• 제목/요약/키워드: gas chromatography-mass selective detector

검색결과 57건 처리시간 0.022초

퍼지-트랩장치와 변형된 간접 결합기를 부착한 기체크로마토그래피/질량 선택성 검출기를 이용한 물중의 휘발성 유기화합물의 분석 (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)

  • 정영자
    • 한국식품영양학회지
    • /
    • 제12권2호
    • /
    • pp.191-191
    • /
    • 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%.

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

  • 이은정;유철;최홍순;박준호;윤주송;조영봉
    • Environmental Analysis Health and Toxicology
    • /
    • 제15권1_2호
    • /
    • pp.53-59
    • /
    • 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.

  • PDF

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
    • /
    • 제39권5호
    • /
    • pp.321-325
    • /
    • 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.

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

  • 이희경;권오승;류재천
    • Environmental Analysis Health and Toxicology
    • /
    • 제15권1_2호
    • /
    • pp.45-51
    • /
    • 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/㎖.

  • PDF

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

  • 엄기동;정병화;정봉철;;박종세
    • 약학회지
    • /
    • 제36권3호
    • /
    • pp.230-240
    • /
    • 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.

  • PDF

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

  • 박규용;김민철;우강융;이나경;백현동
    • KSBB Journal
    • /
    • 제18권1호
    • /
    • pp.74-77
    • /
    • 2003
  • 대표적인 부패산물들로 잘 알려진 indole, skatole, 그리고 $\rho$-cresol 등을 측정하기 위한 방법으로 HPLC, spectrophotometric 법, 그리고 GC 및 GC/MSD 방법 등이 있으며, 수십년 간에 걸쳐 이러한 물질들의 분석이 이루어져 왔다. 본 연구에서는 많은 전처리 과정을 생략하여 분석물의 손실을 최소화하면서 GC 및 GC/MSD를 이용하여 쉽고 빠르게 측정할 수 있는 조건과 방법을 확립하였다. 측정사료는 건강한 성인 남녀의 분변이었으며, 내부 표준물질로 4-isopropylphenol을 사용하였으며, 분변 중 indole의 함량은 10~90 ppm 수준이었으며, skatole의 경우에는 약 40 ppm 정도로 검출되었다. 또한, $\rho$-cresol은 30~300 ppm 수준으로 그 분포 범위가 아주 넓게 나타났었다. GC/MSD를 이용하여 시료 중상기 물질들을 정성적으로 정확히 확인할 수 있었다. DB-17 capillary 컬럼을 이용하여 시료의 전처리 과정을 생략하여도 분석하려던 부패산물의 정성 및 정량에 방해되는 불순 peak는 없었고, 분리능도 매우 우수하였으므로 보다 빠르고 신속하게 상기 물질들을 확인할 수 있었다. 향후 본 연구를 통해 개발된 신속분석법이 분변에 존재하는 주요 부패산물들의 정량에 유용하게 사용되리라 판단된다.

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
    • /
    • 제3권1호
    • /
    • pp.41-47
    • /
    • 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.

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

  • 박승용;허강칠;신중엽
    • 한국축산식품학회지
    • /
    • 제21권3호
    • /
    • pp.256-264
    • /
    • 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.

  • PDF

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

  • 정미숙
    • 한국식품조리과학회지
    • /
    • 제23권4호통권100호
    • /
    • pp.413-422
    • /
    • 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
    • /
    • 제8권4호
    • /
    • pp.315-320
    • /
    • 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.