• Title/Summary/Keyword: Gas chromatography-electron capture detector

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Effect of Bile Salt on the Pharmacokinetics of Bretylium in the Rat (I) - Increased Lipophiiicity of Bretylium by Ion-Pair Complexation with Taurodeoxycholate -

  • Shim, Chang-Koo;Chung, Suk-Jae;Lee, Jeong-Uk;Lee, Min-Hwa;Kim, Shin-Keun
    • Archives of Pharmacal Research
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    • v.9 no.2
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    • pp.111-114
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    • 1986
  • Bretylium tosylate is a quaternary ammonium compound used for the treatment of ventricular fibrilation in humans. It is advantageous to other cationic compound in the study of biliary excretion in that negligible amount is bound to plasma protein and metabolite is not likely is to be formed. Some researchers reported that the formation of ion-pair complex caused to increase the lipothilicity of cationic compound. The partition of bretylium between water and organic phase was increased with the addition of sodium taurodeoxycholate. Also sensitive gas chromatographical assay procedure using flame ionization detector was studied. This procedure can detect as low as 0.1 mg/ml using 0.1 ml biological sample, but contamination by previous injection is the major problem of this method.

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Determination of the Homocysteine, Cysteine and Methionine in Human Plasma by Gas Chromatography with Electron Capture Detector (기체크로마토그래피-전자포획검출기를 이용한 혈장 중의 Homocysteine, Cysteine 및 Methionine의 동시 분석법)

  • Myung, Seung-Woon;Chang, Yoon-Jung;Yoo, Eun-Ah;Park, Joon-Ho;Min, Hye-Ki;Kim, Myung-Soo
    • Analytical Science and Technology
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    • v.12 no.5
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    • pp.408-414
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    • 1999
  • A selective and sensitive method for the derivatization of total homocysteine (Hcy) and the related compounds in plasma by gas chromatograph (GC)-electron capture detector (ECD) has been developed. To determine total homocysteine, cysteine (Cys), and methionine (Met) in human plasma using GC-ECD, analytes were reduced and converted into their N(O,S)-ethylearbonyl pentafluoropropyl (PFP) ester by derivatization with ethyl chloroformate and pentafluoropropyl alcohol (PFP-OH) in plasma. The best derivatizing agent N(O,S)-ethyl carbonyl PFP ester, was chosen by comparing the sensitivity of derivatized analysis in GC-ECD. The derivatized analytes in plasma were extracted by chloroform, and subsequently back-extracted with hexane and analyzed by GC-ECD. The calibration carves ($R^2$ > 0.990) were linear over the range $5-50{\mu}mol/L$ of Hcy and Met, $40-400{\mu}mol/L$ of Cys spiked in plasma. The detection limit observed by the established method was below $0.5{\mu}mol/L$. This method is highly sensitive and specific in the analysis of Hcy, Cys, and Met. Therefore, we suggest that this method is appropriate in the analysis of trace concentration of Hcy, Cys, and Met in biological fluids.

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The analysis of Residual Pesticides and Sulfur Dioxide in Commercial Medicinal Plants (유통 한약재의 잔류농약 및 잔류이산화황의 함량 분석)

