• Korean Journal of Environmental Agriculture
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• v.32 no.3
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• pp.214-223
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• 2013

BACKGROUND: This study focused on the development of an analytical method about dichlorprop (DCPP; 2-(2,4-dichlorophenoxy)propionic acid) which is a plant growth regulator, a synthetic auxin for agricultural commodities. DCPP prevents falling of fruits during their growth periods. However, the overdose of DCPP caused the unwanted maturing time and reduce the safe storage period. If we take fruits with exceeding maximum residue limits, it could be harmful. Therefore, this study presented the analytical method of DCPP in agricultural commodities for the nation-wide pesticide residues monitoring program of the Ministry of Food and Drug Safety. METHODS AND RESULTS: We adopted the analytical method for DCPP in agricultural commodities by gas chromatograph in cooperated with Electron Capture Detector(ECD). Sample extraction and purification by ion-associated partition method were applied, then quantitation was done by GC/ECD with DB-17, a moderate polarity column under the temperature-rising condition with nitrogen as a carrier gas and split-less mode. Standard calibration curve presented linearity with the correlation coefficient ($r^2$) > 0.9998, analysed from 0.1 to 2.0 mg/L concentration. Limit of quantitation in agricultural commodities represents 0.05 mg/kg, and average recoveries ranged from 78.8 to 102.2%. The repeatability of measurements expressed as coefficient of variation (CV %) was less than 9.5% in 0.05, 0.10, and 0.50 mg/kg. CONCLUSION(S): Our newly improved analytical method for DCPP residues in agricultural commodities was applicable to the nation-wide pesticide residues monitoring program with the acceptable level of sensitivity, repeatability and reproducibility.

• Journal of Food Hygiene and Safety
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• v.32 no.4
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• pp.267-274
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• 2017

This paper deals with the natural occurrence of total aflatoxins ($B_1$, $B_2$, $G_1$, and $G_2$) in commercial herbs for food and medicine. To monitor aflatoxins in commercial herbs for food and medicine not included in the specifications of Food Code, a total of 62 samples of 6 different herbs (Bombycis Corpus, Glycyrrhizae Radix et Rhizoma, Menthae Herba, Nelumbinis Semen, Polygalae Radix, Zizyphi Semen) were collected from Yangnyeong market in Seoul, Korea. The samples were treated by the immunoaffinity column clean-up method and quantified by high performance liquid chromatography (HPLC) with on-line post column photochemical derivatization (PHRED) and fluorescence detection (FLD). The analytical method for aflatoxins was validated by accuracy, precision and detection limits. The method showed recovery values in the 86.9~114.0% range and the values of percent coefficient of variaton (CV%) in the 0.9~9.8% range. The limits of detection (LOD) and quantitation (LOQ) in herb were ranged from 0.020 to $0.363{\mu}g/kg$ and from 0.059 to $1.101{\mu}g/kg$, respectively. Of 62 samples analyzed, 6 semens (the original form of 2 Nelumbinis Semen and 2 Zizyphi Semen, the powder of 1 Nelumbinis Semen and 1 Zizyphi Semen) were aflatoxin positive. Aflatoxins $B_1$ or $B_2$ were detected in all positive samples, and the presence of aflatoxins $G_1$ and $G_2$ were not detected. The amount of total aflatoxins ($B_1$, $B_2$, $G_1$, and $G_2$) in the powder and original form of Nelumbinis Semen and Zizyphi Semen were observed around $ND{\sim}21.8{\mu}g/kg$, which is not regulated presently in Korea. The 56 samples presented levels below the limits of detection and quantitation.

• The Korean Journal of Pesticide Science
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• v.18 no.3
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• pp.130-140
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• 2014

