• Title/Summary/Keyword: GC-determination

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Evaluation of QuEChERS Method for Determination of pesticide Residues Using GC/NPD and GC/ECD (GC/NPD와 GC/ECD를 이용한 잔류농약 정량 분석법으로써의 QuEChERS의 평가)

  • Cho, Tae Hee;Park, Young Hye;Park, Hye Won;Hwang, Lae Hwong;Cho, In Soon;Kim, Min Jung;Kim, Hyun Jeong;Kim, Mu Sang;Chae, Young Zoo
    • The Korean Journal of Pesticide Science
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    • v.17 no.1
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    • pp.65-71
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    • 2013
  • The modified QuEChERS method was evaluated for rapid determination of pesticide residues in spinach by gas chromatography-nitrogen phosphorous detector (NPD) and electron capture detector (ECD). Fifty GC-amenable pesticides which were most frequently detected in monitoring were selected in the current study. Matrix-matched calibration was performed. The detector response for all pesticides was linear with determination coefficients higher than 0.995. LODs for most compounds ranged between 0.001 and 0.1 ug/g, and about 90% of the compounds had LODs of less than 0.05 ug/g. LOQs ranged from 0.001 to 0.32 ug/g, which were well below the MRLs permitted for most of pesticides. In the majority of cases, the recoveries (80-120%) and relative standard deviations (RSDs) (less than 20%) were within acceptable levels except for dichlorvos, propamocarb, chlorothalonil, dichlofluanid, cyhalothrin and fenvalerate. Also, this method which is applied to routine samples showed good results when comparing with traditional multi-residue method.

Determination of Cr(Ⅵ) by Glassy Carbon and Platinum Electrodes Modified With Polypyrrole Film (폴리피롤 막으로 변성시킨 유리질 탄소 및 백금 전극에서 Cr(Ⅵ) 이온의 정량)

  • Yoo, Kwang Sik;Woo, Sang Beom;Jyoung, Jy Young
    • Journal of the Korean Chemical Society
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    • v.43 no.4
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    • pp.407-411
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    • 1999
  • Studies have been carried out on the fabrication of PPy/GC and PPy/Pt electrode modified with polypyrrole film and determination of Cr(VI) by using 3-electrode system with modified electrodes. Modified electrodes were able to easily fabricated by cyclic voltammetry scanned from +1.0V to -1.0V(vs. Ag/AgCl) at 50 mV/sec. Film thickness could be controlled at same condition by the number of cycling up to 26 times. Reduction behaviour of Cr(VI) at PPy/GC electrode could be seen at wide potential ranges from +0.6V to -0.5V(vs. Ag/AgCl), and maximum reduction peak potential of the ion was observed at -0.25V(vs.Ag/AgCl). Calibration graph at its potential was linear from 0.1 ppm to 80.O ppm. Slope factor and relative coefficient were 1.75 mA/ppm and 0.998, respectively. Reduction behaviour of Cr(VI) at PPy/Pt electrode was similar to PPy/GC electrode, Calibration graph was linear from l.0 ppm to 60.0 ppm. Slope factor and relative coefficient were 0.5mA/ppm and 0.923, respectively. But PPy/GC modified electrode had about 3 times higher sensitivity than PPy/Pt modified electrode. Reduction behaviour of Cu(II), As(IlI), Pb(II), and Cd(II) couldn't be seen at PPy/GC electrode,Its metals had not lnterfered with Cr (VI) determination.

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An Improved Analytical Method for the Determination of Qualitative and Quantitative Characteristics of Di- and Trisaccharides in Honey using GC and GC/MS (GC 및 GC/MS에 의한 벌꿀 중의 이·삼당류 정성 및 정량 특성과 개선된 동시분석방법의 확립)

  • Kim, Jong-Bae;Jang, Eun-Suk;Kim, In-Suk;Lee, Hee-Jin;Lee, Hye-Jeong;Seo, Hyun-Sun;Park, Nam-Pyo
    • Korean Journal of Food Science and Technology
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    • v.47 no.1
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    • pp.27-36
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    • 2015
  • The improved analytical method with gas chromatography (GC) and GC-mass spectrometry was established to identify and quantify disaccharides and trisacchrides in honey. In this method, the analysis of trimethylsilyl (TMS), TMS-oxime and TMS-methoxime sugars takes into account the determination of a single peak of complete separation on the chromatogram. The number of possible peaks for the qualitative and quantitative determination of TMS, TMS-oxime, and TMS-methoxime sugars was 17, 22, and 25, respectively. This new analytical method allowed for the determination of diand trisaccharides in honey by TMS-oxime and TMS-methoxime derivatives. This study suggested that the improved method is more suitable and precise than the other analytical methods for the simultaneous determination of sugars in honey.

