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

• The Korean Journal of Pesticide Science
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• v.19 no.3
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• pp.218-229
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• 2015

The proficiency testing for the residue laboratories of pesticide registration was conducted in order to improve the reliability and the ability for pesticide residue analysis. On November 2012 the testing was carried out using the soil collected and kept as the moistened state for five years, which was expected to very low residue levels of pesticides. The soil was fortified with azoxystrobin, imidacloprid and methabenzthiazuron in a manner similar to prepare soil samples for indoor soil degradation test, and then sub-samples were prepared for the distribution to participants. Some of them were randomly selected for confirm of homogeneity and to ensure the stability of samples at room temperature. Samples were consisted of two soils treated as different levels, one of which was used to the assessment and another used to confirm. In addition, provided three standard solutions, respectively concentration of 10 mg/L, and untreated soil. Forty eight institutions submitted results. The medians of results were used as the assigned values for pesticide residues. Fitness for purpose standard deviation of proficiency test was calculated by applying 20% RSD as the coefficient of variation allowed in the soil residue test. Z-score was applied for evaluation of individual pesticides, and the average of the absolute value of the Z-score for the overall assessment of pesticides. Laboratories evaluated the absolute value of the Z-score less than 2 to fit the case of azoxystrobin were 48, imidacloprid and methabenzthiazuron 46.

• 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.

• The Korean Journal of Pesticide Science
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• v.20 no.3
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• pp.211-220
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• 2016

This study was to develop the analytical reference material of green-pepper for multi-residue analysis of pesticides. According to the ISO Guide 35, ISO Guide 13528 and EURL-PT protocol, the homogeneity, stability, assigned value and uncertainty were calculated to assess if it was suitable to be used as the proficiency test or quality control. The values of the within-bottle standard variation ($s_{wb}$) and the between-bottle standard variation ($s_{bb}$) were 1.7~3.7% of assigned value according to the requirement of the ISO guide 35. And, the uncertainty ($u^*{_{bb}}$) due to inhomogeneity was 0.8~1.1% for all pesticides. The storage stabilities of ten-pesticides at various conditions were assessed. For all target pesticides, the slop ($b_1$) values were smaller than the corresponding values of $[t_{0.95,n-2}{\times}s(b_1)]$ specified by the ISO guide 35, indicating that there were no statistically significant decreases in the concentration of the target pesticides when the analytical reference material was stored at room temperature ($20{\sim}30^{\circ}C$) for 7 days, freezing ($-20^{\circ}C$) for 30 days and deep freezer ($-80^{\circ}C$. except for bifenthrin, fenpropathrin) for 245 days. For proficiency test by using it developed by Korea Institute of Toxicology, inter-lab test was performed with eight organization performing the residual pesticide analysis. We found that there were some different results among them. Some were assessed as questionable or unacceptable for two pesticides and one organization didn't analyze the six pesticides. From these results, this green-pepper analytical reference material containing ten-pesticides could be used as a tool for the proficiency test to improve the reliability or consistency for pesticide residue's results.

• The Korean Journal of Pesticide Science
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• v.17 no.2
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• pp.94-106
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• 2013

The proficiency testing for the residue laboratories of pesticide registration was conducted in order to improve the reliability and the ability for pesticide residue analysis. On October 2011 the testing was carried out using the soil collected and kept as the moistened state for five years, which is expected to very low residue levels of pesticides. The soil was fortified with chlorpyrifos, metolachlor and procymidone in a manner similar to prepare soil sample for indoor soil degradation test, and then sub-samples were prepared for the distribution to participants. Some of them were randomly selected for confirm of homogeneity and to ensure the stability of samples at room temperature. Samples were consisted of two soil treated as different levels, one of which was used to the assesment and another used to confirm. In addition, provide three standard solutions, respectively concentration of 10 mg/L, and untreated soil. Forty seven institutions submitted results. The medians of results were used as the assigned values for pesticide residues. Fitness for purpose standard deviation of proficiency test was calculated by applying 20% RSD as the coefficient of variation allowed in the soil residue test. Z-score was applied for evaluation of individual pesticides, and the average of the absolute value of the Z-score for the overall assessment of pesticides. Laboratories evaluated the absolute value of the Z-score less than 2 to fit the case of chlorpyrifos and procymidone were 44, metolachlor 40.

