• Title/Summary/Keyword: gas chromatography-mass spectrum

Search Result 47, Processing Time 0.021 seconds

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
    • /
    • v.28 no.2
    • /
    • pp.89-95
    • /
    • 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.

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
    • /
    • v.67 no.9
    • /
    • pp.1232-1238
    • /
    • 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.

Determination of 3-Monochloro-1, 2-propanediol in Acid Hydrolyzed Soysauce(Ganjang) by Gas-Chromatography with Electron Capture Detector (Gas Chromatography-Electron Capture Detector를 이용한 산분해간장중의 3-Monochloro-1, 2-propanediol 분석법에 관한 연구)

  • 최종동;문귀임;오현숙;김동술
    • Journal of Food Hygiene and Safety
    • /
    • v.16 no.1
    • /
    • pp.61-65
    • /
    • 2001
  • To investigate the optimum condition of 3-monochloro-1, 2-propanediol(MCPD) analysis, gas chromatography with electron capture detector was used. Determination of MCPD derivatized with phenylboric acid was more effective than that of underivatized MCPD. In derivatization of MCPD with phenyl boric acid, there were no significantly different between boiling for 2min at 9$0^{\circ}C$ and vortexing for 5min at room temperature. Extrelut column was suitable for extraction of MCPD diluted in 20% NaCl solution and recovery rates were higher than direct extraction of MCPD with ethyl acetate. But, the method of direct extraction of MCPD with ethyl acetate was useful for rapid ants qualitative analysis. The sample extracted in soysauce(ganjang) was derivatized with phenylboric acid and analyzed by gas chromatography-mass selective detector. That was confirmed as MCPD-phenylboronate.

  • PDF

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
    • /
    • v.16 no.3
    • /
    • pp.213-218
    • /
    • 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).

  • PDF

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
    • /
    • v.22 no.2
    • /
    • pp.153-160
    • /
    • 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.

  • PDF

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
    • /
    • v.8 no.1
    • /
    • pp.9-15
    • /
    • 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.

  • PDF

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
    • /
    • v.36 no.3
    • /
    • 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

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
    • /
    • v.11 no.1
    • /
    • pp.177-187
    • /
    • 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.

Screening and identification of bioorganic light-emitting substances from marine macrophytes

  • Jung, Sang Mok;Lee, Han Seong;Lee, Han Joo;Kang, Seul Gi;Son, Ji Su;Jeon, Jae Hyuk;Chae, Hee Baik;Shin, Hyun Woung
    • ALGAE
    • /
    • v.30 no.2
    • /
    • pp.171-179
    • /
    • 2015
  • Organic light-emitting materials in marine macrophytes from various coastal environments were identified. Twentyeight species from the solvent fractions were examined and identified as candidates for bioorganic light-emitting materials using photoluminescence (PL) spectra and gas chromatography-mass spectrometry. We selected 16 solvent fractions from a total of 1,221 prepared from Ishige okamurae, Sargassum confusum, Grateloupia elliptica, Chondracanthus intermedius, Porphyra yezoensis, Meristotheca papulosa, Gelidium amansii, and Scytosiphon lomentaria. The maximum light-emitting PL spectra appeared at various colors, mainly between blue and green, based on chromaticity coordinates, from solvent fractions of M. papulosa, G. amansii, G. elliptica, P. yezoensis, S. lomentaria, I. okamurae, and C. intermedius. These results will contribute to the development of novel organic light-emitting materials.

Inhibition of Klebsiella pneumoniae ATCC 13883 Cells by Hexane Extract of Halimeda discoidea (Decaisne) and the Identification of Its Potential Bioactive Compounds

  • Supardy, Nor Afifah;Ibrahim, Darah;Sulaiman, Shaida Fariza;Zakaria, Nurul Aili
    • Journal of Microbiology and Biotechnology
    • /
    • v.22 no.6
    • /
    • pp.872-881
    • /
    • 2012
  • The inhibitory effect of the Klebsiella pneumoniae ATCC 13883 strain caused by the hexane extract of Halimeda discoidea (Nor Afifah et al., 2010) was further evaluated by means of the microscopy view and its growth curves. The morphological changes of the K. pneumoniae ATCC 13883 cells were observed under the scanning electron microscope (SEM) and transmission electron microscope (TEM) after they were treated at minimum inhibitory concentration (MIC; 0.50 mg/ml) (Nor Afifah et al., 2010) for 12, 24, and 36 h. The results showed the severity of the morphological deteriorations experienced by the treated cells. The killing curve assay was performed for 48 h at three different extract concentrations (1/2 MIC, MIC, and 2 MIC). An increase in the extract concentration of up to 2 MIC value did significantly reduce the number of cells by approximately 1.9 $log_{10}$, as compared with the control. Identification of the potential compounds of the extract responsible for the antibacterial activity was carried out through the gas chromatography-mass spectrum (GC-MS) analysis of the active subfraction, and the compound E-15-heptadecenal was identified and suggested as the most potential antibacterial compound of this extract. The subsequent cellular degenerations showed by the data might well explain the inhibitory mechanisms of the suggested antibacterial compound. All of these inhibitory effects have further proven the presence of an antibacterial compound within H. discoidea that can inhibit the growth of K. pneumoniae ATCC 13883.