Recently, some of the previous studies reported that tolclofos-methyl is still exist in ginseng cultivated soil, even though it is has been banned for ginseng. Therefore, the current study was aimed to examine the levels of absorption and translocation of tolclofos-methyl from ginseng cultivated soil to ginseng root and leaf stem for the period of 1 year. For this study, ginseng plants were transplanted in pots and treated with $5.0mg\;kg^{-1}$ of tolclofos-methyl (50% WP). At the end of each interval periods (every three months) the samples (soil, roots and leaf stems) were collected and analyzed the absorption and translocation levels of tolclofos-methyl using gas chromatography and mass spectrometry (GC-MS). The limit of quantitation of tolclofos-methyl was found to be $0.02mg\;kg^{-1}$ and 70.0~120.0% recovery was obtained with coefficient of variation of less than 10% regardless of sample types. In this study, a considerable amount of translocation of tolclofos-methyl residues were found in soil (4.28 to $0.06mg\;kg^{-1}$), root (7.09 to $1.54mg\;kg^{-1}$) and leaf stem (0.79 to $0.69mg\;kg^{-1}$). The results show that the tolclofos-methyl was absorbted and translocated from ginseng cultivated soil to ginseng root and ginseng leaf stem and found to be decreased time-coursely. Secondly, we were also analyzed soil, root and leaf stems samples from Hongcheon, Cheorwon, Punggi and Geumsan by GC-MS/MS (172 pesticides), LC-MS/MS (74 pesticides). In this study, 43 different pesticides were detected ($0.01{\sim}7.56mg\;kg^{-1}$) in soil, root and leaf stem. Further, tolclofos-methyl was detected 4 times separately in root sample alone which is less ($0.01{\sim}0.05mg\;kg^{-1}$) than their maximum residual limit (MRL) in ginseng. Consequently, the results from both studies indicate the residues of tolclofos-methyl found in ginseng cultivated soil and ginseng ensuring their safety level. Moreover, long-term evaluations are needed in order to protect the soil as well as ginseng free from tolclofos-methyl residues.

• Journal of Food Hygiene and Safety
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• v.37 no.2
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• pp.39-45
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• 2022

This study aimed to investigate the validation and modify the analytical method to determine quercetin-3-𝑜-gentiobioside and isoquercitrin in Abelmoschus esculentus L. Moench for the standardization of ingredients in development of functional health products. The analytical method was validated based on the ICH (International Conference for Harmonization) guidelines to verify the reliability and validity there of on the specificity, linearity, accuracy, precision, detection limit and quantification limit. For the HPLC analysis method, the peak retention time of the index component of the standard solution and the peak retention time of the index component of A. esculentus L. Moench powder sample were consistent with the spectra thereof, confirming the specificity. The calibration curves of quercetin-3-𝑜-gentiobioside and isoquercitrin showed a linearity with a near-one correlation coefficient (0.9999 and 0.9999), indicating the high suitability thereof for the analysis. A. esculentus L. Moench powder sample of a known concentration were prepared with low, medium, and high concentrations of standard substances and were calculated for the precision and accuracy. The precision of quercetin-3-𝑜-gentiobioside and isoquercitrin was confirmed for intra-day and daily. As a result, the intra-day precision was found to be 0.50-1.48% and 0.77-2.87%, and the daily precision to be 0.07-3.37% and 0.58-1.37%, implying an excellent precision at level below 5%. As a result of accuracy measurement, the intra-day accuracy of quercetin-3-𝑜-gentiobioside and isoquercitrin was found to be 104.87-109.64% and the daily accuracy thereof was found to be 106.85-109.06%, reflecting high level of accuracy. The detection limits of quercetin-3-𝑜-gentiobioside and isoquercitrin were 0.24 ㎍/mL and 0.16 ㎍/mL, respectively, whereas the quantitation limits were 0.71 ㎍/mL and 0.49 ㎍/mL, confirming that detection was valid at the low concentrations as well. From the analysis, the established analytical method was proven to be excellent with high level of results from the verification on the specificity, linearity, precision, accuracy, detection limit and quantitation limit thereof. In addition, as a result of analyzing the content of A. esculentus L. Moench powder samples using a validated analytical method, quercetin-3-𝑜-gentiobioside was analyzed to contain 1.49±0.01 mg/dry weight g, while isoquercitrin contained 1.39±0.01 mg/dry weight g. The study was conducted to verify that the simultaneous analysis on quercetin-3-𝑜-gentiobioside and isoquercitrin, the indicators of A. esculentus L. Moench, is a scientifically reliable and suitable analytical method.

