• Title/Summary/Keyword: GC/MS spectrometry

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Gas Chromatography/Mass Spectrometry를 이용한 뇨중 Amineptine과 그 대사체 분석방법에 관한 연구 (Analysis of Amineptine and its Metabolites in Human Urine by Gas Chromatography/Mass Spectrometry)

  • 이정애;김영림;노동석
    • 분석과학
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    • 제13권3호
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    • pp.385-393
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    • 2000
  • 뇨시료 중 amineptine의 (dihydro-10, 11-dibenzo[a, d] cycloheptenyl-5-amino-7-heptanoic acid) metabolites를 분석하기 위한 최적조건을 찾기 위하여 pH 변화에 따른 추출률과 세가지의 유도체화시약에 대한 반응성을 조사해본 결과 pH는 9.5, 유도체화시약은 carboxylic acid group에 MSTFA로 반응 시켰을 경우 좋은 결과를 나타내었다. GC/MS를 이용하여 amineptine을 복용한 사람의 뇨를 분석한 결과 amineptine과 그 대사물질인 dihydro-10, 11-dibenzo[a, d] cycloheptenyl-5-amino-5-pentanoic acid ($C_5$-metabolite)와 $C_5$-metabolite의 lactamized product인 ${\delta}$-lactam을 확인하였다. Amineptine과 그 metabolite들을 GC/MS-SIM mode로 분석하기 위한 monitoring ion들은 m/z 192를 공통 이온으로 선정하였으며, 각각의 분자이온을 선정하였다. Amineptine의 excretion study 결과, amineptine, ${\delta}$-lactam 및 $C_5$-metabolite는 4시간이내에 70-90%가 배설되었고 20시간 이내에 거의 배설이 완결되었다.

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Discrimination of American ginseng and Asian ginseng using electronic nose and gas chromatography-mass spectrometry coupled with chemometrics

  • Cui, Shaoqing;Wu, Jianfeng;Wang, Jun;Wang, Xinlei
    • Journal of Ginseng Research
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    • 제41권1호
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    • pp.85-95
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    • 2017
  • Background: American ginseng (Panax quinquefolius L.) and Asian ginseng (Panax ginseng Meyer) products, such as slices, have a similar appearance, but they have significantly different prices, leading to widespread adulteration in the commercial market. Their aroma characteristics are attracting increasing attention and are supposed to be effective and nondestructive markers to determine adulteration. Methods: The aroma characteristics of American and Asian ginseng were investigated using gas chromatography-mass spectrometry(GC-MS) and an electronic nose (E-nose). Their volatile organic compounds were separated, classified, compared, and analyzed with different pattern recognition. Results: The E-nose showed a good performance in grouping with a principle component analysis explaining 94.45% of variance. A total of 69 aroma components were identified by GC-MS, with 35.6% common components and 64.6% special ingredients between the two ginsengs. It was observed that the components and the number of terpenes and alcohols were markedly different, indicating possible reasons for their difference. The results of pattern recognition confirmed that the E-nose processing result is similar to that of GC-MS. The interrelation between aroma constituents and sensors indicated that special sensors were highly related to some terpenes and alcohols. Accordingly, the contents of selected constituents were accurately predicted by corresponding sensors with most $R^2$ reaching 90%. Conclusion: Combined with advanced chemometrics, the E-nose is capable of discriminating between American and Asian ginseng in both qualitative and quantitative angles, presenting an accurate, rapid, and nondestructive reference approach.

GC-MS를 이용한 사람 뇨시료 중 비만치료제 분석 및 비만치료제 남용 현황의 법과학적 고찰 (Development of a Simultaneous Detection and Quantification Method of Anorectics in Human Urine Using GC-MS and its Application to Legal Cases)

  • 최혜영;이재신;장문희;양원경;김은미;최화경
    • 약학회지
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    • 제57권6호
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    • pp.420-425
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    • 2013
  • Phentermine (PT) and phenmetrazine (PM) have been widely used as anti-obesity drugs. These drugs should be used with caution due to its close relation to amphetamine in its structure and toxicity. PT and PM, amphetamine-type anorectics, have recently been considered as alternatives for methamphetamine abuse in Korea. In addition, the misuse and abuse of PT and PM obtained by illegal sources such as the internet become a serious social problem. In the present study, a simultaneous detection and quantification method for determining PT and PM in human urine was developed and validated according to the international guidelines. The urine samples were screened using a fluorescence polarization immunooassay and analyzed by gas chromatography mass spectrometry (GC-MS) after extraction using automatic solid phase extraction (SPE) with a mixed-mode cation exchange cartridge and derivatization with pentafluoropropionic anhydride (PFPA). The validation results for selectivity, linearity, limits of detection (LOD) and quantification (LOQ), intra- and inter-assay precision and accuracy and recovery were satisfactory. The validated method was successfully applied to authentic urine samples collected from 38 drug abuse suspects. PT and/or PM were identified with or without methamphetamine in urine samples. Abuse of PT and PM have increased continuously in Korea, therefore, closer supervision of the inappropriate use of anoretics is necessary.

기체크로마토그래피/질량분석법을 이용한 캔 물질에서의 bisphenol-A 분석 (Determination of bisphenol-A using GC/MS in Can Materials)

  • 김기철;김양희;최옥경;고환욱;임준래;조규홍;조현우;김혜영;김명수;명승운
    • 분석과학
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    • 제14권6호
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    • pp.499-503
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    • 2001
  • 비스페놀-A는 epoxy resin, polycarbonate, polyester-styrene resin 등의 플라스틱 제조에 사용되는 물질로써, 기체 크로마토그래피를 이용하여 간단하며 빠르고 감도 좋은 분석방법을 연구하였다. 비스페놀-A를 acylating 시약을 사용하여 크로마토그래피의 성질에 적합하도록 유도체화 한 후 SIM(selected ion monitoring) mode를 이용하여 GC/MS(gas chromatography/mass spectrometry)로 분석하였으며, 본 연구 결과 캔 물질에서 비스페놀 A는 $0.11{\sim}11.40{\mu}g/can$이 검출되었다.

