• 제목/요약/키워드: GC/MS spectrometry

검색결과 752건 처리시간 0.028초

헤드스페이스-가스크로마토그래피-질량분석법에 의한 체모 중 포름알데하이드 측정법 연구 (The Study on the Measurement of Formaldehyde in Hair by HS-GC-MS)

  • 신호상;안혜실
    • 한국환경보건학회지
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    • 제32권1호
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    • pp.67-70
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    • 2006
  • A gas chromatography/mass spectrometric method was developed for the determination of formaldehyde in hair. 0.3mg of hair was placed in 10ml headspace vial. 1.5mM pentafluorophenylhydrazine solution (pH 2) in 0.03 M phosphoric acid and $20\;{\mu}l$ of 500 mg/l $acetone-d_6$ as internal standard were added in vial and sealed tightly with cap. The solution was heated for 30 min at $90^{\circ}C$ in heating block. The extraction, the derivatization and the evaporation were performed simultaneously. After heating of the solution, 0.5 ml of headspace was taken up and analyzed by gas chromatography-mass spectrometry (GC-MS). Low limit of detection (LaD) and Low limit of quantitation (LOQ) of formaldehyde were 0.5 and 1.5 ng/g, respectively. The method was used to analyze formaldehyde in rat hair after oral exposure. The developed method may be valuable to be used to analyze formaldehyde in human hair.

Simultaneous Determination of Valproic Acid and its Toxic Metabolites, 4-ene-VPA and 2,4-diene-VPA in Rat Plasma using a Gas Chromatographic-mass Spectrometric Method

  • Lee, Min-Sun;Lee, Young-Joo;Chung, Bong-Chul;Jung, Byung-Hwa
    • Journal of Pharmaceutical Investigation
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    • 제40권3호
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    • pp.155-160
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    • 2010
  • A gas chromatographic-mass spectrometric (GC-MS) method was developed for the simultaneous determination of valproic acid (VPA) and its toxic metabolites, 4-ene-VPA and 2,4-diene-VPA in rat plasma. Extraction was performed in weak acidic condition (pH 5.2) to avoid degradation of 4-ene-VPA and 2,4-diene-VPA. The recoveries for 4-ene-VPA and 2,4-diene-VPA were more than 70% and that for VPA was 33-42%. R value for each compounds exceeded 0.998 in calibration curve during all the analysis. Accuracy and precision ranged from 88.3 to 113.2% and from 2.16 to 14.2%, respectively The method was successfully applied to monitor plasma concentrations of VPA, 4-ene-VPA and 2,4-diene-VPA after intravenous administration of VPA at the dose of 100 mg/kg, suggesting that these toxic metabolites may involved in the hepatotoxicity induced by VPA.

Characterization of Fennel Flavors by Solid Phase Trapping-Solvent Extraction and Gas Chromatography-Mass Spectrometry

  • Shin, Yeon-Jae;Jung, Mi-Jin;Kim, Nam-Sun;Kim, Kun;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • 제28권12호
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    • pp.2389-2395
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    • 2007
  • Headspace solid phase trapping solvent extraction (HS-SPTE) and GC-MS was applied for the characterization of volatile flavors from fennel, anise seed, star-anise, dill seed, fennel bean, and Ricard aperitif liquor. Tenax was used for HS-SPTE adsorption material. Recoveries, precision, linear dynamic ranges, and the limit of detection in the analytical method were validated. There were some similarities and distinct differences between fennel-like samples. The Korean and the Chinese fennels contained trans-anethole, (+)-limonene, anisealdehyde, methyl chavicol as major components. The volatile aroma components from star anise were characterised by rich trans-anethole, (+)-limonene, methyl chavicol, and anisaldehyde. Additionally, principal component analysis (PCA) has been used for characterizing or classifying eight different fennel-like samples according to origin or other features. A quite different pattern of dill seed was found due to the presence of apiol (dill).

