• Title/Summary/Keyword: GC-determination

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The Evaluation of Solid-Phase Microextraction(SPME) Techniques for Analyzing Mixed Fuel Oxygenates and Products

  • 이재선;이시진;장순웅
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2003.09a
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    • pp.458-461
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    • 2003
  • Solid-phase microextraction (SPME) and gas chromatography/headspace techniques(HS) and flame ionization detection (GC/FID) have been combined for determination of very polar compounds in water, including the widely used gasoline oxygenates and by-products. A relatively simple extraction method using a CAR/PDMS(75${\mu}{\textrm}{m}$) SPME fiber was optimized for the routine analysis of gasoline oxygenates and by-products in groundwater and reagent water. A sodium chloride concentration of 25%(w/w) combined with an extraction time of 20 min provided the greatest sensitivity while maintaining analytical efficiency Replicate analyses in fortified reagent and groundwater spiked with microgram per liter concentrations of gasoline oxygenates and by-products indicate quantitative and reproducible recovery of these and related oxygenate compounds. Method dynamic range was 50$\mu\textrm{g}$ L-1 to 3000$\mu\textrm{g}$ L-1 for gasoline oxygenates and by-products.

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Evaluation of Barley Bran Sauce Aroma by Multiple Regression Analysis

  • Choi, Ung-Kyu
    • Food Science and Biotechnology
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    • v.14 no.5
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    • pp.656-660
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    • 2005
  • The relationship between the gas chromatographic (GC) patterns of sauce made of barley bran and ranked order in sensory analysis was investigated by multiple regression analysis (MRA). Most of the 42 barley bran sauce samples comprised about 34 peaks, in which the content of 9, 12-octadecanoic acid methyl ester was the highest, followed by those of 2-furanmethanol and 2-furancarboxaldehyde. It is difficult to estimate the aroma quality of barley bran sauce samples on the basis of only one peak. The 34 aroma compounds of the 42 samples were analyzed by an MRA model featuring six transformations. The most precise fit was calculated from the absolute value transformed with the root square of each peak, and the multiple determination coefficient showed that 91.6% of the variation in the sensory score could be explained on the basis of GC data.

The Simultaneous Analysis of Benzene, Toluene, Ethylbenzene, o,m,p-Xylenes and Total Petroleum Hydrocarbons in Soil by GC-FID after Ultra-Sonication

  • Sin, Ho Sang;Gwon, O Seung
    • Bulletin of the Korean Chemical Society
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    • v.21 no.11
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    • pp.1101-1105
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    • 2000
  • A simultaneous determination method of BTEX (benzene, toluene, ethylbenzene, o,m.p-xylene) and TPH (kerosene, diesel, jet fuel and bunker C) in soil with gas chromatography/flame ionization detection (GC-FID) was described. The effects of extracti on method, extraction solvent, solvent volume and extraction time on the extraction performance were studied. A sonication method was simpler and more efficient than Soxhlet or shaking methods. Sonication with 10 mL of acetone/methylene chloride (1 : 1, v/v) for 10 min was found to be optimal extraction conditions for 20 g of soil. Peak shapes and quantification of BTEX and TPH were excellent, with linear calibration curves over a wide range of 1-500 mg/L for BTEX and 10-5000 mg/L for TPH. Good reproducibilities by sonication were obtained, with the RSD values below 10%. By using about 20 g of soil, detection limits were 0.8 mg/L for BTEX and 10 mg/L for TPH. The advantages of this procedure are the use of simple and common equipment, reduced volumes of organic solvents, rapid extraction periods of less than 20 min, and simultaneous analysis of volatile and semivolatile compounds.

Effective determination of nicotine enantiomers from e-liquids and biological fluids by high performance liquid chromatography (HPLC) using dispersive liquid-liquid microextraction (DLLME)

  • Song, Seunghoon;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.34 no.4
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    • pp.180-190
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    • 2021
  • This study compared the efficacy of chiral GC and chiral HPLC for the analysis of nicotine. To develop a suitable dispersive liquid-liquid microextraction (DLLME) method, the following parameters were optimized: pH, extraction solvent, dispersive solvent, type and quantity of salt, and laboratory temperature. The validation of the method was carried out by the established HPLC method. The LODs were 0.11 ㎍/mL and 0.17 ㎍/mL for the (S)- and (R)- enantiomers, respectively. The LOQs were 0.30 ㎍/mL and 0.44 ㎍/mL, respectively. The optimal calibration range was between 0.30-18 ㎍/mL and 0.44-4.40 ㎍/mL, respectively, and the correlation coefficient (r2) was 0.9978-0.9996. The intra-day accuracy was 79.9-110.6 %, and the intra-day precision was 1.3-12.0 %. The inter-day accuracy was 87.8-108.0 %, and the inter-day precision was 4.0-12.8 %. E-liquid and biological fluids (urine and saliva) were analyzed using the established method.

Determination of MDMA and MDA in 44 hair samples during 2002 to 2003

  • Han, Eun-Young;Yang, Won-Kyung;Lee, Jae-Sin;Park, Yong-Hoon;Kim, Eun-Mi;Lim, Mi-Ae;Chung, Hee-Sun
    • Proceedings of the PSK Conference
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    • 2003.10b
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    • pp.112.1-112.1
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    • 2003
  • The qualitative and quantitative analysis of MDMA and MDA in hair samples by GC/MS were reported. Hairs were collected from subjects aged 22-37 years, who were suspected of abusing MDMA. After washing with methanol, hair samples were cut into small pieces, extracted with methanol containing 1 percent hydrochloric acid for 20th, and the solution was evaporated. MDMA or MDA in the extract were determined by GC/MS using selected ion monitoring after derivatization with trifluoroacetic anhydride. (omitted)

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Rapid Screening Method for the Solid-Phase Extraction and GC/MS analysis of Diazepam.