• Parasites, Hosts and Diseases
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• v.33 no.4
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• pp.357-364
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• 1995

The protozoan parasite, Entcmoeba histoIWticc, is one of major causative agents of intestinal disease all over the world. In acute experimental infection, the early host response to 5. histoIHtica is characterized by an infiltration of neutrophils. However, the chemotactic signal for this response is not well known. Based on the (jading that human epithelial cells produce the potent neutrophil chemoattractant and activator, interleukin-8 (IL-8), IL-8 gene expression was examined thoroughly in human colon epithelial cells exposed to 5. histolvtica trophozoites. Cellular RNAs were extracted from HT-29 or Caco-2 human colon epithelial cells exposed to 5. histoLvtica trophozoites for 30 minutes, 1 and 3 hours. IL-8 mRNA transcripts were measured by reverse transcriptional polprnerase chain reaction (RT-PCR) using synthetic standard RNA. The number of IL-8 mRNA molecules increased from 30 minutes to 3 hours of exposure period, reaching 3.1 H 107 molecules/ug of total RNA. Expression pattern of IL-8 mRNA transcripts was parallel to the amounts of IL-8 protein measured by enzyme-linked immunosorbent assay (ELISA) . Lysates of 5. histoIVtica also induced expression of mRNA for IL-8 in colon epithelial cells. These results sugf:esc that acute inflammatory reaction by 5. histoIVticc may be initially triggered by proinflammatory cytokines such as IL-8 secreted from epithelial cells of the colon.

• Journal of Environmental Health Sciences
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• v.23 no.2
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• pp.72-82
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• 1997

This study was performed to investigate the effect of co-existence of BPMC, carbaryl and chlorothalonil on the short-term bioconcentration factor in Carassius auratus(goldfish). The fishes were exposed to the combined treatment of BPMC, carbaryl and chlorothalonil (0.05 ppm+0.05 ppm+0.005 ppm, 0.05 ppm+0.05 ppm+0.010 ppm, 0.05 ppm+0.10 ppm+0.005 ppm, 0.10 ppm+0.05 ppm+0.005 ppm, 0.10 ppm+0.10 ppm+0.005 ppm) for 3 and 5 days, respectively. BPMC, carbaryl and chlorothalonil in fish and in test water were extracted with n-hexane and acetonitrile. GC-ECD was used to detect and quantitate BPMC, carbaryl and chlorothalonil. 3-day and 5-day bioconcentration factors(BCF$_3$ and BCF$_5$) of each pesticide were calculated from the quantitation results. The depuration rate of each pesticide-from the whole body of fish was determined over the 72-h period after combined treatment.The results were as follows: BCF$_3$ values of BPMC were 4.163, 4.011, 4.122, 4.750 and 4.842 when the concentration of BPMC+ carbaryl+chlorothalonil in combined treatment were 0.05 ppm+0.05 ppm+0.005 ppm, 0.05 ppm+0.05 ppm+0.010 ppm, 0.05 ppm+0.10 ppm+0.005 ppm, 0.10 ppm+0.05 ppm+0.005 ppm and 0.10 ppm+ 0.10 ppm+0.005 ppm. BCF$_5$ values of BPMC were 3.465, 3.270, 3.472, 3.162, 4.227 and 4.157, respectively, under the above conditions. While BCF$_3$ values of carbaryl were 4.583, 4.642, 4.571, 3. 637 and 3.529, respectively, and BCF$_5$ values of carbaryl were 3.932, 3.797, 3.843, 4.293 and 4.132, respectively, under the conditions. While BCF$_3$ values of chlorothalonil were 2.024, 3.532, 2.213, 2.157 and 2.271, respectively, and BCF$_5$ of chlorothalonil were 6.712, 7.013, 6.457, 6.694 and 6.597, respectively, under the conditions. Depuration rate constants of BPMC were 0.019, 0.018, 0.020, 0.022 and 0.021 when the concentration of BPMC+carbaryl+chlorothalonil in combined treatment were the same as above. And depuration rate constants of carbaryl were 0.030, 0.029, 0.030, 0.029 and 0.031, respectively, under the same condition of pesticide mixtures. While depuration rate constants of chlorothalonil were 0.004, 0.004, 0.003, 0.004 and 0.003, respectively, under the same condition. It was observed that no significant differences of BCFs and concentrations of the compounds in fish extracts, test water between combined treatment and single treatment. It was considered that no appreciable interaction at experimental concentrations was due to low concentrations, near environmental level, 0.005-0.1 ppm. Coexistence of BPMC, carbaryl and chlorothalonil had no effect on depuration rate of each pesticide and depuration rate of chlorothalonil was investigated 1/8 and 1/6 slower than those of carbaryl and BPMC in combined treatment. It is similar result in comparison with single treatment. Therefore, it is considered that the persistence of chlorothalonil in fish body would be higher than those of carbaryl and BPMC.

