• 제목/요약/키워드: Gas chromatography-mass spectrometer

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대기 유기질소화합물의 분석방법 및 농도 (Review on the Analytical Methods and Ambient Concentrations of Organic Nitrogenous Compounds in the Atmosphere)

  • 최나래;김용표
    • 한국대기환경학회지
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    • 제34권1호
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    • pp.120-143
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    • 2018
  • The analytical methods and their ambient levels of organic nitrogenous compounds such as nitrosamines, nitramines (nitroamines), imines, amides and nitro-polycyclic aromatic hydrocarbons (nitro-PAHs) in the atmosphere are summarized and discussed. Sampling for the analysis of organic nitrogenous compounds was mostly conducted using high volume air sampler. The direct liquid extraction (DLE) using sonification and the pressurized liquid extraction (PLE) using the accelerated solvent extraction (ASE) have been frequently employed for the extraction of organic nitrogenous compounds in the atmospheric samples. After extraction, clean-up via filtration and the solid phase extraction (SPE) and concentrations using nitrogen and rotary evaporator have been generally conducted but in some studies the clean-up and concentration steps have been omitted to prevent the loss of analyte and improve the recovery rate of the analytical procedure. Instrumental analysis was mainly carried out using gas chromatography (GC) or the high performance liquid chromatography (HPLC) coupled with the single quadrupole mass spectrometer or tandem mass spectrometer in the electron ionization (EI), positive chemical ionization (PCI) and negative chemical ionization (NCI) mode and analysis sensitivity of nitrosamines and nitramines were higher in NCI mode. Desirable sampling and analysis methods for analyzing particulate organic nitrogenous compounds are suggested.

복어로부터 복어독(Tetrodotoxin) 생성능이 있는 해양 미생물의 분리 및 동정 (Isolation and Identification of Tetrodotoxin-producing Marine Microorganism from Pufferfish)

  • 윤성준;차병윤;이명자;정동윤;송병권;김희숙;김동수;이은열
    • 생명과학회지
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    • 제9권6호
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    • pp.653-658
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    • 1999
  • A novel marine microorganism, Vibrio sp. YE-101, was isolated from pufferfish and investigated for its ability to synthesize tetrodotoxin (TTX). Various strains isolated from the intestine of pufferfish were grown on TCBS agar plate, and then cultured on Ocean Research Institute (ORI) medium supplemented with 3% NaCl at 23$^{\circ}C$ for 3days. The cells were harvested, disrupted, fractionated by Bio-Gel P-2 column chromatography and then TTX-producing strain, Vibrio sp. YE-101, was identified using mouse bioassay. The isolated TTX from Vibrio sp. YE-101 was also analyzed and identified by HPLC and gas chromatography-mass spectrometer (GC-MS). The mass fragmentation of trimethylsilyl derivatives of C9-base of TTX from Vibrio sp. YE-101 was interpreted and the pattern of fragmentation was same with that of authentic standard. The purfied TTX was also positive to the mouse bioassay, which clearly represents that Vibrio sp. YE-101 can synthesize TTX.

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Glycyrrhizic acid 와 Glycyrrhetinic acid의 열분해에 관한 연구 (Study on the Pyrolysis of Glycyrrhizic acid and Glycyrrhetinic acid)

  • 이문수;김옥찬
    • 한국연초학회지
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    • 제8권2호
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    • pp.59-66
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    • 1986
  • The Pyrolytic behavior of glycyrrhizic acid and glycyrrhetini c acid, which are natural flavorants for manufactured cigarettes was observed to find its contribution to the smoke composition. Pyrolyzates of them at 800t were identified using a gas chromatography and a mass spectrometer. According to the analysis of the pyrolytic Products, 43 different compounds were identified Among them the aromatic hydrocarbon compounds were found to be the major products.

