• 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.

• 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.

• 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 Soil Science and Fertilizer
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• v.42 no.3
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• pp.192-200
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• 2009

Soil testing is one of the best management practices for sustainable agriculture. Recently, as increasing soil testing needs, simplification of soil analytical procedure has been required. To determine recommendable multi-element extractant, the soil testing results of available phosphate and exchangeable cations between the conventional methods (Lancaster and 1M $NH_4OAc) and multi-element extraction methods such as Mehlich III, Modified Morgan and Kelowna methods were compared. There were highly significant correlation between the conventional methods and multi-element extraction methods (Mehlich III, Modified Morgan and Kelowna) for available phosphate and exchangeable K, Ca, Mg and Na. The coefficients of determination ($R^2) between available phosphate extracted by Lancaster method and multielement extraction methods were in the order of Mehlich III ($0.979^{***}$) > Kelowna ($0.977^{***}$) > Modified(Mod.). Morgan ($0.553^{***}$). For exchangeable cations, there were highly significant correlations between 1M $NH_4OAc method and Mehlich III, Mod. Morgan and Kelowna. However, exchangeable K, Ca and Mg by Mehlich III method were more highly correlated with conventional method than other methods. Therefore, Mehlich III extraction method could be recommended as a single extractant for simultaneous measurement using ICP in the analysis of avaliable phosphate and exchangeable cations.

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

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

• Journal of the Society of Cosmetic Scientists of Korea
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• v.48 no.4
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• pp.321-330
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• 2022

This study attempted to establish an optimal multi-compound simultaneous analysis method that can secure reliable results for 15 - preservatives, 2 - sun screens and 1 - antioxidants of cosmetics using HPLC-PDA. Since the potential of hydrogen (pH) in the mobile phase affects the acid dissociation constant (pKa) of the preservatives, and the peak retention time shift and area change were observed. The peak separation condition was established by adjusting the pH to 0.1% H₃PO₄ addition (mL) when preparing the mobile phase. As a results of method validation, the linearity correlation coefficient (R²) of above 0.999 were obtained, and accuracy 87.9 ~ 101.1%, 0.1 ~ 7.6% precision for two types of cosmetics (cream and shampoo). It was found that the limit of detection (LOD) was 0.1 ~ 0.2 mg/kg and the limit of quantitation (LOQ) was 2.0 ~ 4.0 mg/kg. In addition, it was possible to simultaneously separate p-anisic acid, a natural compound that was difficult to separate in HPLC due to the small difference from methylparaben, a synthetic preservatives. Through this study, it will be effectively used to secure quality control and safety for compound that need restrictions on use cosmetics.

• Korean Journal of Food Science and Technology
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• v.37 no.2
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• pp.304-307
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• 2005

Multiresidue method was set up for the simultaneous determination of various residual pesticides in potatoes and carrots, which was analyzed by gas chromatography-electron capture detector/nitrogen phosphorus detector. Method consisted with acetone/acetonitrile (9 : 1) extraction and dichloromethane partition, followed by florisil cartridge purification with hexane/dichloromethane/acetonitrile (50 : 45 ; 5) elution. Among 197 pesticides (194 kinds) spiked to food materials, 143 and 155 pesticides were recovered over 70% on potatoes and carrots, respectively. Nineteen pesticides including bromacil, cyproconazole, were not detected in water and sample matrices. Matrix components may affect the low detections of 25 pesticides such as benfuracarb, bitertanol from potatoes and 16 pesticides such as bitertanol, carbosulfan from Carrots. Some pesticides including dichlobenil, fluoroimide and iprodione were highly detected from one or both matrices even though they were not detected from water.