• Title/Summary/Keyword: GC/MS(gas chromatography/mass spectrum)

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The Study on the Composition of Rehmanniae Radix Extracts by Supercritical Carbon Dioxide Extraction and by Hydrodistillation Extraction (생지황(生地黃) 증류 추출 약침액과 초임계 유체 추출물의 성분 연구(硏究))

  • Heo, Jong-Won;Yook, Tae-Han
    • Journal of Acupuncture Research
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    • v.28 no.2
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    • pp.89-95
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    • 2011
  • Objectives : The purpose of this study was to investigate the composition of Rehmannia glutinosa's essential oils with Rehmanniae Radix herbal acupuncture Methods : I obtained the essential oils of Rehmannia Radix by hydrodistillation extraction method and supercritical fluid extraction(SFE) method, and then I analyzed those by GC/MS(gas chromatography/mass spectrum). Results : 1. With GC(gas chromatography) and GC/MS(gas chromatography/mass spectrum) analysis. I identified 9 compounds in the Rehmanniae Radix's essential oil obtained through the SFE method. The main compounds were as follows : Hexachloroethane(2.24%), N-Butyl-benzenesulfonamide(2.05%), hexadecanoic acid(1.93%), hexadecanoic acid, ethyl ester(3.49%), 9,12-Octadecadienoic acid(z,z)(2.70%), (9E)-9-Octadecenoic acid(6.14%), ethyl linoleate(4.43%), ethyl oleate(5.80%). 2. I failed to get Rehmanniae Radix's essential oil obtained through the hydrodistillation method. 3. With GC(gas chromatography) and GC/MS(gas chromatography/mass spectrum) analysis. I identified 4 compounds in the Rehmanniae Radix's essential oil obtained through the hydrodistillation method. The main compounds were as follows : Ethylbis(trimethylsilyl)amine(1.04%), 2-(Trimethylsiloxy)benzoic methyl ester(2.65%), Hexadecanoic acid trimethylsilyl ester(12.61%), octadecanoic acid, trimethylsilyl ester(6.28%). Conclusions : The substances by hydrodistillation method may not perfectly match with the substances by supercritical fluid extraction(SFE) method in essential oils extracted form Rehmanniae Radix. But, the main substances was assumed Hexadecanoic acid and octadecanoic acid.

Determination of panthenol, cholecalciferol and tocopherol in cosmetic products by gas chromatography-mass spectrometry in SIM mode

  • Hye-Jin Jeong;Myo
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.22 no.2
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    • pp.153-160
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    • 1996
  • A novel simple method to detect vitamins in cosmetic products by gas chromatography-mass spectrometry(GC-MS) has been developed. Three vitamins(panthenol, cholecalciferol and tocopherol) were used for this study. Vitamins were prepared by dissolving in tetrahydrofuran(THF), and silylated with bis-trimethylsilyltrifluoroacetamide-trichloromethylsilane(BSTFA). Silated vitamins were separated on a fuses-silica capillary column coated with DB-5. The identification of each vitamin was accomplished by retention time and mass spectrum library search with a computer, and the quantitation was made in the selected-ion monitoring(SIM) mode of GC-MS. SIM mode had given sensitivity to determine 50pg of panthenol, 285pg of cholecalciferol and 130pg of tocopherol. Linearity was maintained over the range 0.005-0.20% for each vitamin. Each cosmetic product(i.e. hair tonic and lotion) was found to contain amounts of the vitamins. This method was sensitive and gave 77.5-99.9% recovery of each vitamin from these cosmetic products. From these results, we concluded that silylation with BSTFA followed by GC-MS analysis allows the simple, covenient and exact determination of panthenol, cholecalciferol and tocopherol.

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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.