원유와 석유제품 중의 다환방향족탄화수소류[PAHs] 분포특성과 발생원 (Compositional Characteristics and Origin of Polycyclic Aromatic Hydrocarbons[PAHs] of Crude Oils and Petroleum Products)

  • 정흥호;박은희;최상원
    • 한국환경과학회지
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    • 제15권5호
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    • pp.397-403
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    • 2006
  • Compositional characteristics and origin of polycyclic aromatic hydrocarbons(PAHs), which should be strongly regulated for environmental protection in the crude oils and petroleum products, have been investigated by gas chromatography-mass spectrometry(GC/MS). In the crude oils analyzed, two-rings compound(naphthalene) of PAHs was detected around $72.3\sim93.5%$, but five- or six-rings compound of PAHs was not detected. In the crude oils analyzed, the molecular ratio indices of Phe/Ant(phenanthrene/anthracene)>15, Fla/Pyr(fluoranthene/pyrene)<1, BaA/Chr(benzo (a)anthracene/chrysene)$\leq0.4$ could be effectively applied, and we found that the origin of PAHs was petrogenic sources. Total PAHs concentrations in the crude oils were increased with increasing API gravity and with decreasing sulfur contents of the analyzed crude oils. Five- or six-rings compound of PAHs were not included in ail petroleum products except bunker-C. Furthermore, the molecular ratio indices of Phe/Ant(phenanthrene/anthracene) vs. Fla/Pyr(fluoranthene/pyrene) could be effectively applied as the standard for the PAHs contamination criterion at the other Korean areas.

Fiber내 유도체화/HS-SPME를 이용한 수용액 시료 중 휘발성 지방산의 분석 (Determination of Volatile Fatty Acids in Aqueous Samples by HS-SPME with In-Fiber Derivatization)

  • 안윤경;이지연;김지형;홍종기
    • 분석과학
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    • 제16권6호
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    • pp.458-465
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    • 2003
  • 수용액 시료 중 휘발성 지방산을 HS (headspace)-SPME (Solid phase microextraction)를 이용하여 간편하고 빠르게 분석하는 방법에 대하여 연구하였다. 1-Pyrenyldiazomethane (PDAM)을 이용한 화이버 내 유도체화를 통하여 휘발성 지방산의 검출감도를 향상시킬 수 있었으며, SPME 추출조건으로 pH, 염 효과 및 초음파 추출에 대하여 조사하였다. 본 연구에서 개발된 방법을 기반으로 실제 폐수 중 휘발성 지방산을 추출하여 기체크로마토그래피/질량분석기-선택이온검색법으로 정량 분석하였다.

ZnO를 첨가한 PVC와 PS 혼합물의 열분해 특성에 관한 연구 (A Study on the Co-pyrolysis Characteristics of PVC and PS Mixtures with ZnO)

  • 오세천;정명욱;김희택;이해평
    • 공업화학
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    • 제16권4호
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    • pp.513-518
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    • 2005
  • 혼합비율 및 반응온도의 변화에 따른 ZnO가 첨가된 PVC와 PS의 혼합 열분해 특성에 관한 연구를 TG와 GC-MS를 이용하여 수행하였다. 본 연구로부터 혼합물에 있어서 PS의 양이 증가할수록 액상 생성물은 증가하였으며 기상 생성물은 감소함을 알 수 있었다. 또한 ZnO의 첨가량이 증가할수록 기상 생성물과 염화수소의 발생량은 감소하였으며 염화수소의 발생 억제 및 액상 생성물의 최대수율을 얻기 위한 최적의 반응온도는 $500^{\circ}C$임을 알 수 있었다.

Formation of Polybrominated Dibenzo-p-dioxins/Furans (PBDDs/Fs) by the Pyrolysis of 2,4-Dibromophenol, 2,6-Dibromophenol, and 2,4,6-Tribromophenol

  • Na, Yun-Cheol;Hong, Jong-Ki;Kim, Kang-Jin
    • Bulletin of the Korean Chemical Society
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    • 제28권4호
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    • pp.547-552
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    • 2007
  • This study examined the thermal reactions of 2,4-dibromophenol (diBP), 2,6-diBP and 2,4,6-triBP. The products obtained under pyrolytic conditions were analyzed by gas chromatography/mass spectrometry (GC/MS). 2,7-dibromodibenzo-p-dioxin (diBDD) was the major compound produced from the thermal reaction of 2,4-diBP. In addition, monoBDD and triBDDs were obtained through a process of debromination and bromination, respectively. The pyrolysis of 2,6-diBP and 2,4,6-triBP produced two major brominated dioxin isomers through direct condensation and a Smiles rearrangement. The two ortho-Brs in 2,6-diBP and 2,4,6-triBP mainly led to the production of dioxins, whereas in addition to 2,7-diBDD, 2,4-diBP produced two furans as minor products, 2,8-dibromodibenzofuran (diBDF) and 2,4,8-triBDF, through the intermediate dihydroxybiphenyl (DOHB). The maximum yield of the major dioxins was obtained at 400 oC, and decomposition by debromination at 500 oC resulted in less substituted bromodioxins.

