• Title/Summary/Keyword: GC-MASS

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Simultaneous determination of 11-nor-Δ9-carboxy-tetrahydrocannabinol and 11-nor-Δ9-carboxy-tetrahydrocannabinol-glucuronide in urine samples by LC-MS/MS and its application to forensic science (LC-MS/MS를 이용한 소변 중 11-nor-Δ9-carboxy-tetrahydrocannabinol 및 11-nor-Δ9-carboxy-tetrahydrocannabinol-glucuronide의 동시 분석 및 법과학적 적용)

  • Park, Meejung;Kim, Sineun
    • Analytical Science and Technology
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    • v.34 no.6
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    • pp.259-266
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    • 2021
  • Cannabis (Marijuana) is one of the most widely used drugs in the world, and its distribution has been controlled in South Korea since 1976. Identification of 11-nor-Δ9-carboxy-tetrahydrocannabinol (THCCOOH) in urine can provide important proof of cannabis use, and it is considered scientific evidence in the forensic field. In this study, we describe a simultaneous quantitative method for identifying THCCOOH and THCCOOH-glucuronide in urine, using simple liquid-liquid extraction (LLE), and liquid chromatography-tandem mass spectrometry (LC-MS/MS). THCCOOH-D3 and THCCOOH-glucuronide-D3 were used as internal standards. Validation results of the matrix effect, as well as recovery, linearity, precision, accuracy, process efficiency, and stability were all satisfactory. No carryover, endogenous or exogenous interferences were observed. The limit of detection (LOD) of THCCOOH and THCCOOH-glucuronide were 0.3 and 0.2 ng/mL, respectively. The developed method was applied to 28 authentic human urine samples that tested positive in immunoassay screening and gas chromatography/mass spectrometry (GC/MS) tests. The ranges of concentrations of THCCOOH and THCCOOH-glucuronide in the samples were less than LOQ~266.90 ng/mL and 6.43~2133.03 ng/mL, respectively. The concentrations of THCCOOH-glucuronide were higher than those of THCCOOH in all samples. This method can be effectively and successfully applied for the confirmation of cannabinoid use in human urine samples in the forensic field.

A Study on the analysis method and composition characteristics of organic materials in the pottery excavated at the palace site in Yongjangseong Fortress, Jindo (진도 용장성 왕궁지 출토 도기호 내부 유기물의 분석법과 성분 특성 연구)

  • YUN Eunyoung;YU Jia;KIM Kyuho
    • Korean Journal of Heritage: History & Science
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    • v.56 no.3
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    • pp.158-171
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    • 2023
  • Pottery filled with organic materials was excavated from the G-2 building site of Yongjangseong Fortress, Jingo, a relic of the Goryeo Dynasty. In this study, the characteristics of organic material were confirmed by a scientific analysis of organic material in pottery found at the palace in Yongjangseong, Jindo. In addition, it was intended to review the analysis method to identify the natural resin and to secure characteristic components(biomarkers) for each natural resin and use them as basic data in the future. The organic materials in the pottery were analyzed using attenuated total reflectance Fourier-transformed infrared spectroscopy(ATR-FTIR) and gas chromatography mass spectrometry(GC-MS). The infrared spectral characteristics were estimated to be natural resin, and biomarkers of organic materials were identified as sesquiterpene-based compounds(C15H24, MW 204) and derivatives. The lacquer(T.vemicifluum) is composed mainly of alkenes, alkanes, and catechol. Pine resin(P.densiflora), on the other hand, is primarily composed of diterpenoid(abietic acid, pimaric acid) and Whangchil(yellow lacquer) is identified to have sesquiterpenes(such as selinene, muurolene, calamenene) as its main components. So, the organic material in the pottery can be identified as Whangchil by comparing their compounds with modern resin materials from Dendropanax. morbifera that correspond with the results. Whangchil, which is exuded from the Dendropanax. morbifera, has been used as a natural coating materials since ancient times, and it has been confirmed that the characteristic components are well preserved even 700 years later. It can be assumed that the interior Whangchil was stored not for use as a coating, but rather for ritual purposes when the building was constructed, because the pottery was found near the cornerstone. Furthermore, based on simplified sample preparation using pyrolysis-gas chromatography mass spectrometry(Py-GC-MS), the thermal decomposition products were found to be similar to the characteristic components, suggesting that this method can be applied to the identification of natural resins used in historic artifacts.