Determination of the Concentration of Panaxynol, Panaxydol and Panaxytrio1 by Capillary-GC(FID) (Capillary-GC(FID)에 의한 panaxynol, panaxydol 및 panaxytriol의 정량)

  • 노길봉;손현주
    • Journal of Ginseng Research
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    • v.13 no.2
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    • pp.183-188
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    • 1989
  • A gas chromatographic method was developed for determination of the concentration of three major polyacetylene compounds in ginseng roots---panaxynol, panaxydol and panaxytriol. The column and the detector used were an SPB-1 fused silica capillary (0.2mm i.d.$\times$30m, Supelco) and a flame ionization detector (FID). The column oven temperature was kept at $250^{\circ}C$ isothermally The retention times of panaxynol, panaxydol and panaxytriol peaks were 4.2,5.1 and 6.9 min before TMS-derivatitration and 4.5,5.4 and 7.4 min after TMS-derivatization, respectively. The minimum determinable concentrations of panaxynol, panaxydol and panaxytriol before TMS-derivatiEation were at the 20, 50 and 100 ppm levels, while the concentrations of panaxydol and panaxytriol as well as panaxynol after TMS- derivatisation could be towered to the 5 ppm level. The panaxynol, panaxydol and panaxytriol contents in red ginseng were determined by use of this method after TMS-derivatization : the amounts obtained were 724, 721 and 71$\mu\textrm{g}$/g, respectively.

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Determination of Trace Amount of Linear Alkylbenzene Sulfonates in River Water (하천수 중 미량의 Linear Alkylbenzene Sulfonate의 분석)

  • Hong, Sa Uk;Yoo, Young Chan;Chung, Hee Sun;Chung, Kyu Hyuck
    • Analytical Science and Technology
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    • v.5 no.2
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    • pp.159-167
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    • 1992
  • An improved and accurate method for the determination of linear alkybenzene sulfonate(LAS) in river water is described by using gas chromatography and GC/MS. The gas chromatograph equipped with BP-5 capillary column was satisfactory for isolation of the homologues and isomers of LAS in river water. Four LAS homologues, $C_{10}$, $C_{11}$, $C_{12}$, $C_{13}$ alkyl chains were determined in Jungrang stream, Jinwi stream and down stream of Han river tributary. Especially $5-C_{11}$, $6-C_{11}$, $2-C_{12}$ and $6-C_{13}$, $7-C_{13}$ of LAS were identified by mass chromatogram. Different composition of LAS in standard and river water expressed the distribution and fate of LAS in river water. The remarkable reduced content of $C_{12}$ and $C_{13}$ in river water implied that the biodegradation of LAS more easily occured in longer alkylchain one. This method would be applicable for determination of LAS in water with high resolution and sensitivity.

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Determination of panthenol, cholecalciferol and tocopherol in cosmetic products by gas chromatography-mass spectrometry in SIM mode

  • Hye-Jin Jeong;Myo
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.22 no.2
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    • pp.153-160
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    • 1996
  • A novel simple method to detect vitamins in cosmetic products by gas chromatography-mass spectrometry(GC-MS) has been developed. Three vitamins(panthenol, cholecalciferol and tocopherol) were used for this study. Vitamins were prepared by dissolving in tetrahydrofuran(THF), and silylated with bis-trimethylsilyltrifluoroacetamide-trichloromethylsilane(BSTFA). Silated vitamins were separated on a fuses-silica capillary column coated with DB-5. The identification of each vitamin was accomplished by retention time and mass spectrum library search with a computer, and the quantitation was made in the selected-ion monitoring(SIM) mode of GC-MS. SIM mode had given sensitivity to determine 50pg of panthenol, 285pg of cholecalciferol and 130pg of tocopherol. Linearity was maintained over the range 0.005-0.20% for each vitamin. Each cosmetic product(i.e. hair tonic and lotion) was found to contain amounts of the vitamins. This method was sensitive and gave 77.5-99.9% recovery of each vitamin from these cosmetic products. From these results, we concluded that silylation with BSTFA followed by GC-MS analysis allows the simple, covenient and exact determination of panthenol, cholecalciferol and tocopherol.

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Analysis of 3,4-Methylendedioxymethamphetamine (MDMA) in Human Hair by Gas Chromatography/Mass Spectrometry (GC/MS를 이용한 모발 중 MDMA(Methylendedioxymethamphetamine)의 분석)

  • 박미정;김은미;임미애;정희선
    • YAKHAK HOEJI
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    • v.47 no.4
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    • pp.195-199
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    • 2003
  • An analysis method for the determination of methylendedioxymethamphetamine (MDMA) and its metabolite methylendedioxymethamphetamine (MDA) in hair by gas chromatography/mass spectrometry was proposed. For MDMA and MDA analysis, hair samples were incubated in MeOH (1% HCl), derivatized with trifluoroacetic anhydride and assayed by GC/MS. Hair of 18 subjects for drug abuse was analyzed for MDMA and MDA. Calibration curves for the determination of MDMA and MDA in hair showed a good linearity at a concentration range from 0.5 ng to 250 ng ($r^2$=0.999) The extraction recovery was determined from hair blanks at 50, 100 ng. The percentage of recovery were found to be 96.08∼103.48 with CV value of 1.62∼3.89. The concentrations of MDMA and MDA ranged 1.14∼38.06 ng/mg and 0.07∼3.91 ng/mg, respectively in 18 hair samples from MDMA abusers. The ratio of MDMA to MDA ranged from 9.65∼28.46 in all specimen. Hair analysis for MDMA is a useful method for identification of long-term drug abuser.

