• Title/Summary/Keyword: Gas chromatography-mass spectrometer

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Structural Determination of Cerebrosides from Soybean Embryo by Mass Spectrometer (Mass Spectrometer를 이용한 대두 배아 출추 Cerebroside의 구조 분석)

  • Kim, Jung-Hun;Chang, Sug-Youn;Kim, Yeo-Kyung
    • Analytical Science and Technology
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    • v.6 no.3
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    • pp.335-343
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    • 1993
  • The structure of cerebrosides from soybean embryo was determined using fast atom bombardment mass spectrometer (FAB-MS), gas chromatography mass spectrometer (GC-MS) and TLC. The components of cerebroside were determined by GC-MS after acid hydrolysis. The molecular weight distribution of cerebroside was measured by positive mode FAB-MS with LiOH saturated 3-nitrobenzylalcohol(3-NBA) matrix. Structures of individual components of complex mixtures can be determined easily by this process. The major constituent of soybean extracted cerebroside was determined as the glucoside of N-2'-hydroxypalmitoyl-sphingadienine.

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Gas Chromatography-High Resolution Tandem Mass Spectrometry Using a GC-APPI-LIT Orbitrap for Complex Volatile Compounds Analysis

  • Lee, Young-Jin;Smith, Erica A.;Jun, Ji-Hyun
    • Mass Spectrometry Letters
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    • v.3 no.2
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    • pp.29-38
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    • 2012
  • A new approach of volatile compounds analysis is proposed using a linear ion trap Orbitrap mass spectrometer coupled with gas chromatography through an atmospheric pressure photoionization interface. In the proposed GC-HRMS/MS approach, direct chemical composition analysis is made for the precursor ions in high resolution MS spectra and the structural identifications were made through the database search of high quality MS/MS spectra. Successful analysis of a complex perfume sample was demonstrated and compared with GC-EI-Q and GC-EI-TOF. The current approach is complementary to conventional GC-EI-MS analysis and can identify low abundance co-eluting compounds. Toluene co-sprayed as a dopant through API probe significantly enhanced ionization of certain compounds and reduced oxidation during the ionization.

Supercritical Fluid Extraction of Physiologically Active materials from Agaricus blazei Fruiting Bodies (Agaricus blazei 자실체로부터 초임계 유체를 이용한 생리활성물질 추출공정)

  • 최정우
    • KSBB Journal
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    • v.15 no.4
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    • pp.408-410
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    • 2000
  • The supercritical fluid extraction(SFE) technique was applied for the isolation and purification of nonpolar physiologically acitve mateials from Agaricus blazei fruiting bodies. the qualitative analysis of extract was accomplished by gas chromatography-mass spectrometer(GC-MS) and extract was determined as linoleic acid(cis-9 cis-12-octadecadienoic acid) In order to obtain the optimum operating conditions of supercritical fluid extraction process the various temperatures and pressures were applied for process operation. From the comparison of exraction efficiencies $50^{\circ}C and 200 kg_f/cm^2$ were determined as optimum conditions.

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Algorithm to Improve Mass Spectral Resolution of Gas Chromatography Mass Spectrometer (가스크로마토그래피 질량분석기의 질량 스펙트럼 해상도 개선 알고리즘)

  • Choi, Hun
    • The Transactions of The Korean Institute of Electrical Engineers
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    • v.67 no.9
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    • pp.1232-1238
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    • 2018
  • This paper proposes methods for improving mass spectral resolution for a gas chromatograph mass spectrometer. The slope signs of the 1st and 2nd fitting functions for the ion signal block of each mass index are obtained, and the unnecessary element signals in the ion signal block are removed. The spectrum can be obtained by obtaining the second-order fitting function of the reconstructed ion signal block using only the effective ion signals. In addition, the resolution of the mass spectrum can be improved by correcting the error caused by the shift of the spectral peak position. To verify the performance of the proposed methods, computer simulations were performed using the actual ion signals obtained from the GC-MS system under development. Simulation results show that the proposed method is valid.