• Journal of Environmental Health Sciences
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• v.23 no.2
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• pp.64-71
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• 1997

This study was performed to investigate the effect of co-existence of carbofuran and chlorothalonil on the short-term bioconcentration factor in Brachydanio rerio(zebrafish). The fishes were exposed to the single and combined treatment of carbofuran and chlorothalonil for 1, 3 and 5 days. Experimental concentrations of carbofuran were 0.05 and 0.10 ppm under the single treatment. And those of chlorothalonil were 0.005 and 0.010 ppm. Experimental concentrations of the combined treatment of carbofuran and chlorothalonil were 0.05 ppm+0.005 ppm, 0.05 ppm+0.010 ppm, 0.10 ppm+0.005 ppm for 1, 3 and 5 days, respectively. Carbofuran and chlorothalonil in fish and in test water were extracted with n-hexane and acetonitrile. GC-ECD was used to detect and quantitate carbofuran and chlorothalonil. 1-day, 3-day and 5-day bioconcentration factors(BCF$_1$, BCF$_3$ and BCF$_5$) of each pesticide were obtained from the quantitation results. The depuration rate of each pesticide was determined over the 24-h period after combined treatment. The results were as follows: Carbofuran did not bioaccumulate in zebrafish under the single and combined treatment for testing periods. BCF$_1$ values of chlorothalonil in concentration of 0.005 and 0.010 ppm under the single treatment were 0.508, 0.621, BCF$_3$ were 1.327, 1.511 and BCF$_5$ were 1.331, 1.597, respectively. BCF$_1$ values of chlorothalonil were 0.512, 0.520 and 0.619, respectively, when the concentration of carbofuran and chlorothalonil in combined treatment were 0.05+0.005, 0.05+0.010 and 0.10+0.005 ppm. BCF$_3$ values of chlorothalonil 1.341, 1.338 and 1.513, respectively, and BCF$_5$ values of chlorothalonil were 1.332, 1.327 and 1.521, respectively, under the above combined treatment. Depuration rate constants of chlorothalonil in concentration of 0.005 and 0.010 ppm under the single treatment were 0.011 and 0.012. Depuration rate constants of chlorothalonil were 0.011, 0.010 and 0.011, when the concentration of carbofuran and chlorothalonil in combined treatment were 0.05+0.005, 0.05+0.010 and 0.10+0.005 ppm. It was observed that no significant difference of carbofuran and chlorothalonil concentration in fish extracts, test water, BCFs and depuration rate constants of carbofuran and chlorothalonil between combined treatment and single treatment. It was considered that no appreciable interaction at experimental concentrations due to lower concentrations than LC$_{50}$. It is suggested that the difference of BCFs between carbofuran and chlorothalonil due to those of fat composition of fish and solubility of carbofuran and chlorothaionil.

• The Korean Journal of Pesticide Science
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• v.17 no.1
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• pp.6-12
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• 2013

Methoxyfenozide and novaluron were sprayed with single and triple treatments separately on peach during cultivation period. Samples were collected over 14 days, 8 times in total (0, 2, 4, 6, 8, 10, 12, 14 days). Methoxyfenozide and novaluron were extracted with acetone and partitioned with dichloromethane, and analyzed by HPLC/DAD. Method Quantitation Limit (MQL) were both 0.005 mg/kg, average recoveries of methoxyfenozide at two fortification levels of 0.05 and 0.25 mg/kg were determined $92.7{\pm}2.9%$ and $102.8{\pm}3.1%$, and novaluron were $98.2{\pm}4.8%$ and $96.7{\pm}9.0%$, respectively. The biological half-life of methoxyfenozide was about 4.41 days at single treatment, and 4.24 days at triple treatments. The biological half-life of novaluron was about 14.81 days at single treatment, and 14.50 days at triple treatments. Dissipation of pesticides on peach was influenced by growth dilution effect. In case of application of methoxyfenozide and novaluron following guidelines on safe use of pesticides, the final residue level was predicted to be lower than Maximum Residue Limit (MRL).

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

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