• Title/Summary/Keyword: GC/M S-SIM

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Distributions of Nicotine and Toluene in Teenagers' Urine (청소년의 뇨 중에서 nicotine과 톨루엔의 분포에 관한 연구)

  • Park, Sungwoo;Seo, Baeseck;You, Jaehoon;Kim, Namyee;Shin, Hosang;Han, Wansoo;Kim, Ilkwang
    • Analytical Science and Technology
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    • v.10 no.1
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    • pp.1-8
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    • 1997
  • We identified nicotine, cotinine and toluene in high school volunteer's urine by using GC/NPD, GC/FID and GC/MS. To analyze of nicotine and cotinine, urine samples were extracted with diethylether and centrifuged on a benchtop centrifuge for 5 min. The upper organic layer was injected into a GC. The distributions of nicotine and cotinine were $4{\sim}630{\mu}g/L$ and $63{\sim}1,602{\mu}g/L$ in smoking-group, respectively. To analyze of toluene, head space vial was filled with 2mL sodium citrate solution and 1mL of urine. The vial was warmed in a water bath at $55^{\circ}C$ for 20min, and then $250{\mu}L$ of head space air was injected into a GC. The result show that toluene was not detected in all of the volunteers' samples. However, the range of toluene was 0.1~28.0mg/L in glue sniffer's urine samples(NISI data).

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A Rapid, Simple Determination of Sulfur-containing Compounds and Methylmalonic Acid on Plasma using GC-MS-SIM for the Diagnosis of Homocysteinemia (혈장 중 황함유 화합물과 메틸말론산의 신속 간편한 분석법 개발; GC-MS-SIM을 이용한 호모시스테인혈증의 진단)

  • Yoon, Hye-Ran;Thapa, Maheshwor
    • Journal of The Korean Society of Inherited Metabolic disease
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    • v.15 no.3
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    • pp.138-146
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    • 2015
  • Purpose: If early diagnosis is not made, patients with metabolic disorders as homocystinemia rapidly progress to physical defect or mental retardation resulted in storage of the toxic material into the brain. Therefore, it is necessary to develop an analytical method for a rapid screening and/or correct confirmation diagnosis. Methods: The standard solution of sulfur amino acids spiked plasma was subjected to protein precipitation with methanol, and then consecutively derivatized with trimethylsilyl (TMS) and trifluoroacyl (TFA) and determined by GC-MS. The formation of TMS derivative of the hydroxyl and TFA derivative of amino functional group was performed by BSTFA and MBTFA, respectively. Selective ion monitoring (SIM) mode was used for quantification with selected specific ions. Results: A calibration curve on standard spiked pooled plasma showed a linear relationship with correlation coefficient of 0.9936-0.9992 for all compounds over the range of 0.1-300 ng. The precision and accuracy were within S.D. of 1-15% and RSD of 1-15% for intra-day assay at 2 ng/mL, 15 ng/mL and 30 ng/mL. LOD and LOQ was 0.4 ng/mL and 4 ng/mL respectively. Conclusion: A rapid analytical method was developed to quantify sulfur amino acids and methyl malonic acid, after two-step derivatization procedure with good sensitivity and specificity on human plasma. Advantages of a new method are simplicity and rapidity. The method could be useful for routine analysis, diagnosis of homocysteinemia.

Mean Velocity of Globular Cluster Systems in M86 Virgo Giant Elliptical Galaxy and Massive Early-Type Galaxies