Analysis of E,E-farnesol and squalene in makgeolli using stir bar sorptive extraction coupled with gas chromatography-mass spectrometry (SBSE-GCMS를 이용한 막걸리 중의 E,E-farnesol과 squalene분석법)

  • Ha, Jaeho;Shim, You-Shin;Cho, Yongsun;Seo, Dongwon;Jang, Hyewon;Jang, Hyejin
    • Analytical Science and Technology
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    • v.27 no.1
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    • pp.60-65
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    • 2014
  • The aim of this study was to establish an analytical method for the determination of E,E-farnesol and squalene in makgeolli, which is a traditional type of Korean fermented rice wine. E,E-farnesol and squalene in makgeolli were extracted using stir bar sorptive extraction (SBSE) coupled with gas chromatography-mass spectrometry. SBSE was found to be an effective method for analyzing the E,E-farnesol and squalene levels in makgeolli. The linear dynamic range of the SBSE method for detecting E,E-farnesol and squalene ranged from 0.5 to 200 ng/mL with $R^2=0.9974$ for E,E-farnesol and 100 to 50000 ng/mL with $R^2=0.9982$ for squalene. The limit of detection and the limit of quantification using the SBSE method were 0.1 and 0.5 ng/mL for E,E-farnesol and 15.0 and 40.0 ng/mL for squalene, respectively. The average recoveries obtained were, quantitatively, 101-107% for E,E-farnesol and 98-103% for squalene, respectively, supporting the accuracy of the SBSE-GCMS method.

Volatile Aromatic Components of Ginger(Zingiber officinalis Roscoe) Rhizomes and Japanese Spice Bush(Lindera obtusiloba BL) (생강과 생강나무의 향기성분조성 비교)

  • 문형인;이재학
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.42 no.1
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    • pp.7-13
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    • 1997
  • The composition and chemical structures of same individual components of essential oils from ginger flavor plants were estimated by gas chromatography and gas chromatography-mass spetrometric analysis with the aid of NBS and Wiley library and RI indice searches. Through gas chromatography and gas chromatography /mass spetrometry analysis of 43, 41, 32 essential oil components from flowers, leaves and stems from Lindera obstusiloba., respectively were identified, among which sabinene, $\beta$-myrcene, ι-limonene, phelandrene, ${\gamma}$-selinene, $\alpha$-terpinene, 2, 4a, 5, 6, 7, 8, 9, 9a -octahydro benzocycloheptane, $\delta$-cadinene, ${\gamma}$-terpinene, (Z) -3-hexen-1-ol acetate, ${\gamma}$-elemene, l-boreneol, $\delta$-guaiene, ledene, cis-3-hexanal, elemol, $\alpha$-chamigrene, $\beta$-endesmol: 9-octadecanal, 1-(1, 5-diMe-4-hexenyl)-4-Me. benzene were estimated to be major components.

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Emission Characteristics of HFC-23 (CHF3)/HCFC-22 (CHClF2) between Different Air Masses in Northeastern Asia (동북아시아 지역에서의 공기괴별 HFC-23/HCFC-22의 배출특성)

  • Li, Shanlan;Kim, Joo-Il;Kim, Kyung-Ryul;Muhle, Jens
    • Journal of Korean Society for Atmospheric Environment
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    • v.26 no.5
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    • pp.490-498
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    • 2010
  • HCFC-22 (chlorodifluoromethane, $CHClF_2$), one of the major components in various refrigeration, is emitted mostly from developing countries, as its consumption is not limited until 2013 by the Montreal Protocol. In addition, HFC-23 (trifluoromethane, $CHF_3$), a by-product in the manufacture of HCFC-22, is also a powerful greenhouse gas. Here, we discuss the regional emission characteristics of these compounds based on high-frequency in-situ measurements using the "Medusa" GC-MS system. HCFC-22 and HFC-23 baseline concentrations measured at Gosan (Jeju Island, Korea) from November 2007 to December 2008 increased by 1.8 ppt/yr and 0.6 ppt/yr, respectively. Pollution events of these compounds were observed, very frequently (e.g., ~2~3 times) at Gosan than baseline levels. All the measurement data were divided into four groups by simultaneously considering the ratio (HFC-23/HCFC-22) and concentration (HCFC-22) at Trinidad Head (TH, California, USA). The residence time of trajectories were then analyzed in each of the four groups. The results exhibited the existence of a strong correlation with air mass origin for each group: 1) Air masses originating from Siberia in the north and from the Pacific in the south had ratios of 0.08~0.12 and concentrations of 196.9~254.3 ppt which is highly comparable to background air at TH. 2) Air masses passing over the Southern China exhibited similar ratios but higher HCFC-22 concentrations. 3) Air masses passing over the Northern China had ratios of 0.12~0.21. 4) Air masses passing over Korea and/or Japan had ratios of 0.01~0.08. Our results suggest that the HFC-23/HCFC-22 ratio can be used as a good indicator for the assessment of the pollution with Chinese origin. We also confirmed differences in air masses traveling over Northern and Southern China, most likely due to differences in air mass travelling speed over these regions before arriving at Gosan. This signature may be treated as one of the critical components in identifying the emission sources from different parts of China.