전라남도 지역의 하천수에 존재하는 내분비 장애물질(Bisphenol A와 Styrene oligomer)의 실태조사 (Monitoring of Endocrine Disruptors (Bisphenol A and Styrene Oligomers) in the Streams of Cholla-namdo Province in South Korea)

  • 박송인;정선용;;;나숙현
    • 한국물환경학회지
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    • 제28권5호
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    • pp.669-675
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    • 2012
  • Recently, there have been active researches regarding endocrine-disrupting chemicals (EDCs). In this study, fifteen small freshwater streams in Cholla-namdo province, South Korea were investigated with respect to the concentration of the endocrine disruptors - Bisphenol A (BPA), styrene monomer (SM), styrene dimer (SD), and styrene trimer (ST) by gas chromatography-mass spectrometry (GC-MS). Measured concentration of the target compounds in the sampled water ranged from

Estimation of Korean Adult's Daily Intake of Ethyl Carbamate through Korean Commercial Alcoholic Beverages Based on the Monitoring

  • Ha, Mi-Sun;Hu, Soo-Jung;Park, Hee-Ra;Lee, Hyo-Min;Kwon, Ki-Sung;Han, Eun-Mee;Kim, Kyung-Mi;Ko, Eun-Jung;Ha, Sang-Do;Bae, Dong-Ho
    • Food Science and Biotechnology
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    • 제15권1호
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    • pp.112-116
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    • 2006
  • Levels of ethyl carbamate, by-product produced naturally during fermentation, in Korean alcoholic beverages were determined by Gas Chromatography/mass spectrometry/selected ion mode (GC/MS/SIM), and their daily intake by Korean adult group was estimated. In GC/MS/SIM analysis 0.8-10.1, 0.5-0.8, 0.4-0.9, 3.5-689.9, 8.4-30.3, 13.9-30.0, and 1.7-11.7 ppb of ethyl carbamate were detected in soju, beer, takju, fruit wine, cheongju, whiskey, and grape wine, respectively. Maximum daily exposure of ethyl carbamate through alcoholic beverage consumption was 7.41 ng/kg body weight/day for average Korean male, with one soju brand and two fruit wine brands showing high ethyl carbamate level.

Poly(dimethylsiloxane) Mini-disk Extraction

  • Cha, Eun-Ju;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • 제32권10호
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    • pp.3603-3609
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    • 2011
  • A novel sampling method of the headspace poly(dimethylsiloxane) (PDMS) mini-disk extraction (HS-PDE) was developed, optimized, validated and applied for the GC/MS analysis of spices flavors. A prototype PDMS mini-disk (8 mm outer diameter, 0.157 mm thickness, 9.4 mg weight) has been designed and fabricated as a sorption device. The technique uses a small PDMS mini-disk and very small volume of organic solvent and less sample size than the solvent extraction. This new HS-PDE method is very simple to use, inexpensive, rapid, requires less labor. Linearities of calibration curves for ${\alpha}$-pinene, ${\beta}$-pinene, limonene and ${\gamma}$-terpinene by HS-PDE combined with GC/MS were excellent having $r^2$ values greater than 0.99 at the dynamic range of 6.06~3500 ng/mL. The limit of detection (LOD) and the limit of quantitation (LOQ) showed very low values. This method exhibited good precision and accuracy. The overall extraction efficiency of this method was evaluated by using partition coefficients ($K_p$) and concentration factors (CF) for several characteristic components from nutmeg and mace. Partition coefficients were in the range from $2.04{\times}10^4$ to $4.42{\times}10^5$, while CF values were 0.88-15.03. HS-PDE was applied successfully for the analysis of flavors compositions from nutmeg, mace and cumin. The HS-PDE method is a very promising sampling technique for the characterization of volatile flavors.