• Title/Summary/Keyword: Gas chromatography-mass selective detector

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The Analysis of Volatile Organic Compounds in Water by Using the Purge-and-Trap and the Gas Chromatography/Mass Selective Detector with Modified Indirect Coupling (퍼지-트랩장치와 변형된 간접 결합기를 부착한 기체크로마토그래피/질량 선택성 검출기를 이용한 물중의 휘발성 유기화합물의 분석)

  • 정영자
    • The Korean Journal of Food And Nutrition
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    • v.12 no.2
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    • pp.191-191
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    • 1999
  • A Purge & Trap Concentrator was used to analyze various volatile organic compounds(VOCs) in wat-er. The object of this study was to observe the purge efficiency of 40 VOCs in water according to the change of parameters (purge time drypurge time sample temperature) and to determine the optimum condition for VOCs using the purge & Trap concentrator interfaced with a narrow capillary connected to a gas chromatography/mass spectrometry. The optimum condition of purge and trap is as follows: purge time at 11min drypurge time at 5min sample temperature at 6$0^{\circ}C$ at constant purge flow (40mol/min) constant desorption flow(20ml/min) desorption temperature(2$25^{\circ}C$) and desorption time (1min) At this analytical condition the detection limits of VOCs was in the range of 0.1~0.5$\mu$g/ml and the purge efficiency of each compound was over 70%.

The Determination of Ethyl Isocyanate and Propyl Isocyanate by GC/FID (에틸 이소시아네이트와 프로필 이소시아네이트의 GC/FID 분석)

  • Lee, Eun-Jung;Yoo, Chul;Choi, Hong-Soon;Park, Jun-Ho;Yoon, Ju-Song;Cho, Young-Bong
    • Environmental Analysis Health and Toxicology
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    • v.15 no.1_2
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    • pp.53-59
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    • 2000
  • The purpose of this study is the development of the simple and precise determination method of ethyl isocyanate (EIC) and propyl isocyanate (PIC) through derivatization using secondary aliphatic amines by gas chromatography with flame ionization detector. The urea derivatives are quantitatively and simultaneously derived from EIC and PIC with secondary aliphatic amines such as dipropylamine, dibutylamine. and dipentylamine in methylene chloride, and confirmed by thin layer chromatography and gas chromatography with mass selective detector. For GC/FID, according to the increasing carbon atom of the amines, the retention time and peak area of the urea derivatives are increased. The instrumental detection limits for EIC and PIC were about 23.3∼34.8 $\mu\textrm{g}$ and 21.6∼28.9 $\mu\textrm{g}$, respectively.

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Determination of 5-HT2C agonist KKHQ80114 and KKHQ80109 in Rat Plasma and Urine by Gas-Chromatography/Mass Spectrometry

  • Im, Hye-Yeon;Park, Hye-Sil;Choo, Hyun-Ah;Pae, Ae-Nim;Kwon, Oh-Seung
    • Journal of Pharmaceutical Investigation
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    • v.39 no.5
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    • pp.321-325
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    • 2009
  • 5-HT$_{2C}$ receptors have been considered as therapeutic targets for the treatment of various central nervous system disorders such as depression, anxiety, epilepsy, schizophrenia and sleep disorders. We chemically synthesized KKHQ80114 (K14) and KKHQ80109 (K09), selective 5-HT$_{2C}$ agonists, with the purpose of developing therapeutic agents for the treatment of obesity. The objective of this work is to investigate analytical methods of these compounds in the plasma and urine of rats by gas chromatography/mass spectrometry. In this experiment, K14 was determined in plasma and urine by using K09 as internal standard. Calibration curves give a good linearity in plasma (r$^2$=0.9993) and urine (r$^2$=0.9988). Among hexane, ethyl acetate and diethyl ether, the highest peak was observed in diethyl ether. However, ethyl acetate was used since more interfering peaks were observed with diethyl ether. Inter-day precision and accuracy were determined in the ranges of 50-500 ng/mL for plasma and 10-500 ng/ml for urine. Quantitation limits were 50 ng/mL plasma and 25 ng/ mL urine. These data may be applicable for further studies of these compounds including absorption and metabolism due to no pharmacokinetic or analytical data available.

