• Title/Summary/Keyword: gc/ms

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Structural Determination of Cerebrosides from Soybean Embryo by Mass Spectrometer (Mass Spectrometer를 이용한 대두 배아 출추 Cerebroside의 구조 분석)

  • Kim, Jung-Hun;Chang, Sug-Youn;Kim, Yeo-Kyung
    • Analytical Science and Technology
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    • v.6 no.3
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    • pp.335-343
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    • 1993
  • The structure of cerebrosides from soybean embryo was determined using fast atom bombardment mass spectrometer (FAB-MS), gas chromatography mass spectrometer (GC-MS) and TLC. The components of cerebroside were determined by GC-MS after acid hydrolysis. The molecular weight distribution of cerebroside was measured by positive mode FAB-MS with LiOH saturated 3-nitrobenzylalcohol(3-NBA) matrix. Structures of individual components of complex mixtures can be determined easily by this process. The major constituent of soybean extracted cerebroside was determined as the glucoside of N-2'-hydroxypalmitoyl-sphingadienine.

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Application of Comprehensive 2D GC-MS and APPI FT-ICR MS for More Complete Understanding of Chemicals in Diesel Fuel

  • Cho, Yun-Ju;Islam, Annana;Ahmed, Arif;Kim, Sung-Hwan
    • Mass Spectrometry Letters
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    • v.3 no.2
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    • pp.43-46
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    • 2012
  • In this study, comprehensive two dimension gas chromatography (2D GC-MS) and 15 T Fourier transform ion cyclotron resonance mass spectrometry (15T FT-ICR MS) connected to atmospheric pressure photo ionization (APPI) have been combined to obtain detailed chemical composition of a diesel oil sample. With 2D GC-MS, compounds with aliphatic alkyl, saturated cyclic ring(s), and one aromatic ring structures were mainly identified. Sensitivity toward aromatic compounds with more than two aromatic rings was low with 2D GC-MS. In contrast, aromatic compounds containing up to four benzene rings were identified by APPI FT-ICR MS. Relatively smaller abundance of cyclic ring compounds were found but no aliphatic alkyl compounds were observed by APPI FT-ICR MS. The data presented in this study clearly shows that 2D GC-MS and 15T FT-ICR MS provides different aspect of an oil sample and hence they have to be considered as complementary techniques to each other for more complete understanding of oil samples.

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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Development of the Analytical Method for Diazepam in Fishery Products using Liquid and Gas Chromatography-tandem Mass Spectrometry (LC-MS/MS 및 GC-MS/MS를 활용한 수산물 중 디아제팜의 정량분석법 개발)

  • Shin, Dasom;Kang, Hui-Seung;Kim, Joohye;Jeong, Jiyoon;Rhee, Gyu-Seek
    • Journal of Food Hygiene and Safety
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    • v.33 no.2
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    • pp.110-117
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    • 2018
  • The aim of this study was to develop an analytical method for the quantification of diazepam residues in fishery products, using liquid and gas chromatography-tandem mass spectrometry (LC-MS/MS and GC-MS/MS). The sample utilized in the study was extracted from the fish sample (crucian carp) using 0.1% formic acid in acetonitrile. For the utilization of the purification process, the dispersive solid phase extraction (dSPE) was used for LC-MS/MS, dSPE and SPE was used for GC-MS/MS, respectively. To be sure, the standard calibration curves showed a good linearity as the noted correlation coefficients, $r^2$ was > 0.99. The average recoveries for accuracy ranged in 99.8~124% for the samples which were fortified at three different levels (0.001, 0.002 and 0.010 mg/kg). The correlation coefficient for the precision effect was measured at a range of 4.01~11.8%. The limit of detection (LOD) for the diazepam analysis was 0.0004 mg/kg, and the limit of the quantification (LOQ) was 0.001 mg/kg. The proposed analytical method was characterized with a high accuracy and acceptable sensitivity to meet the established Codex Alimentarius Commission (CAC/GL71-2009) guideline requirements. We therefore established the optimal analysis method for the determination of diazepam in the fishery products using LC-MS/MS and GC-MS/MS. It would be applicable to analyze the diazepam residues in fishery products in further studies on this subject.

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 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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Multi-residue Analysis of Pesticides using GC-TOF/MS, ECD, NPD with QuEChERS Sample Preparation (QuEChERS 전처리법과 GC-TOF/MS, ECD, NPD를 이용한 잔류농약 다성분분석)

  • Park, Jungwook;Kim, Aekyung;Kim, Jongpil;Lee, Hyanghee;Park, Duckwoong;Moon, Sujin;Ha, Dongryong;Kim, Eunsun;Seo, Kyewon
    • The Korean Journal of Pesticide Science
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    • v.18 no.4
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    • pp.278-295
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    • 2014
  • Fast and accurate multi-residue pesticides inspecting method needs in Agro-Fishery Products Inspection Center. So, We tried to seek the optimum method using GC-TOF/MS, GC-ECD, GC-NPD after QuEChERS sample preparation. In GC-TOF/MS, 138 kinds of pesticide were spiked at 0.3 and $0.5{\mu}g/g$for the identification and quantification in lettuce sample. Recoveries of 77 pesticides were between 70 and 130% with RSD (relative standard deviation lower than 20% at $0.3{\mu}g/g$. In GC-ECD, NPD, 146 kinds of pesticide were spiked for the identification and quantification in lettuce. Recoveries of 61 species were between 70 and 130% with lower than 20%. These results indicated that GC-TOF/MS, GC-ECD, NPD analysis with the QuEChERS sample preparation can be partly applied to multi-residue pesticides in vegetables.

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.

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.

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.