Isolation of 3,4-Dihydroxybenzoic Acid, Which Exhibits Antimicrobial Activity, from Fruits of Gardenia jasminoides Ellis (치자 열매에서 항미생물 활성을 갖는 3,4-Dihydroxybenzoic Acid의 분리)

  • Yim, Cheol-Keun;Moon, Jae-Hak;Park, Keun-Hyung
    • Korean Journal of Food Science and Technology
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    • v.31 no.5
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    • pp.1386-1391
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    • 1999
  • The methanol extract of Gardenia jasminoides Ellis showed antimicrobial activity against bacteria and yeasts. The extract was successively purified with solvent fractionation, silica gel adsorption column chromatography, Sephadex LH-20 column chromatography, octadecylsilane column chromatography. The purified active substance was isolated by high performance liquid chromatography. The isolated compound was 3,4-dihydroxybenzoic acid which was determined by mass spectrometer, gas chromatograph-mass spectrometer, $^{1}H-nuclear$ magnetic resonance, $^{13}C-nuclear$ magnetic resonance and two-dimensional nuclear magnetic resonance. The content of 3,4-dihydroxybenzoic acid was $32.7\;{\mu}g/g$ in dried fruits of Gardenia jasminoides Ellis.

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Discrimination Model of Cultivation Area of Alismatis Rhizoma using a GC-MS-Based Metabolomics Approach (GC-MS 기반 대사체학 기법을 이용한 택사의 산지판별모델)

  • Leem, Jae-Yoon
    • YAKHAK HOEJI
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    • v.60 no.1
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    • pp.29-35
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    • 2016
  • Traditional Korean medicines may be managed more scientifically, through the development of logical criterion to verify their cultivation region. It contributes to advance the industry of traditional herbal medicines. Volatile compounds were obtained from 14 samples of domestic Taeksa and 30 samples of Chinese Taeksa by steam distillation. The metabolites were identified by NIST mass spectral library in the obtained gas chromatography/mass spectrometer (GC/MS) data of 35 training samples. The multivariate statistical analysis, such as Principal Component Analysis (PCA), Partial Least Squares Discriminant Analysis (PLS-DA), and Orthogonal Partial Least Squares Discriminant Analysis (OPLS-DA), were performed based on the qualitative and quantitative data. Finally trans-(2,3-diphenylcyclopropyl)methyl phenyl sulfoxide (47.265 min), 1,2,3,4-tetrahydro-1-phenyl-naphthalene (47.781 min), spiro[4-oxatricyclo[5.3.0.0.(2,6)]decan-3-one-5,2'-cyclohexane] (54.62 min), 6-[7-nitrobenzofurazan-4-yl]amino-morphinan-4,5-epoxy (54.86 min), p-hydroxynorephedrine (55.14 min) were determined as marker metabolites to verify candidates for the origin of Taeksa. The statistical model was well established to determine the origin of Taeksa. The cultivation areas of test samples, each 3 domestic and 6 Chinese Taeksa were predicted by the established OPLS-DA model and it was confirmed that all 9 samples were precisely classified.