Analysis of 4-Nitrotoluene in Water by Gas Chromatography/Mass Spectrometry (기체크로마토그래피/질량분석기에 의한 수질시료 중 4-니트로톨루엔의 분석법 연구)

  • 이희경;권오승;류재천
    • Environmental Analysis Health and Toxicology
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    • v.15 no.1_2
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    • pp.45-51
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    • 2000
  • Analytical method of 4-nitrotoluene (4-NT) in water was developed by 9as chromatography/mass selective detector/selected ion monitoring (GC/MSD/SIM). 4-NT was extracted with diethyl ether. Organic layer was washed with 5 % sodium chloride solution. The influence of solvent and evaporation condition on extraction of 4-NT were examined. The retention time of 4-NT peak was 7.72 min. Coefficient of variation (CV) of 4-NT (ng) within day and day-to-day was ranged from 7.0 to 14.6% and from 7.7 to 20.8%, respectively. Recovery of 4-NT was ranged from 84 to 109%, and detection limit of 4-H was lese than 1 ng/㎖.

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Metabolites of Doxylamine succinate in Human Urine (인체 뇨중의 숙신산 독실아민의 대사체)

  • Eom, Khee-Dong;Jung, Byung-Hwa;Chung, Bong-Chul;Slikker, William;Park, Jong-Sei
    • YAKHAK HOEJI
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    • v.36 no.3
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    • pp.230-240
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    • 1992
  • The metabolic profile of doxylamine, N,N-dimethyl-2-[1-phenyl-1-(2-pyridinyl)ethoxy] ethanamine, was determined in the human urine. The free fractions of extracts were obtained without hydrolysis, and the conjugated fractions of extracts were obtained with enzyme hydrolysis using ${\beta}-glucuronidase/arylsulfatase$ from Helix pomatia. The mixture of acetic anhydride/pyridine (10 : 1, v : v) was used to derivatize the urinary extracts and then analyzed by gas chromatography and mass selective detector. N-desmethyldoxylamine, doxylamine carboxylic acid, desaminohydroxydoxylamine, N, N-didesmethyldoxylamine, N-acetyl conjugates of N-desmethyl and N, N-didesmethyldoxylamine, quarternary ammonium N-glucuronide of doxylamine, N-desmethyldoxylamine N-glucuronide and unchanged doxylamine were detected in the human urine obtained after oral treatment with doxylamine succinate. $N-methyl-{\alpha}-hydroxy-2-[1-phenyl-1-(2-pyridinyl)$ ethoxy] ethanamine, which can be a key intermediate of this metabolism, was tentatively identified by the interpretation of its mass spectrum. In this study, we proposed the metabolic pathway of doxylamine in the human on the basis of our data of the identified metabolites of doxylamine.

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Rapid Analysis of Major Putrefactive Metabolites by GC and GC/MSD (GC 및 GC/MSD를 이용한 주요 분변 부패산물 신속분석법)

  • 박규용;김민철;우강융;이나경;백현동
    • KSBB Journal
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    • v.18 no.1
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    • pp.74-77
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    • 2003
  • A simple, reproducible, and rapid gas chromatographic method for putrefactive metabolite determination in feces was developed. The method involves the direct injection of fecal supernatants into the gas chromatograph, without pretreatment. The mass spectra of these metabolites were obtained using an HP 5971 mass selective detector operated in electron impact (EI) ionization mode. This method produced sharp peaks and allowed the simultaneous determination of fecal putrefactive metabolites.

Installation and Test Run of Comprehensive Analysis System for SF6 in Power Equipment

  • Lee, Jeong Eun;Kim, Kwang Sin;Kim, Ah Reum;Park, Seoksoon;Kim, Kyeongsook
    • KEPCO Journal on Electric Power and Energy
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    • v.3 no.1
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    • pp.41-47
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    • 2017
  • After $SF_6$, which is being used in power equipment as an insulating material, is classified as one of the 6 major greenhouse gases, the maintenance and the refinement of used $SF_6$ started to get attention. In regard to this, KEPCO Research Institute (KEPRI) is developing $SF_6$ recovery and refinement technology starting with establishing a comprehensive $SF_6$ analysis system. With the analysis system, qualitative and quantitative analyses of the purity and the impurities of $SF_6$ before and after recovery, and before and after refinement have been carried out. The analysis system is comprised of GC-DID (Gas Chromatograph -Discharge Ionization Detector) for trace impurities analysis, GC-TCD (Thermal Conductivity Detector) for analyses of $SF_6$ purity and major impurities concentration from several hundred ppm up to percent range, GC-MSD (Mass Selective Detector) for analyses of impurities not included in standard gas, FT-IR (Fourier Transform-Infrared) Spectrometer for analysis of HF and $SO_2$, and moisture analyzer for analysis of moisture below 100 ppm. With this analysis system, complete analysis method of $SF_6$ has been established. This analysis system is being used in the maintenance of power equipment and the development of $SF_6$ recovery and refinement technologies. In this paper, the analysis results of four samples - gas and liquid phase $SF_6$ samples from a $SF_6$ refinement system before and after refinement are presented.

