• The Korean Journal of Pesticide Science
• /
• v.17 no.3
• /
• pp.162-167
• /
• 2013

An analytical method for the simultaneous determination of pencycuron in agricultural products was established by using GC-NPD. The method was validated through the guidelines of linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy and precision. The calibration curve of pencycuron was linear over the concentration range of 0.02-2 mg/kg with correlation coefficient of above 0.9999. The limits of detection and quantification were 0.005 and 0.02 mg/kg. Mean recoveries of pencycuron for each sample were 79.6-107.5% at the level of 0.02 mg/kg and 86.4-112.1% at the level of 0.2 mg/kg and 84.0- 104.9% at the level of 1 mg/kg. Relative standard deviation (RSD) in recoveries were all less than 5%. The intra- and inter-day precision (RSD) were 1.6-3.0% and 5.3-11.5%, respectively. The result of validation indicated that this method was accurate and sensitive assay.

• The Korean Journal of Pesticide Science
• /
• v.14 no.4
• /
• pp.361-370
• /
• 2010

Considering the efficiencies of the preparation process at each stage obtained in previous studies, the analytical determination method was established for multi-pesticide residues in soils. It consist of the acetone-extraction, the dichloromethane-partition, the Florisil or silica-gel chromatography and the gas chromatography analysis equipped with the electron capture detector and the nitrogen-phosphorus detector. In the soil recovery test by Florisil clean-up system, the number of pesticides recovered in the range of 70~120% and showed less than 20% of RSD were 165 pesticides for paddy soil, 169 pesticides for upland soil and 159 pesticides in both soils through the tested 183 pesticides. And in the soil recovery test by silica-gel system, the number of pesticides recovered in the range of 70~120% and showed less than 20% of RSD were 154 pesticides for paddy soil, 145 pesticides for upland soil, and 134 pesticides in both soils.

• Korean Journal of Environmental Agriculture
• /
• v.30 no.3
• /
• pp.339-345
• /
• 2011

BACKGROUND: Recently in Korea, the import of agricultural products is rising due to the increasing amount of trade. Unregistered pesticides, allidochlor, propachlor, propham, cycloate, diallate and pebulate are widely used as pesticides for rice cultivation in foreign countries, while they are not registered in Korea. Therefore, the residue amount of imported agri-foods should be verified using the proper official analytical method for each of them that has not registered in Korea. METHODS AND RESULTS: This work was conducted to apply the official method of Korea Food & Drug Administration (KFDA) for determining multi class pesticide multiresidues in agricultural commodities. Brown rice and orange which have different characteristics as a matrix were selected as representative samples for residue analysis. The recoveries of cycloate, diallate and pebulate by GC/MS in fortified brown rice and orange with levels of 0.04~0.4 mg/kg were ranged from 82.8% to 110.3%. The quantification limits of three pesticides in brown rice and orange were 0.04 mg/kg. CONCLUSION: As a result, this method can surely be used as an official method for routine analysis of unregistered pesticides in Korea for imported agri-food.

• The Korean Journal of Pesticide Science
• /
• v.4 no.2
• /
• pp.11-17
• /
• 2000

Optimum parameters were investigated for the simultanious analysis of 24 pesticide residuces using gas-liquid chromatography with electron capture detection. Electronic pressure control(EPC) on column enhanced resolution of 24 analyzes. Using DB-17, SPB-608, and Ultra-2 capillary column without EPC incomplete separation was observed in some pairs of pesticides. When EPC function was adopted, no severe overlapping was observed on SPB-608 column in every pesticides except vinclozolin/acetochlor pair. Total running time was 45 min, much shorter than $69{\sim}81$ min when used without EPC. Limit of determination of each analyze ranged $0.1{\sim}12.9$ ng/mL.

• The Korean Journal of Pesticide Science
• /
• v.14 no.4
• /
• pp.347-360
• /
• 2010

In order to develop the multi-residue purification method for 180 pesticides commonly used in Korea, many analytical methods on individual and multi- pesticide residues in the agricultural commodities and food product were examined. Through the modification of adsorption chromatographic methods used in Europe, the United States and Korea, the Florisil and silica-gel chromatographic systems were developed. Through these purification systems, elution profiles for all pesticides were examined. As the results, 145 pesticides were recovered in the range of 70-120% in Florisil clean-up system. The distribution of pesticides in the elution profile was 12 pesticides in the first fraction, 76 pesticides in the second fraction, 81 pesticides in the third fraction, 60 pesticides in the fourth fraction and 30 pesticides in the last fraction. And, in silica-gel system, 137 pesticides were recovered in the range of 70~120%. The distribution of pesticides in the elution profile was 22 pesticides in the first fraction, 59 pesticides in the second fraction, 102 pesticides in the third fraction, 46 pesticides in the fourth fraction and 8 pesticides in the last fraction.