Determination of methamphetamine in the hair of Korean abuser by CG/MS (GC/MS에 의한 한국인의 모발중 Methamphetamine검출)

  • 유영찬;정희선;최화경
    • YAKHAK HOEJI
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    • v.37 no.4
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    • pp.356-361
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    • 1993
  • A sensitive method for the determination of methamphetamine(MA) and amphetamine(AM) in hair was developed by gas chromatography/mass spectrometry using stable isotope-labeled internal standards, amphetamine-d$_{5}$ and methamphetamine-d$_{5}$. Hair sample was washed with MeOH, incubated with MeOH(I% HCI) overnight at $37^{\circ}C$ while stirring and extracted using solid phase extraction column on a vacuum manifold. The extract obtained was pentafluoropropionated, and applied to GC/MS. The calibration curves of MA and AM were linear from 2.5 to 250 ng (r>0.99 for both). The limit of detection was 0.1 ng/mg in hair and cut-off level was set at 0.25 ng/mg for both. Hair samples of 27 MA abusers showed positive results in the range 0.7 to 106.8 ng/mg. AM, its metabolite, was detected in 20 out of 27 samples. The ratio of MA versus AM was 4.6~38.3 in specimens. Hair analysis for methamphetamine by GC/MS is an effective method for identifying long-term drug abusers.

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Determination of Acrylamide in Foods by Solid Phase Microextraction-Gas Chromatography

  • Chen, Liangbi;Liu, Haizhu;Yu, Ping;Zhao, Jinyun;Chen, Xi
    • Food Science and Biotechnology
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    • v.18 no.4
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    • pp.895-899
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    • 2009
  • A new approach for the determination of acrylamide (AM) in foods by solid phase microextraction-gas chromatography (SPME-GC) was established. AM was bromized and transformed to 2-bromoacrylamide (2-BAM). 2-BAM was then extracted by a commercial SPME fiber, $75-{\mu}m$ Car/PDMS fiber, for GC detection. The influence of extraction and desorption parameters such as extraction temperature and time, stirring rate, desorption temperature, and time were studied and optimized. The mass concentration was proportional to the peak area of 2-BPA from 1.0 to 8,000 ${\mu}g/L$. The detection limit of the SPME-GC for 2-BAM was found to be 0.1 ${\mu}g/L$, and the recoveries and relative standard deviations for different food samples were 74.5 to 102.0%, and 4.2 to 9.1%, respectively. The presented method was applied to the determination of AM in fried foods.

Uncertainty in Determination of Menthol from Mentholated Cigarette (담배 중 멘톨 분석에 대한 불확도 측정)

  • 장기철;이운철;백순옥;한상빈
    • Journal of the Korean Society of Tobacco Science
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    • v.22 no.1
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    • pp.91-98
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    • 2000
  • This study was carried out to evaluate the uncertainty in the analysis of menthol content from the mentholated cigarette. Menthol in the sample cigarette was extracted with methanol containing an anethole as an internal standard, and then analyzed by gas chromatography. As the sources of uncertainty associated with the analysis of menthol, were the following points tested, such as the weighing of sample, the preparation of extracting solution, the pipetting of extracting solution into the sample, the preparation of standard solution, the precision of GC injections for standard & sample solution, the GC response factor of standard solution, the reproducibility of menthol analysis, and the determination of water content in tobacco, etc. For calculating the uncertainties, type A of uncertainty was evaluated by the statistical analysis of a series of observation, and type B by the information based on supplier's catalogue and/or certificated of calibration. Sources of uncertainty were subsequently included and mathematically combined with the uncertainty arising from the assessment of accuracy to provide the overall uncertainty. It was shown that the main source of uncertainty came from the errors in the reproducibility of menthol and water determination, the purity of menthol reference material in the preparation of standard solution, and the precision of GC injections for sample solution. The errors in sample weighing and volume measurement contributed relatively little to the overall uncertainty. The expanded uncertainty in the mentholated cigarettes, Korean and American brand, at 0.95 level of statistical confidence was $\pm$0.06 and $\pm$0.07 mg/g for a menthol content of 1.89 and 2.32 mg/g, respectively.

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