  • Kim, Tae Hee;Jang, Seol;Lee, Ah Reum;Lee, A Young;Choi, Goya;Kim, Ho Kyung
    • The Korea Journal of Herbology
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    • v.27 no.6
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    • pp.43-48
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    • 2012
  • Objectives : This study was investigated to determine the contents of pesticide residues and sulfur dioxide residues in commercial herbal medicines in Korea. Methods : Chromatographic test was performed on 100 samples consisted with 10 kinds of medicinal plants including improted and domestic products. To establish 19 pesticide residues (DDE, DDD, DDT, Dieldrin, Methoxychlor, BHC isomers, Aldrin, Endosulfan isomers, Endrin, Captan, Procymidone, Chlorpyrifos and Imidacloprid) in commercial herbal medicines, chromatographic equipments were used with the gas chromatography-mass detector and gas chromatography-electron capture detector for qualitative analysis. The imidacloprid analysis was performed by high performance liquid chromatograpgy-ultraviolet detector at 270 nm UV wavelength. The contents of sulfur dioxides were analyzed by modified Monnier-Williams method. All methods were based on notification procedure of Korea Food & Drug Administration (KFDA). Results : The residual pesticides were not founded in improted and domestic samples. Among 100 samples, the residues of sulfur dioxide in 73 samples were not detected and 25 samples showed contents in the range of 0~21.90 mg/kg. The excess samples of MRLs were 2 samples (30 mg/kg to medicinal herbs), Asiasari Radix et Rhizoma (Imported product) and the average amount of sulfur dioxide in 2 unsuitable samples were 14.83 mg/kg. These samples were found to transgress KFDA regulatory guidance of residual sulfur dioxide. Conclusion : These results are able to use as basic data to improve the reliability and value of commercial medicinal herbs.

The Concentrations of PCBs in the Serum and Theri Predictors of Exposure n Korean Women (일부 한국 성인 여성들의 혈중 PCBs 농도 및 그 노출요인의 연구)

  • 민선영;정문호;이강숙;노영만;구정환
    • Journal of Environmental Health Sciences
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    • v.26 no.2
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    • pp.97-107
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    • 2000
  • PCBs [Polychlorinated biphenyls] are halogenated aromatic compounds with the empirical formula C12H10-nCln(n=1~10), and are a mixture of possible 209 different chlorinated congeners. PCBs were widely used as dielectric fluids for capacitors, transformers, plasticizers, lubricant inks, and paint additives. once released into the environment, PCBs persist for years because they are so resistant to degradation. In addition to their high degree of lipophilicity. In 1970s, the worldwide production of PCBs seem to be still in use. The environmental load of PCBs was prohibited since 1983 in Korea. In spite of these actions, many PCBs seem to be still in use. The environmental load of PCBs will continue to be recycled through air, land, water, and the biosphere for decades to come. This study was conducted to measure the concentrations of PCBs I the serum samples of 112 women by GC/MSD(Hewlett Packard 5897 Gas Chromatography-Mass Chromatography Detector) and CG/ECD(Hewlett Packard 5890 series-II gas chromatography-Electron capture detector, U.S.A). The main results of this study were as follows; The mean and standard deviation of serum PCBs were 3.613, 0.759 ppb, respectively and median of it was 3.828 ppb. The correlation coefficients of the concentrations of 13 PCB congeners ranged from 0.7913 to 0..9985 and were significantly correlated between each items(p=0.0001). The PCB concentrations were positively associated with age(simple linear regression; R2=0.86, =0.08023, p<0.001) and with total lipids in serums(simple linear regression; R=0.7058, =0.00486, p<0.001). The age adjusted model (Y=$\beta$0+$\beta$1age+$\beta$2X) was applied for possible predictors of PCBs levels in serum. For BMI(Body Mass Index), major residential area, and fish, meat, and dairy consumption, there was no association with PCBs levels, Also there was negative association for the number of pregnancy and lactation period with PCBs levels.

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Comparative Studies on the Analysis of Pesticide Residues. in Rice, Barley and Wheat (주곡중의 잔류농약분석에 관한 연구)

