• Title/Summary/Keyword: GC-MS/MS

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Analysis of Plant Hormones using GC-MS (GC-MS를 이용한 식물홀몬 분석)

  • 조광연
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.34 no.s01
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    • pp.26-32
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    • 1989
  • The analytic principles of GC and MS were explained in relation to plant hormone analyses and the characteristics of two instruments were compared. The selection of column, condition of measurement and the method of ionization to get a good spectrum were also briefly described. Finally, the pre-treatment of sample by solvent extraction method to remove the unnecessary part of sample and the synthetic method, especially reagents and reaction condition, for the preparation of ether or ester derivative which can be easily vaporized in GC were explained.

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Determination of N-nitrosamines in Water by Gas Chromatography Coupled with Electron Impact Ionization Tandem Mass Spectrometry (EI-GC/MS/MS를 이용한 니트로사민류의 수질분석)

  • Lee, Ki-Chang;Park, Jae-Hyung;Lee, Wontae
    • Journal of Korean Society of Environmental Engineers
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    • v.36 no.11
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    • pp.764-770
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    • 2014
  • This study assessed analysis of N-nitrosamines by separation, identification, and quantification using a gas chromatography (GC) mass spectrometer (MS) with electron impact (EI) mode. Samples were pretreated by a automated solid phase extraction (SPE) and a nitrogen concentration technique to detect low concentration ranges. The analysis results by EI-GC/MS (SIM) and EI-GC/MS/MS (MRM) on standard samples with no pretreatment exhibited similar results. On the other hand, the analysis of pretreated samples at low concentrations (i.e. ng/L levels) were not reliable with a EI-GC/MS due to the interferences from impurity peaks. The method detection limits of eight (8) N-nitrosamines by EI-GC/MS/MS analysis ranged from 0.76 to 2.09 ng/L, and the limits of quantification ranged from 2.41 to 6.65 ng/L. The precision and accuracy of the method were evaluated using spiked samples at concentrations of 10, 20 and 100 ng/L. The precision were 1.2~13.6%, and the accuracy were 80.4~121.8%. The $R^2$ of the calibration curves were greater than 0.999. The recovery rates for various environmental samples were evaluated with a surrogate material (NDPA-$d_{14}$) and ranged 86.2~122.3%. Thus, this method can be used to determine low (ng/L) levels of N-nitrosamines in water samples.

Quantitative Analysis of the Seven Marker Components in Asarum sieboldii using the LC-MS/MS and GC-MS (LC-MS/MS와 GC-MS를 이용한 세신 추출물 중 7종 성분의 함량분석)

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Korean Journal of Pharmacognosy
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    • v.44 no.4
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    • pp.350-361
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    • 2013
  • Asarum sieboldii has been used for treatment of fever, pain, common cold, and chronic sinusitis in Korea. In this study, we performed quantification analysis of seven major constituents including aristolochic acid I, aristolochic acid II, ${\alpha}$-asarone, ${\beta}$-asarone, elemicin, methyl eugenol, and safrole in the 70% ethanol extract of Asarum sieboldii and its solvent fractions, n-hexane, ethylacetate, n-butanol, and water ones using a ultra-performance liquid chromatography-electrospray ionization-mass spectrometer(UPLC-ESI-MS) and gas chromatography-mass spectrometer(GC-MS). Regression equations of seven components were acquired with $r^2$ values >0.99. The values of limit of detection(LOD) and quantification(LOQ) were 0.1-3.9 ng/mL and 0.3-11.7 mg/mL, respectively. The amount of the seven compounds in Asarum sieboldii were not detected -143.66 mg/g. The established LC-MS/MS and GC-MS methods will be helpful to improve quality control of Asarum sieboldii.

Analysis of Agrochemical Residues in Tobacco Using QuEChERS Method by GC-MS/MS

  • Lee, Jeong-Min;Jang, Gi-Chul;Hwang, Keon-Joong
    • Journal of the Korean Society of Tobacco Science
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    • v.29 no.2
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    • pp.132-139
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    • 2007
  • This study was performed to apply the more rapid and accurate sample preparation, and the high selectivity and sensitivity of the analyte detection by gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). QuEChERS (quick, easy, cheap, effective, rugged and safe) method was validated for 49 agrochemicals in the CORESTA Agrochemical Advisory Committee guide and amenable to GC-MS/MS determination. In QuEChERS method, the effects of sorbents (PSA, $C_{18}$ and GCB) and matrix of the analytes in tobacco types (flue-cured, burley and oriental) were investigated. MS/MS acquisition provided high specificity and selectivity for agrochemicals and low limit of quantification. QuEChERS by using PSA alone and the matrix-matched standards gave good recoveries and RSD values in three types of tobaccos. QuEChERS method was no needed to be complex clean-up procedure and would be used as the fast and easy method for agrochemical residue analysis in tobacco.

