• Journal of Soil and Groundwater Environment
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• v.11 no.4
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• pp.18-24
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• 2006

The possibility of multiresidue analysis of 24 pesticides out of 30 residual pesticides which are subjected to test in the golf courses was examined. The utility of multiresidue method for pesticide residue test was evaluated by recovery test through a standard addition method of pesticides in water, soil, and lawn grass. The experimental results of the recovery test for individual pesticides are as follows : The number of pesticide of which average recovery rate was over 70% regardless of media was 16 pesticides. These pesticides were composed of 8 organophosphorus pesticides (chlorpyrifos, chlorpyrifosmethyl, diazinon, EPN, fenitrothion, phenthoate, phosalone, and toclofos-methyl). 4-organochlorinated pesticides (daconil, captan, endosulfan, and tetradifon), 2-pyrethroid pesticides(fenpropathrin, lambda-cyhalothrin) and 2 other pesticides (bromopropylate, pendimethalin). On the other hand, in case of dicofol, average recovery rate was over 70% for water and lawn grass but only 53.3% for soil. Therefore, the multiresidue method applied in this experiment is not appropriate for analysis of dicofol in soil. Furthermore, among 7 pesticides, 2 pesticides(amitraz and pyraclofos) showed that theirs average recovery rate deviated from criteria($70{\sim}130%$) in almost ail media, while 5 pesticides(bensulide, deltamethrin, iprodione, phosphamidon and tralomethlin) were not detected from all media by GC/NPD or GC/ECD.

• The Korean Journal of Pesticide Science
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• v.9 no.4
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• pp.311-315
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• 2005

The simultaneous or consecutive product analysis is needed for quality control because the various items are produced in pesticide manufacturer. This study was conducted to establish a multi-pesticide analysis making possible to analyze several active ingredients with one injection of mixed active ingredients under same instrument-condition in the cause of quality control with accuracy and speed. The test was conducted with 3 pesticides, iprobenfos 17%GR, isoprothiolane 12%GR, tebufenozide 20%SC and performed by GLC and HPLC. With the GLC method, 2 active ingredients of iprobenfos and isoprothiolane were analyzed but tebufenozide was not detective simultaneously. With the HPLC method, all of the active ingredients in those three pesticides were simultaneously analyzed in this study.

• Analytical Science and Technology
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• v.9 no.2
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• pp.1033-1060
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• 1996

• The Korean Journal of Pesticide Science
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• v.20 no.2
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• pp.104-127
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• 2016

A new analytical method has been developed to determine 320 pesticides in apple and rice. The extraction of pesticides was carried out based on QuEChERS sample extraction, and determination was performed using LC-MS/MS and GC-MS/MS. 320 pesticides were selected for experiments. 251 and 110 pesticides among them were analysed by LC-MS/MS and GC-MS/MS, respectively. 41 pesticides of them were analyzed by both GC-MS/MS and LC-MS/MS. Among pesticides analysed by LC, 242 pesticides (96% of total number) in apple and 237 pesticides (94% of total number) in rice showed recoveries in the range of 70~120% with RSD ${\leq}20%$. In case of pesticides analyzed by GC-MS/MS, 103 pesticides (94% of total number) in apple and 83 pesticides (76% of total number) in rice were successfully validated. These results indicated that LC-MS/MS and GC-MS/MS analysis with the QuEChERS sample preparation can be partly applied to multi-residue pesticides in agricultural products.

• 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.13 no.3
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• pp.133-147
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• 2009

In order to develop the simultaneous analytical method for pesticide residues which ones in soil are rapidly and inexpensively measured by, many analytical methods for individual pesticide residue and several methods for multi-pesticide residues in agricultural commodities and food were reviewed. Various gas chromatographic conditions and pre-treatment procedures were intensively investigated and modified. And then new optimum procedure was established and its proficiency was validated. The response on detectors of simultaneous determination of 180 pesticides out of pesticides used in Korea was tested. The number of pesticides that their limits of detection (LOD) equal or lower than $0.05\;mg\;kg^{-1}$ were 137 pesticides on ECD, 170 pesticides on NPD and 179 pesticides on ECD/NPD integrated. The retention times of most pesticides ranged appropriately between 10 minutes and 40 minutes in the proposed chromatographic conditions. But about 90 pesticides eluded between 20 minutes and 30 minutes and so they were not resolved enough. In partition with dichloromethane, ethyl acetate/hexane (1:1) and ethyl acetate, number of pesticides whose extraction efficiency ranged from 70% to 120%, were 163, 154 and 147, respectively.