NEAR INFRARED TRANSFLECTANCE SPECTROSCOPY (NIRS) IN PHYTOCHEMISTRY

  • Huck, C.W.;W.Guggenbichler;Bonn, G.K.
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.3114-3114
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    • 2001
  • During the last years phytochemistry and phytopharmaceutical applications have developed rapidly and so there exists a high demand for faster and more efficient analysis techniques. Therefore we have established a near infrared transflectance spectroscopy (NIRS) method that allows a qualitative and quantitative determination of new polyphenolic pharmacological active leading compounds within a few seconds. As the NIR spectrometer has to be calibrated the compound of interest has at first to be characterized by using one or other a combination of chromatographic or electrophoretic separation techniques such as thin layer chromatography (TLC), high performance liquid chromatography (HPLC), capillary electrophoresis (CE), gas chromatography (GC) and capillary electrochromatography (CEC). Both structural elucidation and quantitative analysis of the phenolic compound is possible by direct coupling of the mentioned separation methods with a mass spectrometer (GC-MS, LC-MS/MS, CE-MS, CEC-MS) and a NMR spectrometer (LC-NMR). Furthermore the compound has to be isolated (NPLC, MPLC, prep. TLC, prep. HPLC) and its structure elucidated by spectroscopic techniques (UV, IR, HR-MS, NMR) and chemical synthesis. After that HPLC can be used to provide the reference data for the calibration step of the near infrared spectrometer. The NIRS calibration step is time consuming, which is compensated by short analysis times. After validation of the established NIRS method it is possible to determine the polyphenolic compound within seconds which allows to raise the efficiency in quality control and to reduce costs especially in the phytopharmaceutical industry.

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

  • Shin Ho-Sang;Ahn Hye-Sil
    • Journal of Environmental Health Sciences
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    • v.32 no.1 s.88
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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.

Thermal Decomposition of Ammonium Salts of Transition Metal Oxyacids. V. Study on the Thermal Decomposition of Ammonium Metavanadate (전위금속의 산소산염의 열분해에 관한 연구 (제5보) Ammonium Metavanadate의 열분해에 따르는 $V_2O_5$의 생성)

  • Il-Hyun Park
    • Journal of the Korean Chemical Society
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    • v.16 no.3
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    • pp.157-165
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    • 1972
  • Thermal decomposition of ammonium metavanadate has been investigated by using the quartz spring balance and differential thermal analysis. It showed that the decomposition of ammonium metavanadate is proceeded at two stages which correspond to $180^{\circ}C-220^{\circ}C$ and $310^{\circ}C-330^{\circ}C$ decomposition temperatures, respectively. Evolved ammonia gas in thermal decomposition has been analyzed quantitatively by titration. And the constituents of gases evolved have been evaluated by gas chromatography and omegatron spectrometer. From these results, it was concluded that the gases evolved in the first step decomposition were $NH_3$ and $H_2O$ with 2:1 ratio and the second step decomposition corresponded to the formation of $NH_3$, $H_2O$ and $N_2O$ which was produced in oxidation of $NH_3$ by $V_2O_5$. The decomposition products were identified by means of X-ray diffraction method. The decomposition product in air was V_2O_5 and the product in vacuum $V_3O_7.$ The kinetics of the thermal decomposition was studied, giving the values of the activation energy of 41.4 kcal/mole and 64.4 (kcal/mole) respectively.

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Quantitative Analysis of the Seven Marker Components in Asarum sieboldii using the LC-MS/MS and GC-MS (LC-MS/MS와 GC-MS를 이용한 세신 추출물 중 7종 성분의 함량분석)

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Korean Journal of Pharmacognosy
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    • v.44 no.4
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    • pp.350-361
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    • 2013
  • Asarum sieboldii has been used for treatment of fever, pain, common cold, and chronic sinusitis in Korea. In this study, we performed quantification analysis of seven major constituents including aristolochic acid I, aristolochic acid II, ${\alpha}$-asarone, ${\beta}$-asarone, elemicin, methyl eugenol, and safrole in the 70% ethanol extract of Asarum sieboldii and its solvent fractions, n-hexane, ethylacetate, n-butanol, and water ones using a ultra-performance liquid chromatography-electrospray ionization-mass spectrometer(UPLC-ESI-MS) and gas chromatography-mass spectrometer(GC-MS). Regression equations of seven components were acquired with $r^2$ values >0.99. The values of limit of detection(LOD) and quantification(LOQ) were 0.1-3.9 ng/mL and 0.3-11.7 mg/mL, respectively. The amount of the seven compounds in Asarum sieboldii were not detected -143.66 mg/g. The established LC-MS/MS and GC-MS methods will be helpful to improve quality control of Asarum sieboldii.