• Title/Summary/Keyword: GC-determination

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Optimization of Analytical Procedure for Hydrogen Cyanide in Mainstream Smoke

  • Lee, John-Tae;Kim, Hyo-Keun;Hwang, Keon-Joong;Jang, Gi-Chul;Lee, Jeong-Min;Kim, Ick-Joong
    • Journal of the Korean Society of Tobacco Science
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    • v.29 no.2
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    • pp.125-131
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    • 2007
  • Hydrogen cyanide(HCN), formed from pyrolysis of various nitrogenous compounds such as protein, amino acids and nitrate in tobacco, is present in both the particulate phase and vapor phase of cigarette smoke. Typically the determination of HCN in cigarette smoke has been done through colorimetric and electrochemical techniques, such as fluorescence spectrometry, UV-spectrophotometry (UV), continuous flow analyzer (CFA), capillary GC-ECD and ion chromatography (IC). Most of these techniques are known to be time-consuming and some of them lack specificity or sensitivity. The available results from both our laboratory and reported literatures for 2R4F Kentucky reference cigarette, smoked under ISO condition, show a relatively wide variation ranging from 100 to 120 ug/cig of HCN. Especially, the precision and accuracy of the analytical results of HCN tend to get worse in low tar cigarettes and under intense smoking condition. In this paper, a more optimized analytical methods than previous ones are suggested. This method shows lower detection limit and has improved precision and accuracy, so it is applicable for wide tar level cigarettes under intense smoking condition as well as under ISO smoking condition. Important features of this method are improved sample collection and quantification systems such as the number of trapping units, volume, temperature and type of trapping solution. To avoid volatilization loss of HCN in analyzing mainstream smoke, it is highly recommended that pH values of trapping solutions should be maintained over 11 and cold traps should be used in collecting mainstream smoke.

Determination of Quality Index Components in High-Acidity Cider Vinegar Produced by Two-Stage Fermentation (2단계 발효로 제조된 고산도 사과식초의 품질지표성분 설정)

  • Jo, Yunhee;Park, Yunji;Lee, Hyun-Gyu;Lee, Hye-Jin;Jeong, Yong-Jin;Yeo, Soo-Hwan;Kwon, Joong-Ho
    • Korean Journal of Food Science and Technology
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    • v.47 no.4
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    • pp.431-437
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    • 2015
  • In this study, high-acidity cider vinegar (HACV) was produced by alcoholic and acetic acid fermentation of apple concentrate without any nutrients and then the optimum alcohol concentration was determined through a qualitative study. HACV was fermented with different initial alcohol concentrations (6-9%) during the process of acetic acid fermentation. The highest content of reducing sugar, organic acids, and free amino acids was observed at 6% of initial alcohol concentration. Approximately 20 types of volatile compounds were identified by solid-phase microextraction (SPME) and GC-MS. The total volatile content was the highest at 6% of initial alcohol concentration, and the acid content was the lowest at 9% of the initial alcohol concentration. The HACV produced by a two-stage fermentation process was qualitatively better than commercial HACV presenting the highest value at 6% of initial alcohol concentration. Malic acid, aspartic acid, and hexyl acetate were selected as quality index components of HACV production by two-stage fermentation on the basis of correlation between their physicochemical properties and the sensory attributes of HACV.

Analysis of Genetic Diversity in Echinochloa Species Using Random Amplified Polymorphic DNAs(RAPDs) Markers (RAPD Marker를 이용한 피 수집종의 유연관계 분석)

  • Kim, Kil-Ung;Sohn, Jae-Keun;Shin, Dong-Hyun;Kim, Kyung-Min;Kim, Hak-Yoon;Lee, In-Jung
    • Korean Journal of Weed Science
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    • v.18 no.1
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    • pp.76-83
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    • 1998
  • Echinochloa species maintained by selling for more than 10 years were classified using random amplified polymorphic DNAs(RAPDs) analysis. Seventy-four decamer of randomly sequence markers were used to classify intraspecific variation irt Echinochloa species. The number of amplification products increased with increasing GC content of the primer in the range between 60% and 70% GC. Single-base substitutions of a primer altered amplification, providing new polymorphisms. The size of amplified DNA was mostly between 0.40kbp and 1.4kbp with the most common bands at 1.1kbp. Echinochloa species were detected with 6 primers which generated 26 polymorphic amplified DNAs. By hierarchical cluster analysis, Echinochloa species collected in Korea were divided into three groups. These results revealed that RAPD markers are useful tools for the determination of genetic variations in Echinochloa species.