Analysis of Residual Pesticides in Herbal Drugs: GC/MS Analysis of 27 Controlled Pesticides (생약 중 잔류 농약의 분석법: GC/MS에 의한 27종 잔류 규제 농약의 분석)

  • Park, Man-Ki;Park, Jeong-Hill;Yoon, Hye-Ran;Yoon, In-Byoung;Cho, Sool-Yeon;Hwang, Gwi-Seo
    • YAKHAK HOEJI
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    • v.40 no.2
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    • pp.141-148
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    • 1996
  • GC/MS analysis of 27 controlled pesticides in herbal drugs was studied. Selected ion monitoring(sim) technique was applied to increase the GC/MS sensitivity. Typical peaks in th e mass spectrum of each pesticides were selected as quantitation, comfirmation or alternate ion. Twenty seven pesticides were divided into five groups according to their retention time and the peaks for SIM were programmed accordingly. The combination of two ionization methods, electron impact(EI)-SIM-MS and negative ion chemical ionization(NCI)-SIM-MS, were well-fitted for the detection, confirmation and quantitation of multiclass residual pesticides in herbal drugs.

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The Comparison of VOC Characteristics Emitted from Wood-based Panels Using GC/FID and GC/MS (GC/FID와 GC/MS 분석법에 의한 목질제품에서의 VOC 방출특성 비교)

  • Hwang, Yoon-Seo;Park, Hyun-Ju;Son, Youn-Suk;Kim, Jo-Chun
    • Journal of Korean Society for Atmospheric Environment
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    • v.27 no.4
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    • pp.436-442
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    • 2011
  • In this study, the Total Volatile Organic Compounds (TVOC) emitted from wood-based panels were compared by two analytical methods using the GC/FID and the GC/MS. Japanese Larch, Yellow Poplar, Particle Board (PB) and Medium Density Fiberboard (MDF) were selected as target materials. Major compounds emitted from the panels were Toluene, ${\alpha}$-pinene, ${\beta}$-pinene and limonene. In case of TVOC using GC/FID method, MDF E2 (1,497 ${\mu}g/m^3$) revealed the highest concentration among all wood-based panels, while Japanese Larch (1,772 ${\mu}g/m^3$) showed the highest value with respect to GC/MS method. Furthermore, it was found that the amount of VOC emitted from panels was different depending upon analytical methods. This significant difference was attributed to analytical sensitivities of GC/FID and GC/MS for various VOC. Besides, it was found that the composition ratios of main VOC compounds were not significantly different.

GC/MS and GC/ECD Analysis of Residual Pesticides in Herbal drugs (GC/MS와 GC/ECD를 이용한 한약재 중 잔류 농약의 분석)

  • Kim, Ho-Kyoung;Park, So-Yeon;Ko, Byoung-Seob
    • The Journal of Korean Medicine
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    • v.20 no.1 s.37
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    • pp.44-51
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    • 1999
  • Analysis of residual pesticides in herbal drugs was performed by GC-ECD and GC-MS. Especially, selected ion monitoring(SIM) technique was applied to increase the GC/MS sensitivity. Analysis of residual pesticides was determined sensitivity and selectively without any internal standard by setting the SIM technique to their characteristic fragments for quantitation ion and confirmation ion. The combination of two detector, GC-ECD and MS-SIM technique, is abailable for determining a multiclass residual pesticides in herbal drugs. The average recoveries through the method were $65.9%{\sim}99.7%$ in herbal drugs. The data of gas chromatographic analysis was compared with the limits of residual pesticides in herbal drugs and agricultural foods. 4. 4-DDT was detected above the limits to the residual pesticides in herbal drugs. Diazinon and EPN were detected, but the limits of residual pesticides were less than that of agricultural foods.

