• Title/Summary/Keyword: GC/ECD

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Determination of residual pesticides in crude drugs - Gas chromatographic Analysis of 18 pesticides - (한약재중의 잔류농약 분석 - GC에 의한 18종 잔류농약의 분석 -)

  • Hwang, In-Sook;Choi, Byung-Hyun;Bae, Chong-Ho;Kim, Myung-Hee;Cho, Hae-Jeon
    • Korean Journal of Pharmacognosy
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    • v.32 no.3 s.126
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    • pp.200-211
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    • 2001
  • This study was carried out to determine the 11 organochlorine, 7 organophosphorus residual pesticides in 251 crude drugs. These residual pesticides in herbal drugs were extracted with acetonitrile and the extracts were cleaned up via LC-florisil solid phase extraction column. The prepared samples were assayed for pesticide residues using GC-ECD, NPD with capillary column and identified by GC-MSD. Recoveries were $63.9{\sim}111.5%$ in the organochlorine pesticides and $69.8{\sim}92.4%$ in the organophosphorus pesticides, and detection limits were $0.001{\sim}0.65\;ppm$ in the organochlorine pesticides and $0.0009{\sim}0.0074\;ppm$ in the organophosphorus pesticides. Pesticide residues were detected in 9 cases.

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Discrimination of Ginseng Habitat by Using Instrumental Analysis Techniques

  • Sohn H. J.;Lee S. K.;Cho B. G.;Kim S. J.;Lee N. Y.;Choi D. S.;Jeong M. S.;Bae H. R.;Yang J. W.
    • Proceedings of the Ginseng society Conference
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    • 2002.10a
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    • pp.238-252
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    • 2002
  • In order to screen out indicators for the discrimination of ginseng habitat, some physical and chemical characteristics of Korean red ginsengs (94 kinds) and Chinese red ginsengs (50 kinds) were analyzed by using a rheometer, an electronic nose system, a combined technique of solid phase micro-extraction (SPME) and gas chromatograph equipped with an electron capture detector (GC/ECD), an X-ray fluorescence spectrometer (XRF), an inductively coupled plasma mass spectrometer (ICP/MS), a near infrared spectrometer (NIRs) and high performance liquid chromatography equipped with evaporative light scattering detector (HPLC/ELSD). The results are summarized as follows: (i) The rhizome strengths of Korean red ginsengs were significantly higher than those of Chinese red ginsengs. (ii) The electronic nose patterns of Korean red ginsengs were significantly different from those of Chinese red ginsengs. (iii) Some unidentified peaks were detected not in the headspace of Korean red ginsengs but in the headspace of Chinese red ginsengs when the headspace volatiles prepared by the SPME technique were analyzed by GC/ECD. (iv) Either the content ratios of K to Ca or Mn to Fe were significantly different between Korean red ginsengs and Chinese red ginsengs. (v) The reflectance ratios of NIRs wavenumbers such as $904\;cm^{-1}\;to\;1088\;cm^{-1}$ for Korean red ginsengs were significantly different from those for Chinese red ginsengs. (vi) The content ratios of ginsenoside-Rg to ginsenoside-Re of Korean red ginsengs were significantly higher than those of Chinese red ginsengs. These results indicate that the rhizome strength, the electronic nose pattern, the occurrence of ECD-sensitive headspace volatile components, the content ratios of K to Ca and Mn to Fe, the NIRs pattern and the content ratio of ginsenoside-Rg to -Re may be indicators for the discrimination of ginseng habitat.

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Gas Chromatographic Analysis of TDI, MDI and HDI Using 2-Chlorobenzyl Alcohol and 2,4-Dichlorobenzyl Alcohol Derivatives (2-클로로벤질 알코올 및 2,4-디클로로벤질 알코올 유도체를 이용한 TDI, MDI 및 HDI의 가스크로마토그래피 분석)