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Comparison between the liquid-liquid partition method and modified QuEChERS method for the analysis of pesticide residues in beef fat (소지방 중 잔류농약분석을 위한 액-액분배법과 modified QuEChERS법 비교)

  • Kim, Yoen-Joo;Choi, Yoon-Hwa;Shin, Bang-Woo;Lee, Jung-Hark
    • Korean Journal of Veterinary Service
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    • v.34 no.4
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    • pp.429-439
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    • 2011
  • This article described the comparison of a quick, easy, cheap, effective, rugged and safe (QuEChERS) sample preparation and the classical method established by National Veterinary Research and Quarantine Service (NVRQS) for the determination of pesticide residues in livestock products using GC-tandem mass spectrometry. The classical method by NVRQS used liquid-liquid partioning followed by evaporizing. The modified QuEChERS entailed extraction of 2 g sample with 15 ml acetonitrile containing 1% acetic acid followed by addition of 6 g anhydrous magnesium sulfate and 1.5 g sodium acetate. After centrifugation, 6 ml of the extract underwent a cleanup step (in a technique known as column-based solid phase extraction) using 400 mg each of $C_{18}$ and primary secondary amine sorbents plus 1,200 mg magnesium sulfate. The quantitation of individual pesticides by both methods was based on tissue standard calibration curves with a correlation coefficient in excess of 0.98 for the 24 pesticides. The detection limits by the classical method were ranged 1.3~5.0 ${\mu}g$/kg, with mean recoveries between 76.2% and 114.3% except aldrin (59.3%) and deltamethrin (63.6%). The detection limits by modified QuEChERS were ranged 0.3~6.2 ${\mu}g$/kg, with mean recoveries between 68.0% and 114.3% except dimethipin (152.6%), chlorfenvinphos (138.1%), 4,4-DDT (61.5%), aldrin (60.4%) and chinomethionate (30.3%).

Quantitative Analysis of Allylmethyl Sulfide, Dimethyl Disulfide, and Dipropyl Sulfide in Biopesticides Containing Allium sativum Extract Using Gas Chromatography Mass Spectrometry-Head Space Sampler (Head-space GC-MS를 활용한 마늘추출물 함유 유기농자재 중 Allylmethyl Sulfide, Dimethyl Disulfide 및 Dipropyl Sulfide 분석)

  • Lim, Sung-Jin;Oh, Young-Tak;Kim, Jin-Hyo;Choi, Geun-Hyoung;Park, Byung-Jun
    • Korean Journal of Environmental Agriculture
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    • v.34 no.3
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    • pp.217-222
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    • 2015
  • BACKGROUND: Garlic (Allium sativum) contains polyphenols and sulfur compounds that are recognized as antioxidant, antithrombotic, anticancer, antibacterial, antimicrobial, nematicidal, and insecticidal activity. For this reason, the Environmentally-friendly Agriculture Promotion Act allowed the garlic extract as commercial biopesticide material for crop protection, nine commercial biopesticides containing A. sativum extract have been marketed in Korea. METHODS AND RESULTS: The determination of allylmethyl sulfide (AMS), dimethyl disulfide (DMDS), and dipropyl sulfide (DPS) in biopesticides containing A. sativum extract was developed and validated by gas chromatography (GC) mass spectrometry (MS) with head-space sampler. The developed method was validated, and the limit of quantification (LOQ) and recovery rates of AMS, DMDS, and DPS were 0.08, 0.32, and 0.09 mg/L and 90.3-91.3, 86.2-88.3, and 87.6-89.5%, respectively. From the nine commercial biopesticide samples, contents of AMS, DMDS, and DPS were analyzed using the developed method and results showed