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Analysis of Cyclofenil and its Metabolites in Human Urine using GC/MS (GC/MS를 이용한 소변중의 Cyclofenil 및 그 대사체의 분석)

  • Myung, Seung-Woon;Min, Hye-Ki;Cho, Hyun-Woo;Kim, Dong-Hyun;Kim, Myungsoo
    • Analytical Science and Technology
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    • v.15 no.3
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    • pp.185-189
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    • 2002
  • International Olympic Committee (IOC) prohibits the use of cyclofenil for male. To prove whether cyclofenil product was taken or not, the analytical method in urine using GC/MS was established. The extraction recoveries of cyclofenil and its metabolites were higher in the range of pH 5-9. Because the parent drug (cyclofenil) was not excreted in urine, metabolites were detected and theses were used as a criteria of cyclofenil dose. Therefore the metabolites were hydrolyzed, extracted at pH 9.6, derivatized with MSTFA and analyzed by GC/MS.

Geographical origin discrimination of Korean variety, Angelica gigas Nakai by using TDU (Thermal Desorption Unit)-GC/MS (TDU-GC/MS를 이용한 한국품종 참당귀 국산 판별 기법)

  • Lee, Mi-Na;Kim, Yoon-Suk;Kim, Won-Il;Kim, Jeong-Gyu;Kwon, Oh-Kyung
    • Journal of Applied Biological Chemistry
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    • v.63 no.1
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    • pp.29-33
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    • 2020
  • The objective of this study was to develop a fast and accurate method of variety discrimination and geographical discrimination origin of Korean angelica (Korean variety, Angelica gigas Nakai) by using TDU-GC/MS. Two peaks of decursin and decursinol, which are coumarin derivatives were identified in the range of Total Ion Chromatogram (TIC) RT 26.9-27.2 of the Korean angelica by GC/MS analysis at the time of condensation in a refrigerated condensation system after thermal desorption of sample extracts. In case of Chinese angelica (Chinese variety), ligustilide peak was detected at the RT 17.2. In order to investigate the difference of volatile components according to the geographical origin of Korean variety, the mass spectra were measured by TDU-GC/MS at the range of m/z 40-400 amu. The TIC of domestic cultivation and Chinese cultivation of the Korean variety, Angelica gigas Nakai showed the same tendency as a whole. However, in partial scans of TIC, two peaks detected at 15.54 and 16.05 of RT showed different peak patterns between Korean angelica (Korean variety) cultivated in Korea and in China. The ratio of Peak A (RT 15.54) and B (RT 16.05) was 0.0-0.2 for domestic cultivation and 0.5-2.8 for Chinese cultivation, confirming the possibility of discriminating origin by comparing the TIC peak pattern of TDU-GC/MS.

Analysis of Synthetic Fragrances (SFs) in Water Using Stir Bar Sorptive Extraction (SBSE) and GC-MS/MS (교반막대 추출법과 GC-MS/MS를 이용한 수중의 합성 향물질류 분석)

  • Seo, Chang-Dong;Son, Hee-Jong;Yoom, Hoon-Sik;Choi, Jin-Taek;Ryu, Dong-Choon;Kwon, Ki-Won;Jang, Seung-Ho
    • Journal of Korean Society of Environmental Engineers
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    • v.36 no.6
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    • pp.387-395
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    • 2014
  • A highly sensitive analytical method based on stir bar sorptive extraction (SBSE) technique and gas chromatography/tandem mass spectrometry (GC-MS/MS) has been developed, allowing the simultaneous multi-analyte determination of 11 synthetic fragrances (SFs) in water samples. The stir bar coated with polydimethylsiloxane (PDMS) was added to 40 mL of water sample at pH 3 and stirred at 1,100 rpm for 120 min. Other SBSE parameters (salt effect and presence of organic solvent) were optimised. The method shows good linearity (coefficients > 0.990) and reproducibility (RSD < 10.9%). The extraction efficiencies were above 83% for all the compounds. The limits of detections (LOD) and limits of quantification (LOQ) were 2.1~4.1 ng/L and 6.6~12.9 ng/L, respectively. The developed method offers the ability to detect 11 SFs at ultra-low concentration levels with only 40 mL of sample volume. Matrix effects in tap water, river water, wastewater treatment plant (WWTP) final effluent water and seawater were investigated and it was shown that the method is suitable for the analysis of trace level of 11 SFs. The method developed in the present study has the advantage of being rapid, simple, high-sensitive and both user and environmentally friendly.