National Institute of Food and Drug Safety Evaluation-MFDS (2017) guideline for residue analysis. Thus, this method can be useful for determining the residue in various food matrixes in routine analysis.

• Korean Journal of Environmental Agriculture
• /
• v.18 no.2
• /
• pp.109-115
• /
• 1999

Lead and cadmium were analyzed with different pretreatemnt methods. Paddy soil and wastewater sludge samples were used and the result was compared each other. Pretreatment method affected the concentration obtained from samples significantly. Large difference was illustrated between the results. The concentration by 0.1N HCl extraction method, an official analytical method for soil and solid wastes, was far lower than those by the EPA3050B and mixed-acid digestion methods. The reason might be that metals associated with organics and silicates are not easily extracted by 0.1N HCl, while digestion methods using strong acids and high temperature dissolved all the elements in the samples. It implies that pretreatment method should be specified in addition to concentration on the report of metal analysis for environmental samples. Acid digestion methods are not necessarily good because the concentration obtained does not represent the natural condition which is our concern in many cases. The 0.1N HCl extraction method does not fully represent the natural condition either. The metals associated with organics will be extracted eventually as organics decompose with time. Therefore, proper pretreatment and analytical methods should be developed for specific purpose, and their standardization is recommended.

• Analytical Science and Technology
• /
• v.28 no.3
• /
• pp.175-181
• /
• 2015

Cyantraniliprole, which is an ananthranilic diamide insecticide that was developed by the DuPont Corporation, was registered in the Republic of Korea in 2012. It offers exceptional insecticidal activity on a broad range of Lepidopera, Coleoptera, Diptera, and Isoptera. The maximum residue limits are set to pepper, peach, apple, sweet pepper, welsh onion, and so on (0.2~2.0 mg/kg). Therefore, an analytical method for determining cyantraniliprole residue in agricultural products was developed to ensure food safety. In previous studies, welsh onions were among vegetables included in the allium species, which is a representative plant with sulfur organic compounds. In this study, the analytical method was developed and evaluated for the elimination of sulfur compounds from the test solution of allium species during pesticide residue analysis. In order to inactivate the enzyme allinase and produce sulfur compounds, sample extraction was made in the base state pH 10 by reducing the activity of the enzyme. The recoveries of the developed method ranged from 81.9% to 83.2%, and the relative standard deviations were less than 10%. Therefore, based on the results, the method developed in this study is accurate and appropriate for use in cyantraniliprole determination. It will be used as the official method for managing the safety of cyantraniliprole residues in agricultural products.

• Analytical Science and Technology
• /
• v.26 no.2
• /
• pp.154-163
• /
• 2013

The maximum residue limits of pyrimisulfan is set as 0.05 mg/kg in rice in 2011, so very reliable and sensitive analytical method for pyrimisulfan residues is required for ensuring the food safety of pyrimisulfan residues in agricultural products. In this study, a rapid and sensitive analytical method was developed and validated using liquid chromatography electrospray ionization tandem mass spectrometry (LC-MS/MS) for the determination of herbicide pyrimisulfan residues in agricultural products. Average recoveries of pyrimisulfan ranged from 88.7 to 99.3% at the spiked level of 0.005 mg/kg and from 90.1 to 94.2% at the spiked level of 0.05 mg/kg, while the relative standard deviation was less than 10%. Linear range of pyrimisulfan was between 0.01~1.0 ${\mu}g/mL$ with the correlation coefficient ($r^2$) 0.999 and limit of quantification was 0.005 mg/kg. The results of method validation were satisfied Codex guideline. The results revealed that the developed and validated analytical method is possible for pyrimisulfan determination in agricultural product samples and will be used as an official analytical method.

• The Korean Journal of Pesticide Science
• /
• v.21 no.1
• /
• pp.75-83
• /
• 2017

The single residue analytical method was developed for determining fungicide pencycuron residues in various agricultural commodities with high-performance liquid chromatography (HPLC). Pencycuron residue was extracted with acetone from representative crops such as Korean cabbage, apple, brown rice and green pepper. After ethyl acetate/n-hexane partition and subsequent clean-up with silica gel chromatography, pencycuron residue was quantified by reversed phase HPLC with UV detection at 240 nm. The suspected residue of pencycuron was confirmed using selected-ion monitoring (SIM) LC/mass spectrometry (MS). Instrumental limit of quantitation (ILOQ) and method LOQ (MLOQ) were set at 2 ng and 0.02 mg/kg, respectively. Overall recoveries of pencycuron from different crop samples fortified at three levels (MLOQ, 10MLOQ, 100MLOQ) were 72~108%. This proposed method could be useful as official analytical method for quantification of pencycuron residues in agricultural commodities.