  • Yun, Ju-Song;Park, Jun-Ho;Lee, Kang-Myoung;Choi, Hong-Soon;Cho, Young-Bong;Koh, Sang-Baek;Cha, Bong-Suk
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.16 no.3
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    • pp.222-232
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    • 2006
  • Objectives: The objective of this study was to propose the total isocyanate analytical method which involves derivation of 2,4-toluene diisocyanate(2,4-TDI), 2,6-toluene diisocyanate(2,6-TDI), 4,4'-methylenediphenyl diisocyanate(4,4'-MDI) and 1,6-hexamethylene diisocyanate(1,6-HDI) using 2-chlorobenzyl alcohol(2-CBA) or 2,4-dichlorobenzyl alcohol(2,4-DCBA), and analyzing of hydrolysate of the synthesized urethane with the gas chromatography(GC)/flame ionization detector(FID), GC/pulsed discharge ionization detector-electron capture detector(PD-ECD) and GC/mass selective detector(MSD). Methods: Urethanes were synthesized by reacting 2,4-TDI, 2,6-TDI, 4,4'-MDI and 1,6-HDI to 2-CBA or 2,4-DCBA. Urethanes was verified by TLC, HPLC/UVD and GC/MSD. For field application, the most suitable condition that 2-CBA coated in glass fiber filter removed completely and urethanes were not removed was searched. 2-CBA generated from hydrolysis of urethanes according to hydrolysis conditions. Diisocyanates were collected on field air and analyzed. Results: Urethanes which were white and solid phase synthesized by reacting 2,4-TDI, 2,6-TDI, 4,4'-MDI, 1,6-HDI and 2-CBA or 2,4-DCBA. And urethanes were verified by TLC, HPLC/UVD and GC/MSD. The most suitable conditions to remove 2-CBA coated in glass fiber filter were $87^{\circ}C$ and 20 mmHg and urethanes were not removed under same condition. Hydrolysis yields of urethanes were 99 % to 111 %. 2-CBA, the hydrolysate of urethanes was analyzed by GC/FID, GC/PD-ECD and GC/MSD. Conclusions: Simultaneous analysis of 2,4-TDI, 2,6-TDI, 4,4'-MDI and 1,6-HDI deriving with 2-CBA and 2,4-DCBA, along with a total isocyanate analysis, was feasible with GC/FID, GC/PD-ECD and GC/MSD. This result will be a guide of further study on total isocyanate analysis.

Residual Pattern of Pesticide, Chlorfluazuron in Perilla Leaves Under Plastic House (들깻잎 재배 중 chlorfluazuron의 잔류량 변화 및 잔류분석법 시험)

  • Lee, Min-Ho;Kim, Seok-Ho;Park, Young-Guin;Jo, Gyeong-Yeon;Shin, Byung-Gon;Kim, Jong-Han;Kwon, Chan-Hyeok;Sohn, Jae-Keun;Kim, Jang-Eok
    • The Korean Journal of Pesticide Science
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    • v.11 no.2
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    • pp.106-116
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    • 2007
  • Pesticide, chlorfluazuron was subjected to determine the safety of terminal residues at the harvesting date of perilla leaves cultivated in plastic house. After the pesticide applied on a foliar spray in 2005 and 2006, leaf persistence of its residue was analysed for 10 days before leaf harvest. The degradation rate of chlorfluazuron in the leaf was 32.3 %(standard application), 43.6 %(double application) and 78.0 %(standard), 80.4 %(double) at second and tenth day, respectively, under analysis of GC/ECD in 2005. The degradation rate of chlorfluazuron in the leaf was 33.1 %(GC/ECD analyze), 34.0 %(HPLC/UVD analyze) and 77.9 %(GC/ECD), 78.4 %(HPLC/UVD) at second and tenth day, respectively, under the standard level of pesticide in 2006. The biological half-life of the chlorfluazuron residue was estimated by the regression equation calculated from daily dissipation of pesticide in the perilla leaves. The longest half-life of the chlorfluazuron residue in perilla leaves was 5.5 days. The maximum residual limit(MRL) for chlorfluazuron based on the longest half-life was estimated 2.0ppm at harvesting day, 2.5ppm at second day and 7.1ppm at tenth day before leaf harvesting of perilla.

