• 생약학회지
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• 제32권3호통권126호
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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.

• 고려인삼학회:학술대회논문집
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• 고려인삼학회 2002년도 학술대회지
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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.

• 한국산업보건학회지
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• 제16권3호
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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.

• 농약과학회지
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• 제11권2호
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• pp.106-116
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• 2007

들깻잎의 재배 중에 사용되는 살충제인 chlorfluazuron의 잔류량을 포장시험 하여 생물학적 분해반감기를 구하고 출하 10 일전까지의 각 일자별 농약잔류허용량을 설정하였다. 본 실험은 Benzoylurea계 계통인 chlorfluazuron의 본 GC/ECD 분석 시 2005년 반감기와 2006년의 반감기를 조사 비교하고, 열에 안정된 LC분석법으로도 잔류농약을 분석 비교하였다. 그 결과 GC/ECD 분석 시 1 년차에 기준량으로 살포하였을 때 살포 2 일차에는 최초(0 일차) 농도의 32.3%가 감소하였고, 10 일차에는 78.0%가 감소하였다. 2 년차에 기준량으로 살포하였을 때 살포 2 일차에는 최초 농도의 33.1%가 감소하였고, 10 일차에는 77.9%가 감소하였다. 잔류량 감소 양상으로부터 회귀방정식을 구하고 생물학적 분해반감기(Biological half-life)를 도출한 결과, 기준량 살포하여 GC/ECD 분석 시 1 년차에는 4.7 일, 2 년차에는 5.1 일로 나타났다. HPLC/UVD 분석 시 기준량으로 살포하였을 때 살포 2 일차에는 최초(0 일차) 농도의 34.0%가 감소하였고, 10 일차에는 78.4 %가 감소하였으며, 반감기는 4.7 일이었다. 잔류량 변화 반복실험간 표준편차의 95% 신뢰구간에서도 회귀방정식을 구한 후, 산출된 반감기를 근거로 생산단계의 농약잔류허용량을 설정한 결과 출하일의 2.0 mg $kg^{-1}$을 기준(KFDA, MRL)으로 2 일전에 2.5 mg $kg^{-1}$에서 출하 10 일전에는 7.1 mg $kg^{-1}$으로 설정하였다.

• 한국가축위생학회:학술대회논문집
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• 한국가축위생학회 1999년도 제22차 학술대회
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• pp.188.2-189
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• 1999

• 월간산업보건
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• 통권303호
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• pp.18-26
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• 2013

• 대한약학회:학술대회논문집
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• 대한약학회 2001년도 Proceedings of International Convention of the Pharmaceutical Society of Korea
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• pp.288.1-288.1
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• 2001

• 분석과학
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• 제8권3호
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• pp.237-248
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• 1995

미국 환경청이 지정한 129종의 priority pollutants 중 16종의 유기살충제를 포함한 토양시료를 제조하여 표준분석방법인 기체크로마토그래프-전자포획법과 기체크로마토그래프/질량분석기-SIM (selected ion monitoring)법을 이용하여 동시분석의 효율성을 실험하였다. 토양시료의 추출 및 농축방법으로는 EPA의 SW-846 방법을 조금 수정한 초음파추출법(sonication extraction)과 Soxhlet 추출법(Soxhlet extraction)을 비교 연구하였다. 각 화합물의 회수율, 상대표준편차 및 method detection limit를 측정하여 그 결과들을 보고하였다.

• Bulletin of the Korean Chemical Society
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• 제26권4호
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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.

• 분석과학
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• 제13권6호
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• pp.722-730
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• 2000

감자와 토양 중에서 pyrethroid계 살충제인 cyfluthrin의 반감기와 잔류농도를 기체 크로마토그래피로 조사하였다. 감자시료는 n-hexane으로 분리, 농축하여 Sep-Pdk 실리카겔 컬럼 상에서 aretonitrile과 acetone 혼합액으로 정제하였으며, 전자포획검출기가 장착된 기체 크로마토그래피(GC-ECD)로 분석하였다. 0.01과 $0.1{\mu}g$의 표준물 첨가 실험결과 회수율은 85-87%이였고, 검출한계는 0.005ng 이였다. 토양시료는 acetone과 dichlorormthane으로 추출하여 농축하였으며, n-hexane으로 재용해하여 Sep-Pak 컬럼으로 정제한 후 GC-ECD로 분석하였다. 0.01과 $0.1{\mu}g$ 표준물 첨가 실험 결과 85-91%의 회수율을 얻었으며, 검출한계는 0.005 ng이였다. Cyfluthrin의 반감기는 미사질식토의 경우 실내에서 25일, 야외에서는 0.6일이었으며, 미사질양토의 경우에는 실내에서 38일, 야외에서는 0.5일이었다.