• Analytical Science and Technology
• /
• v.23 no.2
• /
• pp.128-137
• /
• 2010

The purpose of this study is to set up the analytical method of new persistent organic pollutants (POPs) such as chlordecone, endosulfan, ${\alpha}$-HCH, ${\beta}$-HCH, ${\gamma}$-HCH. The analytical methods for these compounds listed as new POPs by the Stockholm Convention need to be newly established. Therefore, we proposed the analytical method for 5 organic chlorinated pesticides (OCPs) and then applied the analytical method to environmental samples. To do this, the pre-treatment such as florisil and activated carbon cleanup process in the Korean official method for classic POPs had been reviewed. All of compounds except chlordecone were pre-treated simultaneously with reviewed cleanup process and detected by GC/MS and HRGC/HRMS respectively. There is a problem that chlordecone could not get a high sensitivity by GC analysis, but in this study GC/MS method was proposed.

• Journal of Radiation Protection and Research
• /
• v.42 no.2
• /
• pp.114-129
• /
• 2017

Background: The purpose of this paper is to confirm the event timings and the magnitude of fission product aerosol release from the Fukushima accident. Over a few hundreds of technical papers have been published on the environmental impact of Fukushima Daiichi accident since the accident occurred on March 11, 2011. However, most of the research used reverse or inverse method based on the monitoring of activities in the remote places and only few papers attempted to estimate the release of fission products from individual reactor core or from individual spent fuel pool. Severe accident analysis code can be used to estimate the radioactive release from which reactor core and from which radionuclide the peaks in monitoring points can be generated. Materials and Methods: The basic material used for this study are the initial core inventory obtained from the report JAEA-Data/Code 2012-018 and the given accident scenarios provided by Japanese Government or Tokyo Electric Power Company (TEPCO) in official reports. In this research a forward method using severe accident progression code is used as it might be useful for justifying the results of reverse or inverse method or vice versa. Results and Discussion: The release timing and amounts to the environment are estimated for volatile radioactive fission products such as noble gases, cesium, iodine, and tellurium up to 184 hours (about 7.7 days) after earthquake occurs. The in-plant fission product behaviors and release characteristics to environment are estimated using the severe accident progression analysis code, MELCOR, for Fukushima Daiichi accident. These results are compared with other research results which are summarized in UNSCEAR 2013 Report and other technical papers. Also it may provide the physically based arguments for justifying or suspecting the rationale for the scenarios provided in open literature. Conclusion: The estimated results by MELCOR code simulation of this study indicate that the release amount of volatile fission products to environment from Units 1, 2, and 3 cores is well within the range estimated by the reverse or inverse method, which are summarized in UNSCEAR 2013 report. But this does not necessarily mean that these two approaches are consistent.

• Korean Journal of Environmental Agriculture
• /
• v.40 no.2
• /
• pp.134-141
• /
• 2021

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.

• Journal of Food Hygiene and Safety
• /
• v.37 no.3
• /
• pp.129-135
• /
• 2022

The official analytical method for the analysis of harmful heavy metals in Meju, distributed in Korea, employs a strong acid to decompose the organic components. This analysis is time consuming and harmful to the users and/or the environment. This study aimed to develop a new pre-treatment technology using laser ablation, to rapidly analyze harmful heavy metals without using strong acids. The results obtained from this method were validated by the National Institute of Food and Drug Safety Evaluation guideline (NIFDS, 2016). Moreover, a comparison of the two methods showed that the analytical time for 55 Meju samples was shortened by 96% or more in the new method. The results showed no significant difference in the recovery ranging from 90-120%. The proposed method proved suitable for detecting harmful heavy metals in Meju.

• Journal of Soil and Groundwater Environment
• /
• v.17 no.6
• /
• pp.33-42
• /
• 2012

This study was performed to find the problems according to interference factors (organic matter, pH, Cr, Mn, Fe, clay, and etc.) when we analyzed the hexavalent chromium [Cr(VI)] in soils using UV/VIS spectrometer (US EPA 7196A), attempted to evaluate the domestic applicability of analytical method (US EPA 7199) using IC-UV/VIS spectrometer as alternative method. The recovery rate of certified reference materials was 75.0% (US EPA 7196A) and 101.4% (US EPA 7199) by the analytical methods. As the results of performing QA/QC about US EPA 7199, method detection limit (MDL) and limit of quantification (LOQ) were 0.062 mg/kg, 0.196 mg/kg, respectively. The LOQ of US EPA 7199 was lower than that of the current soil official testing method in Korea (0.5 mg/kg). Cr(VI) contents in 23 soil samples were compared by the analytical methods of EPA 7196A and 7199. Cr(VI) was detected in 13 of 23 soil samples by EPA 7196A, while EPA 7199 was not detected in any soil samples. The Cr(VI) content in 23 soil samples by EPA 7196A was not clearly correlated with Cr, Fe, Mn and clay content in the soil samples. However, the contents of Cr(VI) and organic matter of the soil samples had the highest coefficient of determination ($R^2$) of 0.80. In order to evaluate the correlation between the recovery rates of Cr(VI) and organic matter contents in the soil samples, the recovery rates of 5 soil samples added Cr(VI) standard solution were analyzed by the analytical methods. According to the results, the higher the organic matter contents in soil samples, the lower the recovery rates of Cr(VI) by US EPA 7196, while in case of US EPA 7199, the recovery rates were stable regardless of the organic matter contents.