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GC-MS를 이용한 신선편의 샐러드 중 dichloroacetic acid와 trichloroacetic acid의 분석 (Determination of dichloroacetic acid and trichloroacetic acid in fresh-cut salads using gas chromatography-mass spectrometry)

  • 김희갑;이성균;윤아현
    • 한국식품과학회지
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    • 제51권1호
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    • pp.12-17
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    • 2019
  • 이 연구에서는 GC-MS를 사용하여 신선편의 채소류 중 DCAA 및 TCAA를 포함한 haloacetic acids를 분석하는 방법을 확립하였다. 분석 방법의 유효성을 검증한 후 일부 시중에서 유통 중인 시료를 분석한 결과, 외국의 수준보다 높아 $19-75{\mu}g/kg$의 수준으로 검출되었다. 본 결과를 바탕으로 실시한 위해 평가에 따르면, 현재 국내에 유통 중인 신선편의 채소류의 섭취에 따른 초과 발암 위해도가 허용 수준을 초과하여, 향후 이에 대한 관리가 필요하다는 것을 시사하였다.

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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    • 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.

전자코 시스템을 이용한 우유의 품질에 따른 휘발성 향기성분 분석 (Analysis of Volatile Flavor Compounds in Milk Using Electronic Nose System)

  • 강내경;전태선;양윤석;김용신
    • 센서학회지
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    • 제23권5호
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    • pp.320-325
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    • 2014
  • Volatile flavor compounds from milk were analyzed and identified by using the analysis methods of headspace solid phase microextraction gas chromatography/mass spectrometry (HSPME-GC/MS) and electronic nose (E-Nose) system. About 30 volatile compounds were identified by HSPME-GC/MS for the fresh and off-flavor milk samples. Also, the correlation between rancidity and ageing days of milk was obtained by the aid of principal component analysis algorithm. It shows that the E-Nose system can identify the various types of milk flavor. These results imply that the analysis method based on the E-nose system can apply to the quality control of milk flavor and the rancidity.

택란(澤蘭)의 정유성분(精油成分)에 관한 연구(硏究) (Studies on Essential Oils of Lycopus lucidus Turcz)

  • 신순희;심연;김유선;지형준;이은방
    • 생약학회지
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    • 제23권1호
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    • pp.29-33
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    • 1992
  • The essential oils of Lycopus lucidus have been studied. The essential oil obtained from the dried herba by steam distillation followed by fractionation by column chromatography was analysed by gas chromatography-mass spectrometry(GC-MS). The compounds identified by GC-MS were carvacrol, 2,5-dimethoxy-p-cymene, trans-caryophyllene, spathurenol and $trans-{\beta}-farnesene$. Two compounds, thymol and caryophyllene were isolated by silica gel column chromatography and analyzed by TLC, IR, Mass and NMR. And the weak diuretic effects of essential oil and water extract from the dried drugs were observed in rats.

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Catalytic Pyrolysis of Waste Polyethylene Terephthalate over Waste Concrete

  • Lim, Sejeong;Kim, Young-Min
    • 공업화학
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    • 제30권6호
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    • pp.707-711
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    • 2019
  • The feasibility of waste concrete as a catalyst for the effective pyrolysis of polyethylene terephthalate (PET) was examined using thermogravimetric (TG) and pyrolyzer-gas chromatography/mass spectrometry (Py-GC/MS) analyses. TG analysis results indicated that the maximum decomposition temperature of PET is not altered by the use of waste concrete, showing similar values (407 ℃ and 408 ℃ at 5 ℃/min). Meanwhile, the volatile product distribution data obtained from the Py-GC/MS analysis revealed that the use of waste concrete promoted the deoxygenation reaction via converting the oxygen containing products such as benzoic acids, benzoates, and terephthalates to valuable deoxygenated aromatic hydrocarbons including benzene, toluene, ethylbenzene, and styrene. This suggests that the waste concrete can be used as a potential catalyst for the production of valuable aromatic hydrocarbons from PET pyrolysis.

Analysis of Poly(Ethylene-co-Vinyl Acetate) Using Off-line Pyrolysis

  • Choi, Sung-Seen;Kim, Eunha
    • Elastomers and Composites
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    • 제51권1호
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    • pp.63-67
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    • 2016
  • Poly(ethylene-co-vinyl acetate) (EVA) was pyrolyzed to eliminate acetic acid of VA unit using off-line pyrolysis, and the deacetylated EVA was analyzed infrared spectroscopy (IR) and pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS). EVA film for deacetylation was prepared by solution casting on aluminum foil and it was pyrolyzed at low temperature of $300^{\circ}C$ in the off-line pyrolysis apparatus. After deacetylation, carbon-carbon double bond (C=C) was formed by 1,2-elimination of the VA unit in the EVA backbone. Most of C=C bonds were trans-1,4-unit and 1,2-unit was also observed. Presence of the 1,2-unit in deacetylated EVA indicates that terminal or branch VA units exist in the raw EVA. Py-GC/MS chromatogram of deacetylated EVA displayed much smaller acetic acid and much more abundant other pyrolysis products than that of raw EVA, which means that the pyrolysis efficiency and separation condition were improved.