A Method for Analysis of Styrene Dimer and Trimer in Foods and Containers (식품 및 용기 중 스티렌 다이머 및 트리머의 분석법)

  • Sung, Jun-Hyun;Kwon, Ki-Sung;Lee, Kwang-Ho
    • Korean Journal of Food Science and Technology
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    • v.32 no.6
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    • pp.1234-1243
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    • 2000
  • A method for quantitative determination of styrene dimer and trimer, which are suspected as endocrine disruptors, in foods and containers was studied. For residual contents of styrene dimer and trimer in two-kinds of containers, which contained instant noodle and yogurt, sample pieces were completely dissolved in tetrahydrofuran. The polymer was precipitated with n-hexane, a portion of supernatant was concentrated for analysis. A sensitive method was also optimized for the quantification of styrene dimer and trimer in foods such as instant cup noodle and yogurt by using GC/MS. Limits of Detection were about 3.2-87.0 ppb for styrene dimers and trimers. The highest recovery was obtained by extraction with acetone/hexane(1:1), followed by florisil clean-up. The levels of styrene dimer and trimer migrated by food simulants were much higher in heptane.

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Development and validation of an analytical method for the quantification of 2,6-diisopropylnaphthalene in agricultural products using GC-MS/MS

  • Lee, Han Sol;Park, Ji-Su;Lee, Su Jung;Shin, Hye-Sun;Chung, Yun mi;Choi, Ha na;Yun, Sang Soon;Jung, Yong-hyun;Oh, Jae-Ho
    • Analytical Science and Technology
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    • v.34 no.1
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    • pp.1-8
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    • 2021
  • An analytical method was developed and optimized for the quantification of a plant growth regulator, 2,6-diisopropylnaphthalene (2,6-DIPN), in agricultural products using gas chromatography-tandem mass spectrometry. The samples were extracted, partitioned, and were purified using a Florisil® cartridge. To validate the analytical method, its specificity, linearity, limit of detection (LOD) and limit of quantification (LOQ) of the instrument, LOQ of the analytical method (MLOQ), accuracy, and repeatability were considered. The method displayed excellent results during validation, and is suitable for the determination and quantification of the low residual levels of the analyte in the agricultural samples. All of the results with the optimized method were satisfactory and within the criteria ranges requested in the Codex Alimentarius Commission guidelines and the Ministry of Food and Drug Safety guidelines for pesticide residue analysis. The developed method is simple and accurate and can be used as a basis for safety management of 2,6-DIPN.

Determination of Phthalates Compounds in the Ambient Atmosphere (I) - Evaluation of a Measurement Method and its Application to a Field Study - (환경대기 중 프탈레이트 화합물의 농도 측정 (I) - 측정방법 평가와 현장 적용 -)

  • Hwang, Yoon-Jung;Park, Young-Hwa;Seo, Young-Kyo;Seo, Gwang-Kyo;Baek, Sung-Ok
    • Journal of Korean Society of Environmental Engineers
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    • v.32 no.5
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    • pp.443-454
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    • 2010
  • Phthalate compounds are widely used as plasticizers in polyvinyl chlororide (PVC) resins and other industrial consumer products, and some of them are known to be endocrine disruptors. In Korea, a number of studies have been carried out for the measurement of phthalates in consumer products and drinking water. However, no data are available for those compounds in the ambient air where the general public are routinely exposed. In this study, we evaluated sampling and analytical methods for the determination of phthalates in the ambient atmosphere. A wide range of phthalates compounds were included in the target analytes, which are dimethyl phthalate (DMP), diethyl phthalate (DEP), di-n-butyl phthalate (DBP), butyl benzyl phthalate (BBP), di(2-ethylhexyl) phthalate (DEHP), and di-n-octyl phthalate (DOP). Most of samples were collected using a high volume sampler with a PUF/XAD-2 column/quartz fiber filter and then analyzed by GC/MS. Some of samples were simultaneously collected on XAD-2 using a low-volume sampler, together with high-volume samples. The analytical method applied in this study showed good repeatability and linearity. Quantitative detection limits were estimated from 0.60 to 17.84 ng/$m^3$ in air, depending on individual compounds. The field measurements were carried out at 3 sites located in Sihwa- Banwall industrial areas and a suburban area from January 2007 to November 2007. From the field experiments, DEHP, DMP and DBP appeared to be the most abundant compounds in the ambient air. It was also found that DMP, DEP and DBP were mainly distributed in the vapor phase, while BBP, DEHP and DOP were predominantly associated with the particulate phase. The concentrations of DEHP and DMP in the industrial areas ranged from 45.7 to 1,012.7 ng/$m^3$ and from 7.7 to 375.1 ng/$m^3$, respectively. Overall, the high-volume sampling method was demonstrated to be superior to the low-volume method for the determination of phthalates in the ambient atmosphere.