A Study on the determination of Residual Antibiotics and Synthetic Antibacterial Agents in Meas (II) - Simultaneous Gas Charomatography/Mass Spectrometry Analysis of Penicillin G, Chloramphenicol and Thiamphenicol - (식육중의 잔류 항생.항균제의 검정에 관한 연구 (II) - Penicillin G , Chloramphenicol, Thiamphenicol, Gas chromatography/Mass spectrometry 동시 분석 -)

  • 류재천;양종순;서지원;김명수;박종세
    • Journal of Food Hygiene and Safety
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    • v.8 no.1
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    • pp.9-15
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    • 1993
  • In an attempt to quantitate and qualitate residual antibiotics and antibacterial agents in meat simultaneously, we studied a gas chromatography-mass spectrometry(GC/M8) analysis. For a simultaneous analysis of penicillin G, chloramphenicol and thiamphenicol in meat, a simple and rapid clean-up procedure including extraction with 0.01 M EDTA-2Na Mcilvaine buffer (pH 4.0), defatting with n-hexane, and elution with 0.01M-methanolic oxalic acid from Bond Elute $C_{18}$ cartridge, and quantitation by selected ion monitoring (SIM) mode after derivatization was performed. The recoveries (%) of penicillin G, chloramphenicol and thiamphenicol (CV, %) at 1 ppm fortification level were 63.5 (7.6), 76.3 (8.1) and 84.7 (2.0), and the detection limits of those were 0.6, 0.085 and $0.084\;\mu\textrm{g}$ beef, respectively. This method using 81M mode allows excellent detection and quantitation of residual antibiotics and antibacterial agents in meat. Moreover, confirmation by a full scan electron impact mass spectrum is possible if residual level in the sample in above 1 ppm.

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Analytical Methods of Levoglucosan, a Tracer for Cellulose in Biomass Burning, by Four Different Techniques

  • Bae, Min-Suk;Lee, Ji-Yi;Kim, Yong-Pyo;Oak, Min-Ho;Shin, Ju-Seon;Lee, Kwang-Yul;Lee, Hyun-Hee;Lee, Sun-Young;Kim, Young-Joon
    • Asian Journal of Atmospheric Environment
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    • v.6 no.1
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    • pp.53-66
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    • 2012
  • A comparison of analytical approaches for Levoglucosan ($C_6H_{10}O_5$, commonly formed from the pyrolysis of carbohydrates such as cellulose) and used for a molecular marker in biomass burning is made between the four different analytical systems. 1) Spectrothermography technique as the evaluation of thermograms of carbon using Elemental Carbon & Organic Carbon Analyzer, 2) mass spectrometry technique using Gas Chromatography/mass spectrometer (GC/MS), 3) Aerosol Mass Spectrometer (AMS) for the identification of the particle size distribution and chemical composition, and 4) two dimensional Gas Chromatography with Time of Flight mass spectrometry (GC${\times}$GC-TOFMS) for defining the signature of Levoglucosan in terms of chemical analytical process. First, a Spectrothermography, which is defined as the graphical representation of the carbon, can be measured as a function of temperature during the thermal separation process and spectrothermographic analysis. GC/MS can detect mass fragment ions of Levoglucosan characterized by its base peak at m/z 60, 73 in mass fragment-grams by methylation and m/z 217, 204 by trimethylsilylderivatives (TMS-derivatives). AMS can be used to analyze the base peak at m/z 60.021, 73.029 in mass fragment-grams with a multiple-peak Gaussian curve fit algorithm. In the analysis of TMS derivatives by GC${\times}$GC-TOFMS, it can detect m/z 73 as the base ion for the identification of Levoglucosan. It can also observe m/z 217 and 204 with existence of m/z 333. Although the ratios of m/z 217 and m/z 204 to the base ion (m/z 73) in the mass spectrum of GC${\times}$GC-TOFMS lower than those of GC/MS, Levoglucosan can be separated and characterized from D (-) +Ribose in the mixture of sugar compounds. At last, the environmental significance of Levoglucosan will be discussed with respect to the health effect to offer important opportunities for clinical and potential epidemiological research for reducing incidence of cardiovascular and respiratory diseases.

