• The Korean Journal of Pesticide Science
• /
• v.18 no.2
• /
• pp.79-87
• /
• 2014

Pyriofenone is an aryl phenyl ketone fungicide that is newly registered in Korea in 2013 to control powdery mildew on food. The objective of this study was to develop reliable and sensitive analytical method for determination of pyriofenone residue in agricultural products for ensuring the food safety. The pyriofenone residues in all samples(Korean melon, pepper, potato, mandarin, soybean, and hulled rice) were extracted with acetonitrile, partitioned with dichloromethane, and then purified with a silica cartridge. The purified samples were analyzed by HPLC-UVD and confirmed with LC-MS. The linear range of pyriofenone was 0.05~5 mg/kg with the correlation coefficient ($r^2$) > 0.999. Average recoveries of pyriofenone ranged from 72.8% to 99.5% at the spiked level of 0.05 and 0.5 mg/kg, while the relative standard deviation was 2.3%~6.4%. In addition, the limit of detection and limit of quantification were 0.01 and 0.05 mg/kg, respectively. The results revealed that the developed and validated analytical method was suitable for pyriofenone determination in agricultural products.

• The Korean Journal of Pesticide Science
• /
• v.8 no.3
• /
• pp.184-188
• /
• 2004

The residue analysis of the insecticide thiodicarb in sweet persimmon was analyzed with a gas chromatograph equipped with nitrogen phosphorus detector(NPD) to evaluate efficacy of analysis method and safety of thiodicarb in persimmon. Minimum detectable amount of methomyl oxime, hydrolysate of thiodicarb, was 0.2 ng and detection limit of thiodicarb was 0.05 ppm. The mean recoveries evaluated from untreated samples spiked at 0.5 ppm and 2.5 ppm were $93.9{\pm}3.9$ and $92.8{\pm}2.0%$, respectively. When thiodicarb was sprayed onto the sweet persimmon two times until 40 and 30 days before harvest, three times until 40, 30 and 21 days before harvest, and four times until 40, 30, 21 and 14 days before harvesting, the mean residual amount in sweet persimmon were $1.50{\pm}0.04$, $1.86{\pm}0.04$ and $2.11{\pm}0.12$ ppm, respectively. It would be safe when thiodicarb 40% WP is treated four times 14 days before harvesting to control fruit moth in sweet persimmon.

• 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.

• The Korean Journal of Pesticide Science
• /
• v.21 no.1
• /
• pp.17-25
• /
• 2017

Dissipation pattern and biological half-lives of fungicides boscalid and pyraclostrobin were calculated on jujube. The pesticides were sprayed on jujube in two different field at the standard rate, respectively. The raw agricultural commodities were harvested at 0 (2 hr), 1, 3, 5, 7, 10 and 14 days after treatment, and analyzed by HPLC/DAD. The method limit of quantification (MLOQ) was $0.02mg\;kg^{-1}$ for boscalid and pyraclostrobin. The recovery ranged 101.8~109.3% with below 5% of CV (Coefficient of variation) for boscalid and 104.2~115.4% with below 5% of CV for pyraclostrobin. An average initial deposit at field 1 and field 2 samples were observed 0.40 and $0.48mg\;kg^{-1}$ for boscalid and, 0.76 and $0.57mg\;kg^{-1}$ for pyraclostrobin, respectively. The biological half-lives of field 1 and field 2 were 11.0 and 13.2 day for boscalid, and 6.1 and 12.7 days for pyraclostrobin.

• Horticultural Science & Technology
• /
• v.34 no.1
• /
• pp.183-194
• /
• 2016

This experiment was conducted to establish an official determination method to measure fluazinam residue in horticultural crops for import and export using GC-ECD/MS. Fluazinam residue was extracted with acetone from fresh samples of four representative horticultural products, the vegetable crops green pepper and kimchi cabbage, and the fruit crops mandarin and apple. The acetone extract was diluted with saline water and n -hexane partitioning was used to recover fluazinam from the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fluazinam was separated and quantitated by GC with ECD using a DB-17 capillary column. The horticultural crops were fortified with three different concentrations of fluazinam. Mean recoveries ranged from 82.5% to 99.9% in the four crops. The coefficients of variation were less than 10.0%. The quantitative limit of fluazinam detection was $0.004mg{\cdot}kg^{-1}$ in the four crop samples. GC/MS with selected-ion monitoring was also used to confirm the suspected residue. This analytical method was reproducible and sensitive enough to measure the residue of fluazinam in horticultural commodities for import and export.

• Journal of Environmental Science International
• /
• v.15 no.4
• /
• pp.293-304
• /
• 2006

Sea water samples collected in August, 1994 from 20 stations in the Kwangyang Bay were analyzed by gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) to investigate persistence and distribution pattern of four organophosphorus pesticides (DDVP, Diazinon, IBP, EDDP). Except for IBP, the contamination by DDVP, Diazinon, and EDDP in marine aquatic environment in Korea has not been reported previously. In this study, however, all these four pesticides were detected in all stations (except DDVP) and their concentrations were in ng/L level. The concentrations ranged from detection limit to 15.3ng/L for DDVP, 1.8-27.7ng/L for Diazinon, 7.3-63.5ng/L for IBP, and 22.2-1100.1ng/L for EDDP. It is noteworthy that the measured concentrations of IBP and EDDP in this study would be much lower than usual, since the use of IBP and EDDP was less than 50% of average annual consumption due to unusually dry and hot weather condition in the summer of 1994. It was very surprising to find that the highest concentrations of organophosphorus pesticides were observed at stations near Daesa Streamlet instead of Seomjin River, which has more point source of the pesticides. This result suggests that the small river discharge during heavy ram period in summer can give harmful effect on marine biota (both wild and aqua-cultured) with its organophosphorus pesticide residue, despite of their short residence time in aquatic environment. In order to protect the marine life properly from acute toxicity of the organophosphorus pesticides, it needs to be emphasized that monitoring the level of agricultural pesticides in river run-off should be done during active consumption period rather at regular intervals.