Simultaneous Analysis of Pesticide Priority Pollutants in Soil (토양 중의 Pesticide Priority Pollutants 동시 분석에 관한 연구)

  • Lee, Seung-Seok;Park, Young-Joo;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.8 no.3
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    • pp.237-248
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    • 1995
  • The simultaneous analysis of 16 organic pesticides, which are listed as a part of 129 priority pollutants by EPA(Environmental Protection Agency), was performed by GC-ECD(electron capture detector) and GC/MS-SIM(selected ion monitoring). Two extraction procedures from SW-846, sonication extraction and Soxhlet extraction, were somewhat modified and compared as an extraction and concentration method for the analysis of priority pollutants in soil. Accuracy and precision of the methods were reported from the calculation of mean recovery, mean relative standard deviation, and method detection limit.

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PYE [2-(1-pyrenyl)ethyldimethylsilylated silica] Column HPLC and HR-GC-(micro) ECD in the Accurate Determination of Toxic Co-planar PCBs and Polybrominated Diphenyl Ethers (PBDEs)

  • Kannan, Narayanan;Hong, Sang-Hee;Oh, Jae-Ryoung;Yim, Un-Hyuk;Li, Donghao;Shim, Won-Joon
    • Bulletin of the Korean Chemical Society
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    • v.26 no.4
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    • pp.529-536
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    • 2005
  • Measurement of toxicologically relevant polychlorinated biphenyl (PCB) congeners such as non-ortho(IUPAC#) 77, 81, 126, 169 and mono-ortho 105, 114, 118, 123, 156, 157, 189 and di-ortho 170, 180 and polybrominated diphenyl ethers (PBDEs) such as 47, 66, 85, 99, 100, 138, 153, 154 in environmental samples become almost mandatory in several countries now. However, most of the available methods involve expensive instrumentations such as HRGC-HRMS or ECNI-LRMS, apart from expensive extraction and clean-up (with large volume of solvents) steps. A method has been devised combining the analytical separation power of PYE [2-(1-pyrenyl)ethyldimethysilylated silica] column HPLC and high-resolution gas chromatographic techniques including micro-electron capture detection (ECD) and two dimensional gas chromatograpy-ECD techniques to determine these eco-toxic substances at parts-per-trillion (ppt) levels. This combination resolves co-elution of congeners that occur in disproportionate ratios (e.g. CB-110 and -77) and allows accurate congener-specific determination of target compounds. This method is cost effective as it requires only hexane, that in small quantities (10 mL) and GC-ECD. The elution and analysis time are optimized to less man hours. This method is effectively utilized in the analysis of co-planar PCBs and PBDEs from archived solvent extracts of samples previously analyzed for pesticides and PCBs. Structure based separation of contaminant classes improves GCECD determination at ppt levels.

Gas Chromatographic Analysis on Residual Concentration and Half-life Time of Cyfluthrin in Potato and Soil (감자와 토양 중에서 Cyfluthrin의 잔류농도와 반감기에 대한 기체 크로마토그래피 분석)

  • Han, Seong Soo;Jeong, Seung Il;Chun, Hyun Ja;Hoang, Geun Chang;Kim, Il Kwang
    • Analytical Science and Technology
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    • v.13 no.6
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    • pp.722-730
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    • 2000
  • The residual concentration and half-life time of synthetic pyrethroid insecticide cyfluthrin in potato and soil were investigated by gas chromatography (GC). The pesticide in potato was extracted with n-hexane, filtered and concentrated. The concentrated phase was transferred to the Sep-Pak silica gel column and purified with acetonitrile and acetone for the analysis by gas chromatography equipped with electron capture detector (GC-ECD). From the standard additional experiments with 0.01 and $0.1{\mu}g$, the recoveries were 85-87% and the detection limit was 0.005 ng. The soil sample was extracted with acetone and dichloromethane. The organic phase was concentrated and redissolved with n-hexane and analyzed with GC-ECD after cleaned with Sep-Pak column. From the standard additional experiments with 0.01 and 0.1 ng, the recoveries were 84-88% and the detection limit was 0.005ng. The half-life time of cyfluthrin in the silty clay was 25 days in the room laboratory and 0.6 days in the fieJd test whereas it was 38 days and 0.5 days for each in case of silty loam.

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