Analysis of Volatile Flavor Components of Pleurospermum kamtschaticum (누룩치의 휘발성 향미성분 분석)

  • 정미숙;이미순
    • Korean journal of food and cookery science
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    • v.14 no.5
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    • pp.541-546
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    • 1998
  • Volatile flavor components in leaf and petiole of fresh Pleurospermum kamtschaticum H$\_$OFFM/ were extracted by SDE (simultaneous steam distillation and extraction) method using diethyl ether as solvent. Essential oils were analyzed by gas chromatography (GC) and combined gas chromatography-mass spectrometry (GC-MS). Identification of volatile flavor components was based on the Rl of GC and mass spectrum of GC-MS. A total of 31 components, including 15 hydrocarbons, 4 aldehydes, 1 ketone, 5 alcohols, 2 esters, 3 acids and 1 oxide were identified in the essential oils. (Z)-${\beta}$-Farnesene, (Z, E)-${\alpha}$-farnesene and farnesene were the major volatile flavor components in fresh Pleurospermum kamtschaticum. Volatile flavor patterns of Pleurospermum kamtschaticum were analyzed using electronic nose. Sensor T30/1 and PA2 that were sensitive to alcohols had the highest resistance for fresh Pleurospermum kamtschaticum. Resistance of six metal oxide sensors was decreased in dried sample compared with fresh one.

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The Study on the Composition of Yongdamsagan-tang(龍膽瀉肝湯)'s Essential Oil Obtained by Supercritical Carbon Dioxide Extraction (초임계 유체 추출법을 이용한 용담사간탕(龍膽瀉肝湯) 약침액(藥鍼液)의 정유(精油)성분에 대한 연구(硏究))

  • Lee, Jae-Eun;Kim, Byeong-U;Im, Tae-Jin;Kim, Dong-Hui;Shin, Min-Seop;Yook, Tae-Han;Gwon, Gi-Rok
    • Journal of Pharmacopuncture
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    • v.11 no.1
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    • pp.177-187
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    • 2008
  • Objectives : This study was performed to analyze the effective components of essential oil obtained from Yongdamsagantang, which has been efficacious against leukorrhea in gynecologic diseases. Methods : I obtained the essential oils of Yongdamsagan-tang by hydrodistillation extraction method and supercritical fluid extraction(SFE) method, and then I analyzed those by GC/MS(Gas Chromatography/Mass Spectrum). Results : 1. The optimum SFE(Supercritical Fluid Extraction) condition was obtained in the following experiment conditions: pressure 200atm, temperature $45^{\circ}C$, duration of extraction 25minutes. 2. With GC(Gas Chromatography) and GC/MS(Gas Chromato- graphy/Mass Spectrum) analysis, I identified 37 compounds in the Yongdamsagan-tang's essential oil obtained through the SFE method. The main compounds were as follows : 3-Methyl-but-2-enoic acid,2,2-dimethyl-8-oxo-3,4-dihydro-2H,8H -pyrano[3,2-g]chromen-3-yl ester(49.81%), (Z)-6-Pentadecen-1 -ol(3.19%), (-)-Spathulenol(2.40%). 3. I identified 4 compounds in the Yongdamsagan-tang's essential oil obtained through the hydrodistillation method. The main compounds were as follows : 3-Methyl-but-2-enoic acid, 2,2-dimethyl-8-oxo-3,4-dihydro-2H,8H-pyrano [3,2-g]chromen-3-yl ester(2.61%). 4. 3-Methy I-but-2-enoic acid, 2,2-dimethyl-8-oxo-3,4-dihydro-2H,8H-pyrano[3,2-g] chromen-3-yl ester, all were identified in both the SFE method and the hydrodistillation method, but the others were not identified in common. 5. I also conducted an additional test in order to examine the essential oil's antimicrobial action against bacteria. Both MIC(Minimum Inhibitory Concentrations) and MBC(Minimum Bactericidal Concentrations) were $0.125mg/m{\ell}$ against N. meningitidis, however MIC and MBC were $1.0mg/m{\ell}$ in antimicrobial action against 12 different genera of bacteria.

