• Title/Summary/Keyword: Gas chromatography-mass spectrometry (GC/MS)

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교반막대 추출법과 GC-MS/MS를 이용한 수중의 합성 향물질류 분석 (Analysis of Synthetic Fragrances (SFs) in Water Using Stir Bar Sorptive Extraction (SBSE) and GC-MS/MS)

  • 서창동;손희종;염훈식;최진택;류동춘;권기원;장성호
    • 대한환경공학회지
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    • 제36권6호
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    • pp.387-395
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    • 2014
  • 본 연구에서는 SBSE 전처리 장치와 GC-MS/MS를 이용하여 합성 향물질 11종을 동시 분석할 수 있는 분석법을 개발하기 위해 흡착 bar의 교반시간, 교반속도, 시료수의 pH, 시료수 용량, 염석제 투입량 및 메탄올 주입량 변화 등 SBSE (stir bar sorptive extraction) 전처리 조건과 GC-MS/MS (gas chromatography/tandem mass spectrometry)의 기기조건을 다양하게 변화시켜 SBSE-GC-MS/MS를 이용한 분석법을 개발하였다. 11종의 합성 향물질들에 대한 검출한계(LOD)는 2.1~4.1 ng/L였으며, 정량한계(LOQ)는 6.6~12.9 ng/L였다. 수돗물, 낙동강 원수, 하수처리장 최종방류수 및 해수를 이용하여 시료수의 matrix 영향을 살펴본 결과, 11종의 합성 향물질들의 회수율 및 RSD의 경우 각각 88%~119% 및 0.8%~7.5%로 양호한 결과를 나타내어 시료수의 matrix 영향을 받지 않는 것으로 나타났다. 본 연구에서 개발된 SBSE-GC-MS/MS 분석법은 40 mL 정도의 적은 시료수량으로도 고감도 분석이 가능하며, 용매류를 사용하지 않기 때문에 분석자의 건강 및 환경친화적인 분석법이라는 장점뿐만 아니라 간편하고, 빠르며 자동화된 방법이라는 장점을 가진다.

화학적 폐수처리 중 GC/MS에 의한 폐놀생성 규명에 관한 연구 (A Study on the Identification of Phenol Production by GC/MS under Chemical Treatment of Industrial Wastewater)

  • 박선구;고오석;신대윤
    • 한국환경과학회지
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    • 제9권1호
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    • pp.89-93
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    • 2000
  • Twenty organic chemical substances(Table 2) were isolated from untreated wastewater, as well as treated wastewater, collected at 76 companys of 9 industry group located in the basin of Youngsan River. Those organic compounds were analyzed by Gas Chromatography/Mass Spectrometry(GC/MS) and confirmed through comparison with each standard reagents. Phenol, which was not detected in the raw wastewater, was identified in the effluent of treatment facility, indicating that phenol is generated from isopropylbenzene of plant wastewater.

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Direct Analysis of Tackifying Resins in Vulcanized Rubber by Simultaneous Pyrosis Methylation-Gas Chromatography/Mass Spectrometry

  • 김승욱;허귀숙;이계호
    • Bulletin of the Korean Chemical Society
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    • 제19권2호
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    • pp.164-169
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    • 1998
  • Vulcanized rubber containing three kinds of oligomeric resins such as cashew resin, t-octylphenol formaldehyde resin and terpene modified wood rosin has been characterized by simultaneous pyrolysis methylation-gas chromatography/mass spectrometry (SPM-GC/MS). After methylation by the SPM method using tetramethylammonium hydroxide, the methylated pyrolyzates of the corresponding resins were detected with higher sensitivity than underivatized pyrolyzates without any interferences from other ingredients of vulcanized rubber.