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2차원 가스크로마토그래프를 이용한 해상유출유 감식기법 연구 (Study for Oil Spill Source Identification by Comprehensive Two Dimensional Gas Chromatography)

  • 이완섭;이상진;김차수;오현정;김한규
    • 해양환경안전학회:학술대회논문집
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    • 해양환경안전학회 2006년도 추계학술발표회
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    • pp.169-174
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    • 2006
  • 모든 원유 (crude oil)와 제품유 (petroleum product)는 서로 구별되는 탄화수소특성을 가지고 있다. 원유의 경우 산지별로 고유한 특성을 지니고 있으며, 제품유의 경우 같은 유종이라 할지라도 그 원료가 되는 원유의 특성, 생산공정, 생산시기 등에서 차이점이 발생한다. 즉, 생산시기가 동일하다 할지라도 선박의 연료탱크내에 남아있는 잔류유와의 혼합 동에 의해 구별되는 특징을 가지게 되며 이러한 특성을 이용한 기법을 유지문기법(oil fingerprint method) 이라 한다. 본 연구에서는 최근 새로운 유지문기법으로 활용 가능성이 대두되고 있는 2 차원 가스크로마토그래프 (Comprehensive Two Dimensional Gas Chromatography)를 이용하여 기존의 가스크로마토그래프 (GC)와 가스크로마토그래프 질량분석기 (GC/MS) 와의 분석방법 비교 등을 통해 유지문 분석기법의 실효성에 대해서 논하고자 한다.

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Validation of an analytical method for cyanide determination in blood, urine, lung, and skin tissues of rats using gas chromatography mass spectrometry (GC-MS)

  • Shin, Min-Chul;Kwon, Young Sang;Kim, Jong-Hwan;Hwang, Kyunghwa;Seo, Jong-Su
    • 분석과학
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    • 제32권3호
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    • pp.88-95
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    • 2019
  • This study was conducted to establish the analytical method for the determination of cyanide in blood, urine, lung and skin tissues in rats. In order to detect or quantify the sodium cyanide in above biological matrixes, it was derivatized to Pentafluorobenzyl cyanide (PFB-CN) using pentafluorobenzyl bromide (PFB-Br) and then reaction substance was analyzed using gas chromatography mass spectrometer (GC/MS)-SIM (selected ion monitoring) mode. The analytical method for cyanide determination was validated with respect to parameters such as selectivity, system suitability, linearity, accuracy and precision. No interference peak was observed for the determination of cyanide in blank samples, zero samples and lower limit of quantification (LLOQ) samples. The lowest limit detection (LOD) for cyanide was $10{\mu}M$. The linear dynamic range was from 10 to $200{\mu}M$ for cyanide with correlation coefficients higher than 0.99. For quality control samples at four different concentrations including LLOQ that were analyzed in quintuplicate, on six separate occasions, the accuracy and precision range from -14.1 % to 14.5% and 2.7 % to 18.3 %, respectively. The GC/MS-based method of analysis established in this study could be applied to the toxicokinetic study of cyanide on biological matrix substrates such as blood, urine, lung and skin tissues.

목질(木質) 폐재(廢材)의 열(熱)-화학적(化學的) 방법에 의한 메틸알콜과 대체(代替)에너지 가스의 합성(合成)(I) - 알카리염(鹽)을 촉매로 사용한 톱밥, 볏집 그리고 왕겨의 열화학적(熱化學的) 분해(分解) - (Synthesis of Methyl Alcohol and Alternative Gases for Petroleum by Thermochemical Gasification of Waste Lignocellulosic Materials (I) - Thermochemical Conversion of Sawdust, Ricestraw and Ricehusk Using Alkali Salts as Catalyst -)