• Korean Journal of Environmental Agriculture
• /
• v.16 no.4
• /
• pp.373-381
• /
• 1997

In order to investigate the drift of pesticides sprayed on Chinese cabbage, 7 pesticides chlorpyrifos, EPN, pirimiphos-methyl, phenthoate, tetradifon, dicofol and bifenthrin were applied in two sets of field tests. The pesticide residues were quantified bar multiple-residue analysis, in which the recovery rate was 78${\sim}$92% and standard deviation was ${\pm}0.683{\sim}52%$. It was found that most of the tested pesticides were spread by drift to neighbouring area and brought about the contamination of the unsprayed crops. The extent of drift varied depending upon the pesticide, distance and wind direction. The mean residue levels on unsprayed crops were 0.66% at 3 meter distance, 0.10% at 6 m distance and 0.05% at 9 m distance from the applied area and the maximum level was 1.83% of the residue on sprayed crops.

• The Korean Journal of Pesticide Science
• /
• v.16 no.3
• /
• pp.242-256
• /
• 2012

QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method has been a lot of research for pesticide analysis, because it is very simple and fast. However, this method requires high sensitivity instrument such as LC-MS/MS because of the use of small sample volume and many impurities compared to the conventional method. So, QuEChERS method needs to be modified for using with HPLC and GC-ECD/NPD. The aim of this work was to study the application of the QuEChERS method as well as its modification for the extraction and preconcentration of 5 groups of 61 pesticides from 4 fruits prior to their determination by HPLC-PDA, GC-ECD/NPD, and LC-MS/MS. The method was validated using spiking levels at 0.1 mg/kg (or 0.01 mg/kg) in apple, grapes, pear and persimmon. The average recovery by QuEChERS AOAC Official 2007. 01 version using the LC-MS/MS varied from 71.1127.4% for 61 pesticides. The average recovery rates using modified QuEChERS varied from 70.9~126% for 61 pesticides by HPLC-PDA and GC-ECD/NPD. The results satisfied the criteria of multiple pesticide residue analysis, setting 70~130% for recovery rates and below 30% for CV.

• Korean Journal of Food Science and Technology
• /
• v.29 no.3
• /
• pp.427-431
• /
• 1997

A simultaneous and rapid gas chromatographic determination of organophosphorus, organo-chlorine, carbamate, and pyrethroid pesticides in polished rice was developed. The pesticides were extracted from samples with acetone by automated soxhlet apparatus and this extract was evaporated to dryness. The residue was dissolved in hexane, the solvent was applied to a Sep-Pak florisil catridge, was eluted with 50% ethyl acetate in n-hexane, and was injected to dual GC-ECD/NPD system. This simple method affords a high recovery of hydrophilic pesticides, allows rapid analysis, and is cheap to perform. Except for dichlorvos and captan, recoveries of 46 pesticides were over 60%.

• Korean Journal of Food Science and Technology
• /
• v.36 no.6
• /
• pp.863-871
• /
• 2004

Analyses of residual pesticides in raw materials used for dietary supplements were performed using multi-ingredients simultaneous analysis method. Pesticides such as BHC, chlorpyrifos, and quintozene were detected in 12 domestic and 7 imported samples, suggesting need for monitoring pesticides in domestic and imported raw materials and establishing residual limit of each pesticide.

• Journal of Dairy Science and Biotechnology
• /
• v.33 no.1
• /
• pp.27-34
• /
• 2015

The aim of this study was to optimize a simple, fast, and economic analytical method for the simultaneous determination of various pesticides (aldrin, p,p'-DDT, o,p'-DDT, p,p'-DDE, ${\alpha}$-endosulfan, ${\beta}$-endosulfan, dieldrin, heptachlor, permethrin, chlordane, deltamethrin, diazinon, bifenthrin, methoprene, propargite, fenpropathrin, cypermethrin, fenvalerate, and fenpropathrin) in milk by using dispersive solid phase extraction (SPE). In this study, two different extraction methods (low temperature cleanup and liquid-liquid partitioning), which were followed by a cleanup process based on dispersive-SPE, were evaluated and compared for the 19 pesticides. The results for all the pesticides were determined by gas chromatography mass spectrometry (GC/MS) with selected-ion monitoring mode, and the matrix effect of the method was evaluated. Comparison of these approaches yielded higher and more consistent recoveries of most pesticides at fortification levels of $1{\mu}g/mL$ using low-temperature fat precipitation, followed by cleanup process based on dispersive-SPE with PSA and C18 as sorbents, than other preparation process. The relative standard deviation was <20 % and the combination of this method were very effective for the cleanup.