Identification of urinary metabolite(s) of CKD-712 by gas chromatography/mass spectrometry in rats

  • Jean, Hee-Kyung;Choi, Hae-Yeon;Kim, Youn-Jung;Kwon, Oh-Seung;Ryu, Jae-Chun
    • 대한약학회:학술대회논문집
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    • 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.1
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    • pp.314.1-314.1
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    • 2003
  • Examination was made of the urinary metabolite(s) of CKD-712, which is a chiral compound, named S-YS49 derived from higenamine (one component of Aconite spp.) derivatives. First of all. to analyze the metabolite(s) of CKD-712, a simple and sensitive detection method for CKD-712 was developed by using gas chromatography-mass spectrometry(GC/MS). (omitted)

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Quality Assessment of Curcuma longa L. by Gas Chromatography-Mass Spectrometry Fingerprint, Principle Components Analysis and Hierarchical Clustering Analysis

  • Li, Ming;Zhou, Xin;Zhao, Yang;Wang, Dao-Ping;Hu, Xiao-Na
    • Bulletin of the Korean Chemical Society
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    • 제30권10호
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    • pp.2287-2293
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    • 2009
  • Gas Chromatography-Mass Spectrometry (GC-MS) fingerprint analysis, Principle Components Analysis (PCA), and Hierarchical Cluster Analysis (HCA) were introduced for quality assessment of Curcuma longa L. (C. longa). The GC-MS fingerprint method was developed and validated by analyzing 33 batches of samples of C. longa from different geographic locations. 18 chromatographic peaks were selected as characteristic peaks and their relative peak areas (RPA) were calculated for quantitative expression. Two principal components (PCs) were extracted by PCA. C. longa collected from Guizhou and Fujian were separated from other samples by PC1, capturing 71.83% of variance. While, PC2 contributed for their further separation, capturing 11.13% of variance. HCA confirmed the result of PCA analysis. Therefore, GC-MS fingerprint study with chemometric techniques provides a very flexible and reliable method for quality assessment of C. longa.

Identification of Propentofylline Metabolites in Rats by Gas Chromatography/Mass Spectrometry

  • Kwon, Oh-Seung;Ryu, Jae-Chun
    • Archives of Pharmacal Research
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    • 제23권4호
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    • pp.374-380
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    • 2000
  • Propentofylline (PPF, 3-methyl-1-(5-oxohexyl)-7-propylxanthine) has been reported to be a compound for treatment of both vascular dementia and dementia of the Alzheimer type. The short half-life (about 15 min) of PPF at the terminal elimination phase and poor bioavailability after oral administration of PPF to rabbits (Kim et al., 1992) suggest in part that this drug takes the extensive first-pass metabolism in the liver. In addition, the metabolic pathway for PPF remains unclear. The objective of this experiment is to identify urinary metabolites of PPF in rats. For the identification of the metabolites, rat urine was collected after oral administration of 100${m}g/kg$ PPF. PPF metabolite, 3-methyl-1-(5-hydroxyhexyl)-7-propylxanthine, was synthesized and confirmed by gas chromatography/mass spectroscopy (GC/MS) and $^1H$ nuclear magnetic resonance spectroscopy. The urinary metabolites of PPF were extracted with diethyl ether and identified by electron impact and chemical ionization GC/MS. One urinary metabolite was confirmed to be 3-methyl-1-(5-hydroxyhexyl)-7-propylxanthine by synthesized authentic compound. Several metabolites of monohydroxy- and dihydroxy-PPF were identified based on mass fragmentation of both intact and trimethylsilylated derivatives of PPF metabolites and the novel structure of these metabolites is suggested based on mass spectra.

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Isotope-Dilution Mass Spectrometry for Quantification of Urinary Active Androgens Separated by Gas Chromatography

  • Lee, Su-Hyeon;Choi, Man-Ho;Lee, Won-Yong;Chung, Bong-Chul
    • Mass Spectrometry Letters
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    • 제1권1호
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    • pp.29-32
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    • 2010
  • Cross reacting antibodies can cause an overestimation of the results of immunoassays. Therefore, alternative methods are needed for the accurate quantification of steroids. Gas chromatography combined with isotope-dilution mass spectrometry (GC-IDMS) is developed to quantify urinary active androgens, testosterone, epitestosterone and dihydrotestosterone, which are clinically relevant androgens to both hair-loss and prostate diseases. The method devised involves enzymatic hydrolysis with $\beta$-glucuronidase, solid-phase extraction, liquid-liquid extraction using methyl tert-butyl ether and subsequent conversion to pentafluorophenyldimethylsilyl-trimethylsilyl (flophemesyl-TMS) derivatives for sensitive and selective analysis in selected-ion monitoring mode. Flophemesyl-TMS derivatization not only eliminates matrix interference but also has a good peak resolution within a 6 min-run. A selective and sensitive GC technique with flophemesyl-TMS derivatives also allows accurate quantitative analysis of three active androgens when combined with IDMS. The limit of quantification of the three analytes was <50 pg/mL, and extraction recoveries ranged from 91.9 to 102.1%. The precision and accuracy were 1.2~6.5% and 89.0~106.7%, respectively. This GC-IDMS method can be useful for evaluating the drug efficacy and monitoring the biological processes responsible for male-pattern baldness and prostate diseases.