  • 이병근
    • Journal of the Korean Wood Science and Technology
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    • 제14권2호
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    • pp.21-28
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    • 1986
  • 목질물질(木質物質)인 톱밥, 볏짚 그리고 왕겨를 열분해(熱分解)하여 기상물질(氣相物質)을 합성(合成)하기 위해, 석영으로 설계 제작된 반응탑(反應塔)을 사용하였다. 최초의 반응온도 350$^{\circ}C$로부터 열분해(熱分解)와 gasification 반응(反應)이 완결된다고 예상되는 550$^{\circ}C$까지 가열하였다. 촉매가 반응온도에 어떤 영향을 미치는지 조사하기 위해 $K_2CO_3$$Na_2CO_3$를 촉매로 사용하였다. 합성(合成) gas chromatograph와 mass spectrometer에 의해 CO, $CO_2$, $CH_4$ 그리고 $CH_3CHO$등인 것으로 판명되었다. 합성(合成) gas의 수율(收率)과 조성(組成)은 반응온도(反應溫度)와 이 반응에 사용되는 촉매에 달려있지만, 톱밥을 시료(試料)로 반응온도 550$^{\circ}C$, $K_2CO_3$를 촉매로 사용한 반응(反應)에서 생성되는 gas 체적(體積)은 1,800$m{\ell}$/g 톱밥에 달한다.

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Single cell-strain부터 유래된 무세포 효소 시스템을 이용한 톨루엔 및 아세트산 분해 (Degradation of Toluene and Acetic Acid Using Cell-Free Enzyme System from Single Cell-Strain)

  • 장재현;김예지;노태용;박중곤
    • Korean Chemical Engineering Research
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    • 제54권5호
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    • pp.665-670
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    • 2016
  • 본 연구에서는 톨루엔 분해 균주인 Pseudomonas putida와 아세트산 분해 균주인 Cupriavidus necator에 무세포 효소 시스템(cell-free enzyme system)을 적용하여 톨루엔과 아세트산에 대한 분해 가능성을 확인하는 실험을 수행하였다. P. putida는 톨루엔 존재 하에서만 toluene dioxygenase를 생성하여 톨루엔을 cis-toluene dihydrodiol로 분해하며, C. necator는 acetyl coenzyme A synthetase-1을 생성하여 아세트산을 acetyl CoA로 전환시켜 생존에 필요한 ATP나 생분해성(biodegradable) 고분자인 Polyhydroxyalkanoate (PHA)를 합성한다. P. putida의 톨루엔 분해 효소인 toluene dioxygenase는 유도효소이기 때문에 toluene dioxygenase 생성 전과 후로 나누어 실험을 진행하였다. P. putida의 톨루엔 분해능력 확인을 위한 gas chromatography (GC) 분석 결과, 대조군과 toluene dioxygenase 생성 전인 실험군 1에서는 검출된 톨루엔의 양이 거의 유사하였으나, toluene dioxygenase 생성 후인 실험군 2에서는 검출된 톨루엔의 양이 대조군 및 실험군 1에 비해 감소하였다. 또한 C. necator의 아세트산 분해능력 확인을 위한 gas chromatography-mass spectrometer (GC-MS) 분석 결과, 무세포 효소 시스템을 적용한 실험군에서는 아세트산에 대한 피크가 검출되지 않았다. 따라서 P. putida와 C. necator는 무세포 효소 시스템 적용 후에도 톨루엔 및 아세트산 분해 능력이 유지되었으나, P. putida는 무세포 효소 시스템을 적용하기 전에 유도 효소를 생성하는 과정이 필요하다.

기체 크로마토그래피 질량 분석법을 이용한 다크닝 샴푸의 성분 분석 및 안전성에 관한 연구 (A Study on the Analysis of Ingredients and Safety of Darkening Shampoo using Gas Chromatography Mass Spectrometer (GC-MS))