Pyrolysis/GC-Mass Spectrometry Analysis for Rapid Identification of Volatile Flavour Compounds of Accelerated Ripened Cheddar Cheese and Enzyme-Modified Cheese (단기숙성치즈 및 EMC 치즈의 휘발성 풍미성분 신속분석방법으로서 Pyrolysis/GC-Mass Spectrometry의 이용)

  • ;;;S.S.B. Haileselassie;V.A. Yaylayan;B.H. Lee
    • Food Science of Animal Resources
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    • v.21 no.3
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    • pp.256-264
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    • 2001
  • Pyrolysis/GC-mass spectrometry(Hewlet-Packard 5890GC/mass selective detector, 5971 BMSD), interfaced to a CDS Pyroprobe 1500 was optimized for rapid analysis of flavour compounds in Cheddar cheese. Twenty flavour compounds, including aldehydes(4), ketones(4), fatty acids(10), alcohol(1), and hydrocarbon(1), were identified from Cheddar cheeses. In total, Twenty-three flavour compounds aldehydes(2), ketones(8), alcohols(3), fatty acids(7), lactone(1), benzene derivative(1) and amide(1) were identified from two samples of accelerated-ripened Cheddar cheese treated with the proteolytic enzymes of Lactobacillus casei LGY. In total, Twenty-one flavour compounds; aldehydes(2), ketones(5), alcohols(2), fatty acids(11), and lactone(1) were identified from enzyme-modified cheese(EMC) treated with the combination of the proteolytic enzymes of Lactobacillus casei LGY and commercial endopeptidase or lipase. However, All the flavour compounds identified by pyrolysis/GC/MS in samples of ARC and EMC were not determined whether they are recognized as typical Cheddar flavour or not. More studies were requested on the development of methods for a rapid and convienent analysis of dairy fermented products using pyrolysis/GC-mass spectrometry.

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Changes in the Volatile Compounds of Artemisia capillaris Essential Oil during Storage (사철쑥 정유의 저장 중 향기성분 변화)

  • Chung, Mi-Sook
    • Korean journal of food and cookery science
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    • v.23 no.4 s.100
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    • pp.413-422
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    • 2007
  • In this study, changes in the volatile compounds of Artemisia capillaris essential oil were investigated under six different storage conditions for 6 months. The essential oil was collected by steam distillation and analyzed by a gas chromatography-mass selective detector (GC-MSD). Seventy-five volatile compounds were identified from the fresh essential oil of Artemisia capillaris. During storage, the total levels of aldehydes, alcohols, and ketones slightly decreased and the level of hydrocarbons greatly decreased; the total level of esters also decreased in the essential oil. Notably, the levels of carvacrol, eugenol, myrcene, 1,8-cineole, caryophyllene, coumarin, ${\alpha}-thujone$, ${\beta}-thujone$, borneol, and ${\gamma}-terpinene$, known as antioxidants and antimicrobial agents, decreased during storage. Finally, aerobic storage conditions caused greater reductions in some compounds even at low temperatures.

Optimization of Headspace Analysis of Volatile Compounds from Oxidized Fish Oil

  • Shin, Eui-Cheol;Jang, Hae-Jin;Lee, Hyung-Il;An, Hae-Jung;Lee, Yang-Bong
    • Preventive Nutrition and Food Science
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    • v.8 no.4
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    • pp.315-320
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    • 2003
  • Headspace volatile compounds of oxidized fish oil were analyzed by the combination of hexane solvent or solid phase microextraction, gas chromatography and mass selective detector. The optimum condition of headspace analysis by hexane trapping was 23 min absorption time, 96$^{\circ}C$ sample temperature and 20 mL/min air flow rate. The numbers of volatile compounds identified by solvent trapping and SPME were 35 and 14, respectively. Groups having the largest amount and many kinds were hydrocarbons and aldehydes, respectively. The numbers of aldehydes were 15 and 6 for solvent trap and SPME, respectively. These basic data could be used as indicators for the quality changes of fish oil.