• Journal of Acupuncture Research
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• 제28권2호
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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.

• 대한화장품학회지
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• 제22권2호
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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.

• 전기학회논문지
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• 제67권9호
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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.

• 한국식품위생안전성학회지
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• 제8권1호
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• pp.9-15
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• 1993

어패류를 포함한 식용 육류중에 잔류하는 항생물질 및 항균성물질을 검출하기 위하여, 분석기기로서 Gas chromatography/ Mass spectrometry(GC/MS)를 사용한 동시분석법을 개발하였다. 여러 항생.항균제중에서 penicillin G, chloramphenicol, thiamphenicol을 중심으로 간단한 전처리과정과 유도체화를 하여 GC/MS 분석을 시행하였다. 전처리 과정을 요약하면 pH 4.0의 0.01 M EDTA-2Na McIlvaine buffer로의 추출, n-hexane으로의 탈지, Bond-Elute $C_{18}$ cartridge에 흡착된 물질의 0.01 M-methnolic oxalic acid로의 용출 그리고 건조 후 유도체화의 순으로 되어 있다. 본 방법에 의한 1 ppm spike시의 회수율은 penicillin G, chloramphenicol, thiamphenicol 각각 63.5%, 76.3%, 84.7%이었고, 검출한계는 각각 시료 g당 0.6, 0.085, $0.084\;\mu\textrm{g}$이었다. 또한 GC/MS 확인과정에서 실제 잔류농도가 1 ppm 이상이면 full scan spectrum으로 확인이 가능하였다. 이와 같은 GC/MS에 의한 잔류물질의 정량 및 확인시험은 앞의 미생물학적 방법의 복원은 물론 식품의 안전성 재고 및 규제독성의 측면에서도 매우 뜻 있는 연구라 하겠다.

• Asian Journal of Atmospheric Environment
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• 제6권1호
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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.

• 한국식품조리과학회지
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• 제14권5호
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• pp.541-546
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• 1998

자생 누룩치의 휘발성 향미성분을 연속수증기증류 장치로 추출한 후 GC, GC/MS로 분석하여 31개의 휘발성 향미성분이 확인되었는데, 탄화수소류가 15종으로 전체 peak area의 64.98%를 차지하였고 알데히드류 4종 9.54%, 케톤류 1종 0.16%, 알코올류 5종 7.65%, 에스테르류 2종 2.06%, 산류 3종 2.0% 및 옥사이드류 1종 2.75%로 이루어져 있었다. 탄화수소류 중 mono-terpenes은 peak area 0.54% 및 sesquiterpenes은 52.11% 를 차치하였다. 누룩치의 주요 휘발성 향미성분은 sesquiterpenes인 (Z)-$\beta$-farnesene, (Z, E)-$\alpha$-farnesene 및 farnesene으로 사료된다. Headspace법에 의하여 신선한 누룩치의 휘발성 향미성분을 포집하여 전자코로 분석한 결과, 알코올류와 같은 극성화합물이 가장 많이 감지되었고 알데히드류, 탄화수소류 순서로 감지되었다. 또한 건조된 누룩치는 신선한 시료와 유사한 향미성분 패턴을 보였으나, 각 sensor의 저항치가 현저히 낮아 건조된 시료의 휘발성 향미성분이 비교적 적음을 확인하였다.

• 대한약침학회지
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• 제11권1호
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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.

• 분석과학
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• 제25권5호
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• pp.292-299
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• 2012

GC/MS (gas chromatography/mass spectrometry)는 훌륭한 분리능과 재현성으로 인해 널리 활용되고 있으며, 정립된 데이터베이스의 활용을 통한 성분 분석에서 활용도가 높다. 또한 HS-SPME (headspacesolid phase micro extraction)법은 용매로 추출을 하지 않은 휘발성 물질의 추출을 하는데 널리 사용되었다. 이 두 방법의 연계는 다양한 시료에서 발생하는 휘발성 성분의 분석에 널리 활용되었다. 위 특징을 이용하여 살아있는 Camponotus japonicus가 분비하는 미량의 페로몬 구성 성분의 분석 방법을 확립하였다. n-Decane, n-undecane, n-tridecane 등의 물질이 미량 페로몬에서 검출되었으며, 이 탄화수소들을 분석하는데 적합한 SPME fiber, 추출 온도, 추출 시간을 최적화하였다. 살아있는 시료를 분석할 수 있기 때문에 특정 현상이 발생하는 그 순간을 분석하는 장점이 있는 한편, 살아있는 시료를 분석하기 때문에 추출 시간 등이 제한된다는 한계점이 있었으나 살아있는 HS-SPME GC/MS 분석방법이 정립된다면 살아있는 시료를 죽일 필요 없다는 점에서 친환경적인 연구의 발전에 해결책이 될 수 있을 것으로 전망한다.

• Archives of Pharmacal Research
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• 제16권3호
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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).

• 한국환경농학회지
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• 제29권2호
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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.