  • Choi, Hwa-Kyung;Lee, Ju-Seon;Choi, Hye-Young;Woo, Sang-Hee;Park, Yoo-Sin;Chung, Hee-Sun
    • Proceedings of the PSK Conference
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    • 2003.10b
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    • pp.118.3-119
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    • 2003
  • Diazepam (DZ) is one of the most frequently prescribed drugs as an antianxiety agent, muscle relaxant, and anticovulsant and sometimes causes intoxication due to accidental overdose, misuse or abuse. Screening or confirmation methods for DZ and NDZ in plasma are very important for clinical and toxicological studies and in forensic cases. GC/MS assay with SPE was developed for the determination of diazepam and its metabolite, nordiazepam in human plasma. Diazepam in plasma was extracted by a rapid and sensitive procedure based on C18 bonded-phase extraction. (omitted)

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MEASUREMENT OF PESTICIDES RESIDUES USING SPECTROSCOPY ON AGRICULTURAL PRODUCTS

  • Kim, Y. W.;S. H. Noh
    • Proceedings of the Korean Society for Agricultural Machinery Conference
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    • 2000.11c
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    • pp.525-532
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    • 2000
  • A new spectroscopic method for pesticide residues detection on agricultural products was developed. The general determination methods are high performance liquid chromatography (HPLC), gas chromatography (GC) or GC-mass spectrometry. They have provided relatively good detection limit and accuracy with complicated and time-consuming (5hrs above) procedures. In addition freshness is very important for evaluating qualities of agricultural products. This requires a simple and fast method for detection of pesticides. Reflectance, transmittance and fluorescence spectrometry of pesticides were tested using UV range because most of pesticides contain conjugation band in the molecular structures. Fluorescence spectrometry showed better sensitive to detect pesticide residues than did reflectance and transmittance spectrometry. Intensity and shape of fluorescence spectra showed different patterns with different structures of pesticides. Detection limit for fluorescence spectrometry was 0.1 ppm to 10 ppm depending on the structures of pesticides. Application of fluorescence spectrometry appears to be an easy method for detection of pesticide residues on agricultural products.

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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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Determination of trace impurities of HFC-134a by gas chromatograph with atomic emission detector (GC/AED) (GC/AED를 이용한 HFC-134a의 미량 불순물 분석)

  • Kim, Myeongja;Lim, Jeongsik;Lee, Jinbok;Lee, Jeongsoon
    • Analytical Science and Technology
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    • v.30 no.5
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    • pp.240-251
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    • 2017
  • 1,1,1,2-Tetrafluoroethane (HFC-134a), which is used as refrigerant in air conditioners, has been recently regulated as a greenhouse gas and is recommended for reuse by refining. It is very important to quantitatively analyze trace impurities present in the refrigerant to evaluate the criteria for reuse. In this study, trace impurities including C, H, Cl, and F, which are difficult to quantify because there are no reference materials, were quantitatively analyzed by a gas chromatograph-atomic emission detector (GC/AED); for this analysis, this was preceded by a qualitative analysis with a GC-mass selective detector (GC/MSD). In addition, the AED response was investigated using a hydrocarbon mixed reference material, which was proportional to the number of atoms in the component. Fifteen refrigerant components were detected as trace impurities in HFC-134a by qualitative analysis of trace impurities including C, H, Cl, and F in the samples. Based on the results of the qualitative analysis, quantitative analysis of trace impurities using AED showed that the highest mole fractions were for the $CHClF_2$ component ($45438.38{\mu}mol/mol$) in one sample and for the $C_2H_2ClF_3$ component ($1311.47{\mu}mol/mol$) in another sample. From this study, it has been shown that it is possible for this analytical method to be applied to the qualitative and quantitative analysis of trace compounds in refrigerants, which are difficult to quantify because of the absence of reference materials.

Analysis of Synthetic Fragrances (SFs) in Water Using Stir Bar Sorptive Extraction (SBSE) and GC-MS/MS (교반막대 추출법과 GC-MS/MS를 이용한 수중의 합성 향물질류 분석)

  • Seo, Chang-Dong;Son, Hee-Jong;Yoom, Hoon-Sik;Choi, Jin-Taek;Ryu, Dong-Choon;Kwon, Ki-Won;Jang, Seung-Ho
    • Journal of Korean Society of Environmental Engineers
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    • v.36 no.6
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    • pp.387-395
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    • 2014
  • A highly sensitive analytical method based on stir bar sorptive extraction (SBSE) technique and gas chromatography/tandem mass spectrometry (GC-MS/MS) has been developed, allowing the simultaneous multi-analyte determination of 11 synthetic fragrances (SFs) in water samples. The stir bar coated with polydimethylsiloxane (PDMS) was added to 40 mL of water sample at pH 3 and stirred at 1,100 rpm for 120 min. Other SBSE parameters (salt effect and presence of organic solvent) were optimised. The method shows good linearity (coefficients > 0.990) and reproducibility (RSD < 10.9%). The extraction efficiencies were above 83% for all the compounds. The limits of detections (LOD) and limits of quantification (LOQ) were 2.1~4.1 ng/L and 6.6~12.9 ng/L, respectively. The developed method offers the ability to detect 11 SFs at ultra-low concentration levels with only 40 mL of sample volume. Matrix effects in tap water, river water, wastewater treatment plant (WWTP) final effluent water and seawater were investigated and it was shown that the method is suitable for the analysis of trace level of 11 SFs. The method developed in the present study has the advantage of being rapid, simple, high-sensitive and both user and environmentally friendly.