Simultaneous Analytical Method for the Neomycin, Gentamicin Residues in Seafood (수산물 중 네오마이신, 겐타마이신 동시분석법 개발)

  • Hong, Young-Min;Lee, Seok-Ki;Kim, Hyoung-Ah;Hwang, Yu-Kyung
    • Journal of Applied Biological Chemistry
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    • v.53 no.1
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    • pp.25-30
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    • 2010
  • This paper describes a simultaneous method for the determination of two aminoglycosides (neomycin and gentamicin) using solid phase extraction followed by liquid chromatograph-mass spectrometry. The extract was applied to an WCX and HLB solid phase extraction cartridge. The cartridges were washed with water and methanol, and analytes were eluted with TCA buffer-acetonitrile mixture. The aminoglycosides were separated by ion-pairing reversed phase mode prior to ESI-LC/MS. Under the conditions applied neomycin was almost separated from all the gentamicin compounds. No interfering peaks from endogenous compounds of matrix were noted at the elution position of the analytes. Recoveries of neomycin fortified at levels of 0.25, 0.5, 1.0 and 2.0 mg/kg seafood samples ranged from 92 to 115%. Recoveries of gentamycin fortified at levels of 0.05, 0.1, 0.2, 0.4 mg/kg seafood samples ranged from 99 to 116%. Method detection limits in four seafood sample matrices were between 0.002 and 0.033 mg/kg.

Mass-Based Metabolomic Analysis of Lactobacillus sakei and Its Growth Media at Different Growth Phases

  • Lee, Sang Bong;Rhee, Young Kyoung;Gu, Eun-Ji;Kim, Dong-Wook;Jang, Gwang-Ju;Song, Seong-Hwa;Lee, Jae-In;Kim, Bo-Min;Lee, Hyeon-Jeong;Hong, Hee-Do;Cho, Chang-Won;Kim, Hyun-Jin
    • Journal of Microbiology and Biotechnology
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    • v.27 no.5
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    • pp.925-932
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    • 2017
  • Changes in the metabolite profiles of Lactobacillus sakei and its growth media, based on different culture times (0, 6, 12, and 24 h), were investigated using gas chromatography-mass spectrometry (MS) and liquid chromatography-MS with partial least squares discriminant analysis, in order to understand the growth characteristics of this organism. Cell and media samples of L. sakei were significantly separated on PLS-DA score plots. Cell and media metabolites, including sugars, amino acids, and organic acids, were identified as major metabolites contributing to the difference among samples. The alteration of cell and media metabolites during cell growth was strongly associated with energy production. Glucose, fructose, carnitine, tryptophan, and malic acid in the growth media were used as primary energy sources during the initial growth stage, but after the exhaustion of these energy sources, L. sakei could utilize other sources such as trehalose, citric acid, and lysine in the cell. The change in the levels of these energy sources was inversely similar to the energy production, especially ATP. Based on these identified metabolites, the metabolomic pathway associated with energy production through lactic acid fermentation was proposed. Although further studies are required, these results suggest that MS-based metabolomic analysis might be a useful tool for understanding the growth characteristics of L. sakei, the most important bacterium associated with meat and vegetable fermentation, during growth.