Simultaneous Determination of Pesticide Residues in Soils by Dichloromethane Partition - Adsorption Chromatography - GC-ECD/NPD Analytical Methods (Dichloromethane 분배 - 흡착 크로마토그래피 - GC-ECD/NPD 분석법에 의한 토양잔류농약 다성분 분석)

  • Kim, Chan-Sub;Lee, Byung-Moo;Park, Kyung-Hun;Park, Byung-Jun;Park, Jae-Eup;Lee, Young-Deuk
    • The Korean Journal of Pesticide Science
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    • v.14 no.4
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    • pp.361-370
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    • 2010
  • Considering the efficiencies of the preparation process at each stage obtained in previous studies, the analytical determination method was established for multi-pesticide residues in soils. It consist of the acetone-extraction, the dichloromethane-partition, the Florisil or silica-gel chromatography and the gas chromatography analysis equipped with the electron capture detector and the nitrogen-phosphorus detector. In the soil recovery test by Florisil clean-up system, the number of pesticides recovered in the range of 70~120% and showed less than 20% of RSD were 165 pesticides for paddy soil, 169 pesticides for upland soil and 159 pesticides in both soils through the tested 183 pesticides. And in the soil recovery test by silica-gel system, the number of pesticides recovered in the range of 70~120% and showed less than 20% of RSD were 154 pesticides for paddy soil, 145 pesticides for upland soil, and 134 pesticides in both soils.

Determination of Octylphenol, Nonylphenol, and Di(2-ethylhexyl)phthalate in water samples (물 시료 중 Octylphenol, Nonylphenol, Di(2-ethylhexyl)phthalate의 연구)

  • Kim, Jong-Hun
    • Analytical Science and Technology
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    • v.15 no.2
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    • pp.172-179
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    • 2002
  • Determination were performed for the presence of three common environmental endocrine disrupting compounds (EDC), namely nonylphenol (NP), octylphenol (OP), di(2-ethylhexyl)phthalate (DEHP) in rainwater, distilled water, millipore water, groundwater, tap water, and bottle water in market, using OASIS cartrige extraction and GC/MS-SIM. Octylphenol was not detected in any water samples. The order of nonylphenol concentrations were increased in rainwater < millipore water < distilled water < groundwater < tap water < bottle water. The concentration of nonylphenol in bolltle water was $0.44{\mu}g/L$(ppb) at highest. Di(2-ethylhexyl)phthalates were detected in every water samples, and the concentrations were to be $1.70{\sim}2.92{\mu}g/L$ in rainwater, $8.7{\sim}31.7{\mu}g/L$ in distilled water, $0.6{\sim}5.6{\mu}g/L$(mean: $2.5{\pm}0.3{\mu}g/L$) in millipore water, and that were very stable values than other waters, $1.1{\sim}6.0{\mu}g/L$ in groundwater at near Jeonju, $3.1{\sim}5.8{\mu}g/L$ by means in tap water, $0.5{\sim}67.6{\mu}g/L$ in bottle water from market. The concentration of DEHP in bottle water samples from market were in higher than USEPA regulation at over 40%.