  • Park, Hong Soo;Lee, Myung Gyoon;Arimoto, Nobuo
    • The Bulletin of The Korean Astronomical Society
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    • v.40 no.2
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    • pp.33.3-34
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    • 2015
  • We present the spectroscopic study of the globular clusters (GCs) in the massive elliptical galaxy M86 in the Virgo galaxy cluster. Using the spectra obtained from the Multi-Object Spectroscopy (MOS) mode of Faint Object Camera and Spectrograph (FOCAS) on the Subaru Telescope, we measure the radial velocities for 56 GCs in M86. The mean velocity of the GCs is derived to be $<v_p>=-335{\pm}41km/s$, which is different from the velocity of the M86 nucleus ($<v_{gal}>=-224{\pm}5km/s$) within ${\sim}2.5{\sigma}$. The mean velocity ($<v_p>=-342{\pm}60km/s$) of 33 blue GCs in M86 is similar to that ($<v_p>=-314{\pm}71km/s$) of 23 red GCs. We also derive the mean velocities of the GC systems in other 16 nearby early-type galaxies (ETGs) from the radial velocity data in the literature. The mean value of the differences between the mean velocity of the GC systems in each galaxy and the nucleus velocity of their host galaxies, is almost zero except the M86 GC system. But the scatter of the differences in the blue GC system is larger than that in the red GC system. We will discuss these results in the context of GC formation in ETGs.

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Effect of Various Plasticizers and Ferulic Acid on the Physical Properties of Gelidium corneum Film (다양한 가소제와 Ferulic Acid 처리한 Gelidium corneum 필름의 물성)

  • Lim, Geum-Ok;Hong, Yun-Hee;Song, Kyung-Bin
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.38 no.6
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    • pp.727-731
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    • 2009
  • Effects of various plasticizers (1.5%) such as glycerol, sorbitol, fructose, sucrose, and polypropylene glycol, and ferulic acid on the physical properties of Gelidium corneum (GC) film were examined. GC films containing plasticizer and ferulic acid were prepared by incorporating various amounts (10, 30, 50, 70, 100 mg/100 mL) of ferulic acid into the film. Water vapor permeability (WVP) of the GC film varied depending on the type of plasticizer, and among them the film containing sucrose had the lowest WVP. Tensile strength (TS) and % elongation (%E) of the film were in the range of $1.29{\sim}11.29$ MPa and $5.55{\sim}36.44$ %, respectively, and the WVP values were of $1.30{\sim}1.60\;ng\;m/m^{2}sPa$. In addition, the GC films were prepared using ferulic acid as a cross-linking agent. WVP of the film decreased with the addition of ferulic acid, and the film containing 30 mg ferulic acid had the lowest WVP value. TS value of the GC film containing 10 mg of ferulic acid was significantly higher than that of the control. However, further increase of ferulic acid concentration decreased the TS value. Therefore, 10 mg of ferulic acid was determined to be the optimal concentration for the film.

Simultaneous Determination of C22-C26 Very Long - Chain Fatty Acids Following tert-Butyldimethylsilyl Derivatization by Stable Isotope GC- MS for the Screening of Adrenoleucodystrophy

  • Yoon, Hye-Ran
    • Biomolecules & Therapeutics
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    • v.15 no.4
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    • pp.266-272
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    • 2007
  • A rapid analytical method was developed to quantify very long-chain fatty acids (VLCFAs, C22:0, C24:0, C26:0) in human plasma with good sensitivity and specificity using tert-butyldimethylsilyl (TBDMS) derivatization and stable isotope GC-MS selective ion monitoring (GC-MS/SIM). Two-hundred and fifty ${\mu}L$ of plasma was fortified with deuterated stable isotope internal standards (d3-C22:0, d3-C24:0, d3-C26:0) and standard mixtures of chloroform and methanol, and then extracted with hexane and acetonitrile. To upper layer of liquid-liquid-extraction, N-(t-Butyldimethylsilyl)-N-methyltrifluoroacetamide was added and then heated to $60^{\circ}C$ for 30 min to produce the TBDMS derivatives. Derivatives of VLCFAs were analyzed by GC-MS/SIM. Calibration curves showed a linear relationship for the target compounds in the concentration range of $10^{-4}{\sim}2{\times}10^3\;{\mu}g/mL$ with the correlation coefficient ranging from 0.996 to 0.999. The limit of quantification for the plasma was $10^{-4}{\sim}2{\times}10^{-4}\;{\mu}g/mL$ (S/N=3). When applied to the plasma specimens of patients with peroxisomal disorder, X-linked adrenoleucodystropy (ALD, Mckusick 202370), the method clearly differentiated normal subjects from ALD patients. The C24:0/C22:0 and C26:0/C22:0 ratios were significantly elevated in the plasma of patients with X-linked ALD compared to normal subjects. The new developed method might be useful for a rapid and sensitive diagnosis of X-linked ALD and other peroxisomal disorders.

