• Title/Summary/Keyword: 다성분동시분석방법

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Establishment of Simultaneous Analysis Method for the Detection of Multi-Pesticide Residue Used in Golf Courses (골프장 농약 검사를 위한 다성분 동시분석방법 확립에 관한 연구)

  • Yun, Jeong-Ki;Lee, Min-Hyo;Noh, Hoe-Jung;Park, Jong-Gyum;Kim, Hyuk;Kim, Chan-Sub
    • 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.

Comparison of Multi-element Extraction Methods to Determine Available Phosphate and Exchangeable Cations of Korean Soils (토양의 유효태 인산과 치환성 양이온의 다성분동시추출 분석방법 비교)

  • Kim, Myung-Sook;Yang, Jae Eui;Kim, Yoo-hak;Yoon, Jung-Hui;Zhang, Yong-Seon;Kwak, Han-Gang;Ha, Sang-Keon;Hyun, Byung-Keun
    • 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.

Application of the Pesticide Multiresidue Analysis Method for Potatoes and Carrots (감자 및 당근의 개선된 농약 동시다성분 분석법 적용 연구)

  • Kim, Min-Jung;Jung, See-Sub;Park, Jong-Sel;Kim, Jang-Eok;Lee, Young-Deuk;Kim, Jeong-Han;Oh, Chang-Hwan
    • 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.

Multi-residue Analysis of Pesticides using GC-TOF/MS, ECD, NPD with QuEChERS Sample Preparation (QuEChERS 전처리법과 GC-TOF/MS, ECD, NPD를 이용한 잔류농약 다성분분석)

  • Park, Jungwook;Kim, Aekyung;Kim, Jongpil;Lee, Hyanghee;Park, Duckwoong;Moon, Sujin;Ha, Dongryong;Kim, Eunsun;Seo, Kyewon
    • The Korean Journal of Pesticide Science
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    • v.18 no.4
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    • pp.278-295
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    • 2014
  • Fast and accurate multi-residue pesticides inspecting method needs in Agro-Fishery Products Inspection Center. So, We tried to seek the optimum method using GC-TOF/MS, GC-ECD, GC-NPD after QuEChERS sample preparation. In GC-TOF/MS, 138 kinds of pesticide were spiked at 0.3 and $0.5{\mu}g/g$for the identification and quantification in lettuce sample. Recoveries of 77 pesticides were between 70 and 130% with RSD (relative standard deviation lower than 20% at $0.3{\mu}g/g$. In GC-ECD, NPD, 146 kinds of pesticide were spiked for the identification and quantification in lettuce. Recoveries of 61 species were between 70 and 130% with lower than 20%. These results indicated that GC-TOF/MS, GC-ECD, NPD analysis with the QuEChERS sample preparation can be partly applied to multi-residue pesticides in vegetables.

Comparative Study of the Efficiency of GC with Large Volume Injector and SPE Clean-up Process Applied in QuEChERS Method (GC-대용량 주입장치와 SPE를 적용한 QuEChERS 잔류농약 분석법의 효율성 비교)

  • Park, Young Jun;Hong, Su Myeong;Kim, Taek Kyum;Kwon, Hye Young;Hur, Jang Hyun
    • 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%.

고출력 ICP (RF) 열플라즈마 시스템을 이용한 다성분계 나노 복합체 합성

  • Lee, Mi-Yeon;Kim, Jeong-Su;Choe, Chae-Hong;Kim, Min-Ho;Seo, Jun-Ho;Hong, Bong-Geun
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.08a
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    • pp.415-415
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    • 2012
  • ICP (RF) 열 플라즈마 분말 합성법은 초고온 열플라즈마(~10,000 K) 속으로 원료물질을 투입한 뒤, 용융, 기화 및 재합성의 과정을 거쳐 초미분(<1 ${\mu}s$)을 합성하는 방법으로 고출력 시스템의 경우 고온/고 엔탈피 열 유동을 통한 고융점 및 저융점 복합물질의 동시 기화에 의한 물질 조성이 제어된 나노 복합체의 대량 합성이 가능할 것으로 기대되고 있다. 본 연구에서는 전북대학교 고온플라즈마 응용연구센터의 60&200 kW의 고출력 ICP (RF) 열 플라즈마 시스템을 이용하여 LTO (Lithium Titanium Oxide)와 IZTO (Indium Zinc Tin Oxide), Barium Borosilicate Glass (K2O-BaO-B2O3-SiO2)의 다성분계 나노 복합체를 합성하였으며, FE-SEM, TEM, XRD, ICP-OES를 이용하여 그 특성을 분석하였다.

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Comparative Evaluation of the Analytical Methods used to Determine Pesticide Residues in Milk via Dispersive Solid Phase Extraction (Dispersive Solid Phase Extraction을 사용한 우유 내 잔류농약 다성분 동시 분석법 비교연구)

  • Oh, Nam Su;Shin, Yong Kook;Lee, Ji Young;Baick, Seung Chun
    • Journal of Dairy Science and Biotechnology
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    • v.33 no.1
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    • pp.27-34
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    • 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.

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Analytical Method of Multi-Preservatives in Cosmetics using High Performance Liquid Chromatography (HPLC 를 이용한 화장품 중 살균보존제 다성분 동시분석법 연구)

  • Min-Jeong, Lee;Seong-Soo, Kim;Yun-Jeong, Lee;Byeong-Chul, Lee
    • 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.

Simultaneous Determination of Tetracyclines and Sulfonamides Residues in Pork and Flatfish Using Matrix Solid Phase Dispersion (MSPD) Extraction and HPLC (MSPD와 HPLC를 이용한 돼지고기 및 광어 중의 테트라싸이클린계 항생제와 sulfonamide의 다성분 잔류분석법 개발)

  • Gil, Geun-Hwan;Ko, Kwang-Yong;Lee, Yong-Jae;Park, Hye-Jin;Lee, Kyu-Seung
    • Korean Journal of Environmental Agriculture
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    • v.28 no.3
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    • pp.266-273
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    • 2009
  • This study was conducted to develop more convenient simultaneous determination method by matrix solid phase dispersion (MSPD) and HPLC for sulfonamides such as sulfamerazine (SMR), sulfamethazine (SMT), sulfamonomethoxine (SMM), sulfadimethoxine (SDM), sulfaquinoxaline (SQX), and tetracyclines including oxytetracycline (OTC), tetracycline (TC) chlortetracycline (CTC) in prok and flatfish. The limits of detection were 0.047 $mg{\cdot}kg^{-1}$ for OTC, TC, SMR, SMT and SMM, and 0.033 $mg{\cdot}kg^{-1}$ for CTC, SDM, and SQX, respectively. So it is sufficiently possible to detect the eight tetracyclines and sulfonamides under their MRLs ($0.1{\sim}0.2mg{\cdot}kg^{-1}$). The average percentage recoveries of sulfonamides and tetracyclines from pig muscle and flatfish spiked standard solution were approximately $80.25{\sim}101.25%$ and $85.77{\sim}121.42%$, respectively. Therefore this method was efficient for simultaneous analysis of eight tetracyclines and sulfonamides.

Adsorption Column Chromatography for Simultaneous Determination of Multi-pesticide Residues (잔류농약 다성분 동시분석을 위한 흡착 크로마토그래피의 적용)

  • Kim, Chan-Sub;Ihm, Yang-Bin;Choi, Ju-Hyun;Lee, Kyoung-Mi;Lee, Young-Deuk
    • The Korean Journal of Pesticide Science
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    • v.14 no.4
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    • pp.347-360
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    • 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.