  • Park Seung Heui
    • Korean journal of applied entomology
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    • v.13 no.4 s.21
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    • pp.235-243
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    • 1974
  • Recenty, the pesticides Pollutions in connection with the maintenance of dietary life are poised as serious sanitary problems. Author have established an appropriate analysis method in this connection and, at the same time, analysed the levels of pesticides residues, such as organochloride pesticides and organic mercurials, contained in main cereals (rice, barley, and wheat) collected throughout the country. Using gas liquid chromatography method, comparative analyses were made of organochloride Pesticides with electron capture detector, and organic mercurials with electron capture detector and the Dithizone Method. As a result, the organic mercurials analysis using gas liquid chromatography is believed to hold out an especially good method for both in terms of its sensitivity and its Practical applications. The summary obtained from these results is as follows; The detectable limit of organochloride pesticides is $5\times10^{-10}$ grams and that of organic mecurials is $5\times10^{-9}$ grams. The detections using the Dithizone Method are difficult. The gas liquid chromatographic analysis of organic mercurials is very simple in its operation and high in its sensitivity, compare with the analysis using the Dithizone Method. Therefore, this analysis is expected to be a good method applicable to the pesticide residues analysis. The levels of pesticide residues contained in samples are very little for tolerance and, therefore, no problem i.: foreseen for eating. The appropriate conditions of gas liquid chromatographic analysis obtained from these results are expected very useful for the date establishing an officially authorized analysis method.

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Analysis of Multiple Pesticide Residues in Apples and Pears Using Gas-Liquid Chromatography (Gas-Liquid Chromatography를 이용한 사과 및 배 중의 농약 다성분 잔류분석법)

  • Park, Ju-Hwang;Kim, Taek-Kyum;Oh, Chang-Hwan;Kim, Jeong-Han;Lee, Young-Deuk;Kim, Jang-Eok
    • Korean Journal of Environmental Agriculture
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    • v.23 no.3
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    • pp.148-157
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    • 2004
  • A rapid analytical method was developed to determine multiple pesticide residues in apples and pears using gas-liquid chromatography (GLC). The samples were extracted with water-miscible solvents and purified by cleanup procedures serially comprising liquid-liquid partition and solid-phase extraction (SPE). Each analyte was separated and determined by a high-resolution GLC equipped with electron-capture detector (ECD) and nitrogen-phosphorous detector (NPD). A total of 196 pesticides, which were previously classified into 5 groups each for ECD and NPD based on their retention behaviors on the capillary column and responses to the detector, were subjected to the recovery experiment. In compliance with the analytical criteria, 70 to 120% of recovery and less than 20% relative standard deviation the proposed method could be successfully applied to analyze 136 and 133 pesticide residues in apples and pears, respectively, which enabled not only rapid screening but quantitation of the residues. Even though less reliability was resulted from unacceptable recovery range, rest of pesticides including 43 and 45 analyzes in apples and pears, could be also detected for their identity. The proposed method fliled to cover 17 and 18 pesticides for apples and pears, which mostly showed high polarity or heat-lability but could be suitable far fast surveilance or monitoring of fruit harvests.

Monitoring and Risk Assessment of Pesticide Residues in Commercially Dried Vegetables

  • Seo, Young-Ho;Cho, Tae-Hee;Hong, Chae-Kyu;Kim, Mi-Sun;Cho, Sung-Ja;Park, Won-Hee;Hwang, In-Sook;Kim, Moo-Sang
    • Preventive Nutrition and Food Science
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    • v.18 no.2
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    • pp.145-149
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    • 2013
  • We tested for residual pesticide levels in dried vegetables in Seoul, Korea. A total of 100 samples of 13 different types of agricultural products were analyzed by a gas chromatography-nitrogen phosphate detector (GC-NPD), an electron capture detector (GC-${\mu}ECD$), a mass spectrometry detector (GC-MSD), and a high performance liquid chromatography- ultraviolet detector (HPLC-UV). We used multi-analysis methods to analyze for 253 different pesticide types. Among the selected agricultural products, residual pesticides were detected in 11 samples, of which 2 samples (2.0%) exceeded the Korea Maximum Residue limits (MRLs). We detected pesticide residue in 6 of 9 analyzed dried pepper leaves and 1 sample exceeded the Korea MRLs. Data obtained were then used for estimating the potential health risks associated with the exposures to these pesticides. The estimated daily intakes (EDIs) range from 0.1% of the acceptable daily intake (ADI) for bifenthrin to 8.4% of the ADI for cadusafos. The most critical commodity is cadusafos in chwinamul, contributing 8.4% to the hazard index (HI). This results show that the detected pesticides could not be considered a serious public health problem. Nevertheless, an investigation into continuous monitoring is recommended.