  • 김유리;김운중
    • 산업진흥연구
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    • 제9권1호
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    • pp.13-20
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    • 2024
  • 본 연구에서는 국내 시장에서 판매되는 다크닝 샴푸 5종에 대한 성분 분석을 실시하고, 그 결과를 바탕으로 해당 제품들의 유효 성분과 안전성에 대해 평가하였다. GC-MS 분석을 통해 각 샴푸의 주요 성분을 확인한 결과, 제조사가 표기한 전성분 목록과 일부 차이가 있는 화합물들이 검출되었다. 이는 GC-MS 분석의 한계와 특정 화합물의 휘발성 여부에 따른 것으로 해석된다. 이러한 분석을 바탕으로, 모발의 색상 변화에 기여할 가능성이 있는 화합물을 조사하였다. 그러나 이러한 화합물들이 모발 다크닝 과정 자체에 직접적으로 관련된 역할을 하는 성분이라고 단정지을 수는 없었다. 다만 헤어 케어 제품의 성능을 향상시키고 모발에 대한 일부 추가적인 이점을 제공하거나 제품의 질감, 안정성 또는 보존 등의 특성을 향상시키는 역할을 하는 것으로 추정할 수 있었다. 또한 GC-MS 성분 분석 결과, 확인된 성분 중 안전성이 우려되는 화합물에 대한 조사를 통해 화장품 원료로 사용될 경우 주의가 필요한 몇 가지 화합물에 대한 정보를 제시하였다.

Analysis of Agrochemical Residues in Tobacco Using Solid Phase Microextraction-Gas Chromatography with Different Mass Spectrometric Techniques

  • Lee, Jeong-Min;Jang, Gi-Chul;Kim, Hyo-Keun;Hwang, Geon-Joong
    • 한국연초학회지
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    • 제30권2호
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    • pp.117-124
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    • 2008
  • A solid phase microextraction (SPME) method in combination with gas chromatography/mass spectrometric techniques was used for the extraction and quantification of 12 selected agrochemical residues in tobacco. The parameters such as the type of SPME fiber, adsorption/desorption time and the extraction temperature affecting the precision and accuracy of the SPME method were investigated and optimized. Among three types of fibers investigated, polyacrylate (PA), polydimethylsiloxane (PDMS) and polydimethylsiloxane-divinylbenzene (PDMS-DVB), PDMS fiber was selected for the extractions of the agrochemicals. The SPME device was automated and on-line coupled to a gas chromatograph with a mass spectrometer. Mass spectrometry (MS) was used and two different instruments, a quadrupole MS and triple quadrupole MS-MS mode, were compared. The performances of the two GC-MS instruments were comparable in terms of linearity (in the range of 0.01$\sim$0.5 $\mu$g/mL) and sensitivity (limits of detection were in the low ng/mL range). The triple quadrupole MS-MS instrument gave better precision than that of quadrupole MS system, but generally the relative standard deviations for replicates were acceptable for both instruments (< 15%). The LODs was fully satisfied the requirements of the CORESTA GRL. Recoveries of 12 selected agrochemicals in tobacco yielded more than 80% and reproducibility was found to be better than 10% RSD so that SPME procedure could be applied to the quantitative analysis of agrochemical residues in tobacco.

A comparison study of extraction methods for bio-liquid via hydrothermal carbonization of food waste

  • Bang, YeJin;Choi, Minseon;Bae, Sunyoung
    • 분석과학
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    • 제31권3호
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    • pp.112-121
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    • 2018
  • The hydrothermal carbonization method has received great attention because of the conversion process from biomass. The reaction produces various products in hydrochar, bio-liquid, and gas. Even though its yield cannot be ignored in amount, it is difficult to find research papers on bio-liquid generated from the hydrothermal carbonization reaction of biomass. In particular, the heterogeneity of feedstock composition may make the characterization of bio-liquid different and difficult. In this study, bio-liquid from the hydrothermal carbonization reaction of food wastes at $230^{\circ}C$ for 4 h was investigated. Among various products, fatty acid methyl esters were analyzed using two different extraction methods: liquid-liquid extraction and column chromatography. Different elutions with various solvents enabled us to categorize the various components. The eluents and fractions obtained from two different extraction methods were analyzed by gas chromatography with a mass spectrometer (GC/MS). The composition of the bio-liquid in each fraction was characterized, and seven fatty acid methyl esters were identified using the library installed in GC/MS device.