• Analytical Science and Technology
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• v.27 no.1
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• pp.66-77
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• 2014

This study was carried out to examine the authenticity discrimination of circulated vegetable oils by using carbon isotope ratio (${\delta}^{13}C$) and fatty acid composition. This analysis was applied to vegetable oils which we can buy in Korean markets, and the analytical instrument was measured by using EA-IR/MS for ${\delta}^{13}C$ and GC/FID for fatty acid composition. ${\delta}^{13}C$ was separated into 3 groups as $C_3$ plant including sesame oil, $C_4$ plant including maize oil, and rice bran oil. Fatty acid composition was significantly different among vegetable oils. In addition, the interval of low and high price vegetable oils was classified through the scatter plot analysis showing the correlation of the ${\delta}^{13}C$ and fatty acid composition. Therefore, through a simultaneous determination of the ${\delta}^{13}C$ and fatty acid composition, we are able to determine the majority of vegetable oils. It help to ensure food safety in Korean market by exclusion of economically modified adulteration in food.

• Journal of Food Hygiene and Safety
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• v.30 no.4
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• pp.366-371
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• 2015

This work was conducted to apply the multi class pesticide multiresidue method for determining the use of hexaconazole in the agricultural products using GC-NPD. The multi class pesticide multiresidue method results were validated for the assay of hexaconazole by using linearity, accuracy, precision, limit of detection and quantitation. The linearity in the concentration ranged from 0.025 to 5.0 mg/L ($R^2$ > 0.999). Lettuce recoveries ranged from 89.42% to 94.15% with relative standard deviations below 7.78%, for spiking levels from 0.04 to 4.0 mg/kg. The limit of detection was 0.04 mg/kg, and the limit of quantitation was 0.11 mg/kg. The intra- and inter-day precisions were 2.42~3.49% and 4.90~7.78%, respectively. We suggested that the multi class pesticide multiresidue method for determining hexaconazole was highly accurate and reproducible, and it will be used as a routine analysis in agricultural products.

• The Korean Journal of Pesticide Science
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• v.4 no.1
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• pp.1-10
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• 2000

The purpose of this study is to establish the assessment techniques of hazardous chemicals by the development of analytical method of biological samples. In this study, we have developed an extraction method of nine pesticides used for rice paddy that resulted in high recovery from the spiked human urine by the liquid-liquid extraction with diethyl ether at pH 7.0. Calibration curve obtained from each pesticide standard using by gas chromatography/mass spectrometry/selected ion monitoring has shown good linearity and detection limits were the range of $0.4{\sim}2.0$ ng/mL in urine. As a biological monitoring, urine samples of local farmers exposed directly to nine pesticides in the field were collected and analyzed by GC/MS. Of the tested pesticides, metabolites of phenthoate assumed were identified by GC/MS analysis. No parent compound was detected.

• The Korean Journal of Pesticide Science
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• v.18 no.4
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• pp.278-295
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• 2014

Fast and accurate multi-residue pesticides inspecting method needs in Agro-Fishery Products Inspection Center. So, We tried to seek the optimum method using GC-TOF/MS, GC-ECD, GC-NPD after QuEChERS sample preparation. In GC-TOF/MS, 138 kinds of pesticide were spiked at 0.3 and $0.5{\mu}g/g$for the identification and quantification in lettuce sample. Recoveries of 77 pesticides were between 70 and 130% with RSD (relative standard deviation lower than 20% at $0.3{\mu}g/g$. In GC-ECD, NPD, 146 kinds of pesticide were spiked for the identification and quantification in lettuce. Recoveries of 61 species were between 70 and 130% with lower than 20%. These results indicated that GC-TOF/MS, GC-ECD, NPD analysis with the QuEChERS sample preparation can be partly applied to multi-residue pesticides in vegetables.

• The Korean Journal of Pesticide Science
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• v.15 no.2
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• pp.140-148
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• 2011

The official analytical method of residue pesticides in herbal medicines by KFDA cannot be applied to all of the pesticides and herbal medicines because of various active materials in herbal medicines and various physicochemical properties of pesticides. Moreover, liquid-liquid partition uses harmful solvents such as methylene chloride and is consuming a lot of time and effort. In order to improve the problems, we have studied for the availability of the analytical method applying the macroporous diatomaceous earth (MDE) column instead of liquid-liquid partition to simultaneously analyze five pesticides in two dried herbal medicines. The results showed that the recovery rates of acetamiprid and azoxystrobin in Astragalus root by GC/ECD ranged from 89.6 to 94.1%, from 86.8 to 94.4%, respectively, and those of bifenthrin, chlorfenapyr, chlorpyrifos in Cnidii Rhizoma by GC/MS ranged from 83.6 to 88.4%, from 77.4 to 83.8%, from 82.6 to 84.3%, respectively. Also, the coefficients of variation (CV) for triplication ranged from 0.5 to 1.7%. The results satisfied the criteria of residue pesticide analysis, setting 70~120% for the recovery rate and below 10% for the coefficient of variation. The improved methods are safer to residue pesticide analysts, faster and less laborious than the KFDA official method.