Development of Simultaneous Analytical Method for Various Residual Pesticides Using GC-ECD (GC-ECD를 이용한 잔류 농약 다성분 동시 분석법 개발)

  • 김우성;손영욱;정지윤;안경아;홍무기;임무혁;이홍재;이봉헌;박흥재
    • Journal of Environmental Health Sciences
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    • v.27 no.1
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    • pp.88-92
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    • 2001
  • The simultaneous analytical method for 37 residual pesticides was developed by a gas chromatography with $^{63}$ Ni electron capture detector. Pesticides added in soybean sample were extracted with 70% acetone in water and methylene chloride in oder, and then cleaned up via open-column apparatus packed with florisil and alumina N. The Ultra-2 fused capillary column was used to separate the products. The resolution between the last isomeric peak of cypermethrin (56.398 min) and the first isomeric peak of flucythrinate (56.421 min) was not satisfactory and the last isomeric peak of fenvalerate(58.783 min) and the first isomeric peak of fluvalinate(58.835 min) was overlapped. Except for $\alpha$-BHC, dichlofluanid, captan, and captafol, most recoveries were showed over 70%.

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5% $Cr_2O_3/{\gamma}-Al_2O_3$ Catalysts Synthesized as Research for Oxidation Activation of Trichloroethylene

  • Myung, So-Young;Suh, Myung-Gyo;Lee, Yong-Hee
    • Proceedings of the Korean Environmental Health Society Conference
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    • 2005.12a
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    • pp.78-82
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    • 2005
  • The research addressed the ability of 5% $Cr_2O_3/{\gamma}-Al_2O_3$ to catalytically oxidize trichloroethylene(TCE). In order to determine which procedure gives the most active catalyst among the attempted several procedures, catalytic oxidation reaction of TCE was conducted to every catalysts synthesized according to different process in tubular reactor system, which had functional relationships with temperature and space velocity. The ratio of TCE conversion was analyzed by gas chromatography with electron capture detector.

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Atmospheric Sulfur Hexafluoride $(SF_6)$ near the Kwanak Mountain, Seoul (서울 관악산 대기 중의 $SF_6$에 관한 연구)

  • Lee, Junghyun;Kim, Kyung-Ryul
    • Atmosphere
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    • v.18 no.3
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    • pp.225-235
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    • 2008
  • Sulfur hexafluoride ($SF_6$), man-made compound, has been paid attention as a potent greenhouse gas. After Kyoto Pototcol on Climate Change in 1997, nations established the policy aimed at minimizing release of $SF_6$ to atmosphere. We have developed and operated an automatic analytical system for monitoring atmospheric $SF_6$ using gas chromatography with electron capture detector (GC-ECD) and packed separate-column. Here, we report and discuss 4-month record of atmospheric $SF_6$ concentrations monitored at Seoul National University (SNU) pilot station near the Kwanak Mountain, Seoul. Most of observed $SF_6$ concentrations were excessively high compared with Northern Hemisphere (NH) background trend obtained from National Oceanic and Atmospheric Administration (NOAA) Earth System Research Laboratory (ESRL) monitoring stations. And the observed $SF_6$ showed extremely wide variability ranging from 4.6 pptv to $1.1{\times}10^3$ pptv, which may be affected by local sources placed nearby. Simultaneous wind data with $SF_6$ measurements show that relatively high values of $SF_6$ correspond to weak wind as well as southerly. There are many engineering installations to the south of the station. The regional value of the atmospheric $SF_6$ estimated from the data selection by wind conditions is about 6.8 pptv. This value, which is similar to concentrations of urban areas, is higher than NH background concentration.