• Korean Journal of Environmental Agriculture
• /
• v.39 no.2
• /
• pp.142-169
• /
• 2020

BACKGROUND: A new analytical method has been developed to determine 261 pesticide residues in herbal medicines. METHODS AND RESULTS: The extraction of pesticides was carried out by modified method of the Korea Food Standards Codex sample extraction and determination was performed using GC-MS/MS and LC-MS/MS. During the pre-treatment process of the test method, Solid-liquid separation was changed to centrifugation. The method was validated by the precision and accuracy results. 261 pesticides spiked at three level 20, 50, 100 ug/kg in herbal medicines. The limit of quantification of method were 4-40 ug/kg for GC-MS/MS and 2-45 ug/kg for LC-MS/MS, respectively. Among the pesticides analysed by GC-MS/MS and LC-MS/MS, 244 pesticides (94% of total number) in chinese matrimony vine and 224 pesticides (86% of total number) in korean angelica root and 231 pesticides (89% of total number) in jujube and 214 (82% of total number) in cnidium showed recoveries in the range of 70-120% with RSD⪯20%. CONCLUSION: These results indicated that GC-MS/MS and LC-MS/MS analysis with the sample extraction in this study can be applied to multi-residue analysis of pesticides in herbal medicines.

• Korean Journal of Environmental Agriculture
• /
• v.40 no.2
• /
• pp.99-107
• /
• 2021

BACKGROUND: Pesticide uptake by a rotational crop after being used for the primary crop is a potential cause of violation against the pesticide law if the pesticide is not registered in the secondary crop. This study was conducted to investigate the plant back interval (PBI) of fluopyram for the rotational cultivation of radish. METHODS AND RESULTS: Two experimental approaches were performed the evaluation of residues in radish cultivated successively in soil 16 days after treated with fluopyram onto pepper plant (T1) and in radish cultivated in bare soil treated with fluopyram at PBI 30 and PBI 60 days (T2). A modified QuEChERS method coupled with LC/MS/MS analysis showed good linearity of matrix-matched standard calibration of fluopyram with the coefficient values of determination greater than 0.995. Recovery values at levels of 0.01, 0.05, 0.1 and 0.25 mg/kg ranged from average 84.9 to 117.6% with RSD less than 10%. Fluopyram residues in radish harvested from T1 and T2 were found as levels less than maximum residue limit. CONCLUSION: This study suggests 20~30 days as the PBI of fluopyram for the rotational cultivation of radish in the greenhouse soil treated with fluopyram used for pepper as the primary crop.

• Korean Journal of Environmental Agriculture
• /
• v.41 no.4
• /
• pp.261-275
• /
• 2022

BACKGROUND: Prior to implementing a positive list system (PLS), there is a need to establish acceptable daily intake (ADI) and maximum residue limit (MRL) for veterinary drugs that have been approved a few decades ago in South Korea. On top of that, chronic dietary exposure assessment of veterinary drug residues should be performed to determine whether the use of these veterinary drugs would cause health concerns or not. METHODS AND RESULTS: To establish the ADI, the relevant toxicological data were collected from evaluation reports issued by international organizations. A slightly modified global estimate of chronic dietary exposure (GECDE) model was employed in the exposure assessment owing to the limited residual data. Therefore, only the ADI of ephedrine was established due to insufficient data for the other veterinary drugs. Thus, instead of ADI, the threshold of toxicological concern (TTC) value was used for the other drugs. Lastly, the hazard index (HI) was calculated, except for etizazole hydrochloride, due to the potential of mutagenicity. CONCLUSION(S): The HI values of ephedrine, menichlopholan, and anacolin were found to be as high as 6.4%, suggesting that chronic dietary exposure to the residues from these uses was unlikely to be a public health concern. Further research for exposure assessment of veterinary drug residues should be performed using up-todate Korean national health and nutrition examination survey (KNHANES) food consumption data. In addition, all relevant available data sources should be utilized for identifying the potentials of toxicity.

• The Korean Journal of Pesticide Science
• /
• v.16 no.2
• /
• pp.131-136
• /
• 2012

This study was carried out to elucidate residual characteristics of azoxystrobin and difenoconazole in fresh ginseng. Test pesticides were sprayed onto ginseng both in 2009 for 3-year-old ginseng and in 2010 for 4-year-old ginseng according to their pre-harvest intervals (PHIs). Limit of quantitation (LOQ) of both azoxystrobin and difenoconazole was 0.003 mg/kg. Analytical methods set up for the test pesticides were considered to be suitable for the analysis of their residues in fresh ginseng, considering that their recoveries ranged from 87.58 to 112.79%. Concentration of azoxystrobin in 3-year-old ginseng ranged from 0.004 to 0.011 mg/kg and that in 4-year-old ginseng ranged from 0.007 to 0.016 mg/kg. Amounts of difenoconazole in 3- and 4-year-old ginsengs were from 0.003 to 0.007 and from 0.007 to 0.01 mg/kg, respectively, representing no accumulation effect observed in residue amount between them.