• Korean Journal of Environmental Agriculture
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• v.31 no.3
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• pp.277-285
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• 2012

BACKGROUND: For safety evaluation of imported agri-food in Korea, the multiresidue analysis method was establised for unregistered organophosphorus pesticides, aspon, chlorthion, chlorthiophos, crotoxyphos, demeton-O, demeton-S, demeton-S-methyl, dioxathion, heptenophos, iodofenphos, leptophos, methyl-trithion, propetamphos and sulfotep. METHODS AND RESULTS: The used method for multiresidue analysis in brown rice and orange used as representative samples of imported agri-food was the official method of Korean Food and Drug Administration. The results of validation test of 13 organophosphorus pesticides except crotoxyphos for multiresidue analysis method are compared to the criteria such as specificity, linearity, accuracy, precision and limit of quantification. CONCLUSION: The used method for multiresidue analysis of unregistered 13 organophosphorus pesticides except crotoxyphos in Korea can surely be used as an official method for routine analysis of imported agri-food.

• The Korean Journal of Pesticide Science
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• v.19 no.4
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• pp.370-393
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• 2015

This study was conducted to compare STQ method, multi-residue method in Korean food code and QuEChERS method for validated selected and accuracy, reproducibility and efficiency. A total of 45 selected and targeted pesticides were the analyzed by GC and 5 of them were crops (apple, potato, green pepper, rice, soy bean). $R^2$ values were calculated in the standard calibration curve was over 0.990. Recovery tests were performed by three replications in two levels and the relative standard deviation of the repeated experiments was less than 30%. The average percentage of recoveries in the multi-residue method in Korean food code was 89.13%, QuEChERS method was 92.45% and STQ method was 85.28%. In addition, matrix effects in multi-residue method in Korean food code was 24.61%, QuEChERS method was 23.98% and STQ method showed 11.24%. The STQ method is easy and showed high clean-up effect in extracting the sample solution than the QuEChERS method and clean-up with C18, PLS, PSA cartridge columns. A large volume of the sample was injected in order to compensable for the problem, that occurred due to high detection limit in the analyser. When the STQ method was applied using a large volume injector, the standard calibration curve showed a higher linearity $R^2=0.990$, and method detection limit was 0.01 mg/kg. It showed an average recovery of 91.84% and the relative standard deviations of three replications repeated in two level process was less than 30% and had an average matrix effect of 17.90%.

• Environmental Analysis Health and Toxicology
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• v.17 no.3
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• pp.265-272
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• 2002

This study was carried out with the detection for multiresidue of the organophosphorus pesticides such as malathion, parathion. diazinon, and carbamate pesticide such as carbaryl, by enzyme-inhibition method. The acetylcholinesterase (AChE) and cholinesterase (ChE) activities in chicken brain determined by the Ellman's method were 166.6 and 5.8 $\mu$mol/min/g protein, and in chicken plasma were 23.1 and 8.3 $\mu$mol/min/g protein, respectively. The optimum pH of AChE and ChE was 8.2 and 7.8, respectively. The Km of AChE and ChE was 0.034 and 0.045 mM, respectively. I$\_$50/ for AChE and ChE by some organophosphorus was 55.82 and 99.42 mg/L of malathion, 31.16 and 29.13 mg/L of parathion, and 17.89 and 19.62 mg/L of diazinon, respectively. I$\_$50/ for AChE and ChE by carbaryl of carbamate was 0.10 and 0.05 mg/L, respectively. The 0.07 mg/L of drinking water advisory level for carbaryl could be detected with I$\_$50/ of AChE and ChE. Enzyme-Inhibition (EI) method with AChE and ChE was used the multiresidue method to detect the 1 mg/L of the carbamate pesticides.

• The Korean Journal of Pesticide Science
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• v.19 no.3
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• pp.161-173
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• 2015

The multiresidue method 4.1.2.2 in Korea Food Code was extended for the analysis of 24 unregistered pesticide residues. The method includes acetonitrile extraction, liquid-liquid partition, Florisil SPE clean-up and GC analysis. The limits of quantification (LOQ) range of the method was 0.02~0.05 mg/kg for orange, brown rice and banana. The linearity for targeted pesticides were $R^2$ > 0.99 at the level ranged from 0.05 to 5 mg/L. Recovery test was performed at two concentration levels of LOQ and 4~10 times of LOQ. Recoveries and relative standard deviations (RSDs) of target pesticides were acceptable, showing 70~120% range and less than 20%, respectively, except for ethiprole, picloram and sulcotrion. This method is effectively applicable to routine analysis of target pesticides in orange, brown rice and banana.