Analysis of the composition of trail pheromone secreted from live Camponotus japonicus by HS-SPME GC/MS (HeadSpace-Solid Phase MicroExtraction Gas Chromatography/Mass Spectrometry) (HS-SPME GC/MS법을 이용한 일본왕개미의 trail pheromone 성분 분석)

  • Park, Kyung-Eun;Lee, Dong-Kyu;Kwon, Sung Won;Lee, Mi-Young
    • Analytical Science and Technology
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    • v.25 no.5
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    • pp.292-299
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    • 2012
  • GC/MS has been utilized for many applications due to great resolution and reproducibility, which made it possible to build up the database of mass spectrum, while HS-SPME has the advantage of solventfree extraction of volatile compounds. The combination of these two methods, HS-SPME GC/MS, enabled many scientific applications with various possibilities. In this study, the analysis of trail pheromone excreted from live Camponotus japonicus with the feature of solvent-free extraction was carried out and the optimization for this analysis was performed. The major compounds detected were n-decane, n-undecane, and n-tridecane. Optimization for the best detection of these hydrocarbons was processed in the point of SPME parameter (selection of fiber, extraction temperature, extraction time, etc.). The advantage of the analysis of live sample is to analyze phenomenon right after it is excreted by ants. But the experimental process has restriction of extraction temperature and time because of the analysis of live ants. Establishing the process of HS-SPME GC/MS applied to live samples shown in this study can be a breakthrough for the ecofriendly and ethical research of live things.

Identification of Higenamine nad its Metabolites in Rat by Gas Chromatography/Mass Spectrometry

  • Ryu, Jae-chun;Song, Yun-Seon;Kim, Myung-Soo;Cho, Jung-Hyuck;Yunchoi, Hye-Sook
    • Archives of Pharmacal Research
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    • v.16 no.3
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    • pp.213-218
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    • 1993
  • ($\pm$)-Higenamine is known as a cardiotonic principle of aconite root (root of Aconitum spp., Ranunculaceae). A simple and sensitive detection method for higenamine was developed by using gas chromatography-mass spectrometry (GC/MS). The recovery of higenamine after extraction and concentration with XAD-2 resin column was around 95% from rat biological fluids such as bile, plasma and urine. The limits of detection of higenamine in these biological fluids were approximately 0.1 ng/ml each. It has well been suggested that tetrahydroisoquinolines possessing catechol moiety such as higenamine should be subjected to the catechol-O-methyl transferase (COMT) activity in vivo. We detected two major peaks of presumed metabolites of higenamine in the total ion chromatogram obtained from the rat urine sample after the oral adminstration of ($\pm$)-higenamine. The scan mass spectrum of one of the metabolties coincided with those obtained from coclaurine $(C_6$-O-methyl higenamine) and those of the other metabolite are suggestive of isococlaurine $(C_7$-O-methyl higenamine).

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Determination of Captan, Folpet, Captafol and Chlorothalonil Residues in Agricultural Commodities using GC-ECD/MS (GC-ECD/MS를 이용한 농산물 중 Captan, Folpet, Captafol 및 Chlorothalonil의 잔류분석법)

  • Lee, Su-Jin;Hwang, Young-Sun;Kim, Young-Hak;Kwon, Chan-Hyeok;Do, Jung-A;Im, Moo-Hyeog;Lee, Young-Deuk;Choung, Myoung-Gun
    • Korean Journal of Environmental Agriculture
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    • v.29 no.2
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    • pp.165-175
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    • 2010
  • A gas chromatographic (GC) method was developed to determine residues of captan, folpet, captafol, and chlorothalonil, known as broad-spectrum protective fungicides for the official purpose. All the fungicide residues were extracted with acetone containing 3% phosphoric acid from representative samples of five agricultural products which comprised rice, soybean, apple, pepper, and cabbage. The extract was diluted with saline, and dichloromethane partition was followed to recover the fungicides from the aqueous phase. Florisil column chromatography was additionally employed for final cleanup of the extracts. The analytes were then determined by gas chromatography using a DB-1 capillary column with electron capture detection. Reproducibility in quantitation was largely enhanced by minimization of adsorption or thermal degradation of analytes during GLC analysis. Mean recoveries generated from each crop sample fortified at two levels in triplicate ranged from 89.0~113.7%. Relative standard deviations (RSD) were all less than 10%, irrespective sample types and fortification levels. As no interference was found in any samples, limit of quantitation (LOQ) was estimated to be 0.008 mg/kg for the analytes except showing higher sensitivity of 0.002 mg/kg for chlorothalonil. GC/Mass spectrometric method using selected-ion monitoring technique was also provided to confirm the suspected residues. The proposed method was reproducible and sensitive enough to determine the residues of captan, folpet, captafol, and chlorothalonil in agricultural commodities for routine analysis.