유류화재의 감식기법의 실험적 특성에 관한 연구 (A Study on Experimental Characteristics in Fire Investigation Techniques of Flammable Liquids)

  • 황태연;최돈묵
    • 한국화재소방학회논문지
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    • 제26권6호
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    • pp.7-14
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    • 2012
  • 본 연구에서는 화재현장에서 유류와 관련되어 실화나 방화의 매개체로 사용되어 화재가 발생했을 때 석유류의 정확한 분석기법을 개발하기 위하여 발화지점 주변의 온도분포, 연소되고 남은 물질의 흔적과 GC/MS 분석으로 물질의 종류를 확인하는 것을 가연성 고체와 비교해서 실험하였다. 연구결과 천장에 도달하는 온도는 휘발유와 시너는 점화되자마자 불꽃이 생성되어 천장의 온도가 매우 빠르게 상승하여 그곳에 물질이 있을 경우 2차 화재발생이 전개될 것으로 나타났다. 연소된 후에 바닥에는 가연성 고체와 유류가 상이한 특징적인 패턴을 형성하였다. 연소된 장판은 탄화수소계열이지만 가스검지관을 통해 반응을 확인한 결과 가연성 고체는 아무런 반응을 띠지 않았으나 유류는 즉시 반응을 하였고 그 연소물질을 7일이 경과된 후에 GC/MS로 분석한 결과 유류의 존재를 확인할 수 있었다. 화재조사가 복잡한 과정이지만 물질의 특성을 통한 세밀한 조사는 유류화재를 입증하는 데 중요하고 GC/MS분석기기를 통해 실체를 확인하는 과정이 요구된다.

GC-MS에 의한 라일락 꽃 향기 분석 (Characterization of Fragrances from Lilac Blossom by Gas Chromatography-Mass Spectrometry)

  • 김남선;이동선
    • 분석과학
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    • 제17권1호
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    • pp.85-89
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    • 2004
  • 라일락 꽃 향기 성분의 특성을 고체상 포집 용매추출법과 기체크로마토그래피 이온 포집형 질량분석법으로 연구하였다. 라일락 품종에 따라 향기성분의 조성이 현저한 차이를 보였다. 백색 라일락 꽃의 경우 벤즈알데히드, 페닐 아세트알데히드 및 알파-파네센인데 비하여 보라색 라일락 꽃은 벤즈알데히드, 알파-피넨 및 오시멘이 주된 향기성분으로 발견되었다. 라일락 꽃 향기성분 중 알파-피넨의 거울상 이성질체의 본질을 분석한 결과 ( )형태임을 알 수 있었다.

Volatile Flavor Compounds of Saussurea lappa C.B. Clarke Root Oil by Hydro Distillation-GC and $GC/MS^+$

  • Chang, Kyung-Mi;Kim, Gun-Hee
    • Food Quality and Culture
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    • 제1권1호
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    • pp.13-17
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    • 2007
  • The volatile flavor compounds of Saussurea lappa C.B. Clarke, a perennial, aromatic and medicinal herbaceous plant of the Asteraceae family, were isolated by the hydro distillation extraction method using a Clevenger-type apparatus, and analyzed by gas chromatography (GC) and gas chromatography-mass spectrometry (GC/MS). The plant yielded a light yellow colored oil (0.02%, v/w). From S. lappa C.B. Clarke root oil, sixty-three volatile flavor compounds were tentatively identified, among which sesquiterpene was predominant (21.70%). The identified compounds of the root oil constituted 87.47% of the total peak area. From the constituents making up more than 5% of the volatile flavor components, a long-chain aldehyde, (7Z, 10Z, 13Z)-7, 10, 13-hexadecatrienal, was the most abundant volatile flavor compound (21.20%), followed by dehydrocostuslactone (10.30%) belonging to sesquiterpene lactone, valerenol (5.30%) and vulgarol B (5.06%).

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