Studies on the EPA(eicosapentaenioc acid) production by marine bacteria (해양세균(海洋細菌)을 이용(利用)한 EPA(eicosapentaenoic acid) 생성(生成)에 관한 연구(硏究))

  • Joh, Yong-Goe;Kim, Seong-Jin;Kim, Ji-Soo;Lee, Min-Kyeng
    • Journal of the Korean Applied Science and Technology
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    • v.12 no.2
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    • pp.121-130
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    • 1995
  • This project has been worked out for isolation of EPA-producing bacteria from marine source of sea water, sea sediment and intestinal contents eviscerated from some red-muscle fish such as mackerel, horse-mackerel and spike fish. The samples were precultured on the media of PPES-II glucose broth and then pure-cultured on Nutrient agar and P-Y-M glucose. Lipids extracted from those bacterial mass collected by centrifugation were analysed in terms of lipid class and fatty acid composition. The results are resumed as follows : 1. 112 strains from sea water and 76 strains from sea sediment were tested for their EPA producing capability, but both strains of (SA-67 and SA-91) from the former and four strains(SS-35, 37, 51 and 71) from the latter have been proved to produce EPA above the level of 2% of total fatty acids. The strains such as GS-11, 29, 31, HM-9, 29, B-18, 33, 107, YL-129, 156, 203, 77, 104 and 256 which were isolated from fish intestinal contents, have also produced EPA at higher level than 2% of total fatty acids. 2. Contents of total lipids extracted from the cultures of these strains grown at $25^{\circ}C$, range from 2.8% to 6.9% (on dry weight %), and they are mainly composed of polar lipids($40.9{\sim}52.9%$) such as phosphatidyl glycerol($^{+}cardiolipin$)(?) and phosphatidyl ethanolamine ($33.8{\sim}40.0%$), with smaller amount of free fatty acid ($11.2{\sim}20.2%$). 3. EPA was isolated from a mixture of fatty acid methyl esters obtained from the lipid of each strain by HPLC in silver-ion mode and was identified by GC-Mass spectrometry. 4. The strains of SW-91, GS-11, GS-29, HM-9, B-18 and YL-203 grown at $25^{\circ}C$ have a level of 5% EPA in their total fatty acids, and the GS-11 and HM-9 strains show a tendency of increase in the EPA level with an increase of growth temperature.

Effect of Carbon Dioxide in Fuel on the Performance of PEMFC (연료중의 이산화탄소 불순물에 의한 고분자전해질연료전지의 성능변화 연구)

  • Seo, Jung-Geun;Kwon, Jun-Taek;Kim, Jun-Bom
    • Journal of the Korean Electrochemical Society
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    • v.11 no.1
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    • pp.42-46
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    • 2008
  • Even though fuel cell have high efficiency when pure hydrogen from gas tank is used as a fuel source, it is more beneficial to generate hydrogen from city gas (mainly methane) in residential application such as domestic or office environments. Thus hydrogen is generated by reforming process using hydrocarbon. Unfortunately, the reforming process for hydrogen production is accompanied with unavoidable impurities. Impurities such as CO, $CO_2$, $H_2S$, $NH_3$, $CH_4$, and $CH_4$ in hydrogen could cause negative effects on fuel cell performance. Those effects are kinetic losses due to poisoning of the electrode catalysts, ohmic losses due to proton conductivity reduction including membrane and catalyst ionomer layers, and mass transport losses due to degrading catalyst layer structure and hydrophobic property. Hydrogen produced from reformer eventually contains around 73% of $H_2$, 20% or less of $CO_2$, 5.8% of less of $N_2$, or 2% less of $CH_4$, and 10ppm or less of CO. This study is aimed at investigating the effect of carbon dioxide on fuel cell performance. The performance of PEM fuel cell was investigated using current vs. potential experiment, long run(10 hr) test, and electrochemical impedance measurement when the concentrations of carbon dioxide were 10%, 20% and 30%. Also, the concentration of impurity supplied to the fuel cell was verified by gas chromatography(GC).

Cause Analysis in Candle Fire Investigation (양초화재 원인 감정에 관한 연구)

  • Han, Dong-Hun
    • Fire Science and Engineering
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    • v.30 no.3
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    • pp.104-109
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    • 2016
  • Candle fires do not occur frequently, but can easily result in death. In this study, the thermal characteristics of candles and conditions and debris of candle fires were investigated to determine the causes of candle fires. The rates of decrease in weight of 10 candles were measured and found to be between 2.6 g/h and 6.7 g/h. Most candle fires are caused by the ignitiong of combustible materials close to them. The temperature near a candle ranges from about $200^{\circ}C$ to $400^{\circ}C$ at a distance of 1 cm and low ignition temperature materials such as papers can easily catch fire. The melting temperature of candles ranges between $50^{\circ}C$ and $70^{\circ}C$ and their major chemical components are fatty acids and normal hydrocarbons (over C20). Using pretreatment conditions involving the use of activated charcoal strips at $150^{\circ}C$ for 16 hours, the fire debris including candle residues were analyzed using a Gas-chromatograph/Mass-spectrometer (GC/MS).