Determination of sulforaphane in cruciferous vegetables by SIM (선택이온 측정법에 의한 십자화과 채소중의 Sulforahane 함량)

  • Kim, Mee-Ree;Lee, Kun-Jong;Kim, Jin-Hee;Sok, Dai-Eun
    • Korean Journal of Food Science and Technology
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    • v.29 no.5
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    • pp.882-887
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    • 1997
  • Quantitative determination of sulforaphane, S-methylsulfinylbutyl isothiocyanate in 20 cruciferous vegetables of Korean origin was performed. Homogenate of vegetable was extracted with dichloromethane, and the extract, after drying, was subjected to GC/MS analysis, which was based on single ion monitoring (SIM) at m/z 72, 160, 55, 114 and 177. The content of sulforaphane was found to be the highest in the extract of broccoli $(80.2{\sim}617.7\;ppm)$ followed by turnip $(15.4{\sim}23.1\;ppm)$, red cabbage $(9.9{\sim}32.1\;ppm),\;radish\;(5.5{\sim}8.8\;ppm)$ and kale (8 ppm). Among various cultivars of broccoli, broccoli '1243' and broccoli 'Pilgrim' showed higher content of sulforaphane than others. Especially, in the stem of broccoli '1243' and the floret of broccoli 'Pilgrim' the amount of sulforaphane was the highest (>700 ppm). Thus, the content of sulforaphane differed according to the cultivars and the portion of the vegetables.

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Determination of Lignan Compounds in Fruits of Schisandra chinensis BAILLON by Capillary-GC(FID) (Capillary-GC(FID)에 의한 오미자 Lignan 성분의 정량)

  • Sohn, Hyun-Joo;Bock, Jin-Young;Baik, Soon-Ok;Kim, Yong-Ha
    • Applied Biological Chemistry
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    • v.32 no.4
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    • pp.350-356
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    • 1989
  • The determinabilities of several lignan compounds by capillary-GC (F1D) were studied. The lignan compounds used were deoxyschizandrin, gomisin N, schizandrin, wuweizisu C, gomisin A, angeloylgomisin H and tigloylgomisin H which were isolated from fruits of Schisandra chinensis BAILLON and identified with GC/MS(EI, 70eV), 1H-NMR(300MHz) and IR. The GC column used was SPB-1 fused silica capillary$(0.25mm\;ID{\times}30m,\;Supelco)$, and the column oven temperature was programmed from $200^{\circ}C$ to $300^{\circ}C$ at the rate of $4^{\circ}C$ per minute. The linearities between concentration and FID response were maintained in $2{\sim}500ppm$ of deoxyschizandrin and wuweizisu C and in $5{\sim}500ppm$ of gomisin N, schizandrin, gomisin A, angeloylgomisin H and tigloylgomisin H. The contents of lignan compounds in fruits of S. chinensis BAILLON produced at Moo-ju area were analyzed by the GC method: the values obtained of schizandrin and gomisin N were 6.5 and 5.9mg/g respectively, and those of gomisin A, wuweizisu C, angeloylgomisin H, deoxyschizandrin and tigloylgomisin H were $0.5{\sim}1.6mg/g$.

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Simultaneous determination of aromatic material causing allergic in children's products by Gas Chromatography (어린이 제품 중 가스 크로마토그래피를 이용한 알러지 유발 방향성 물질의 동시분석법)

  • Ko, Kyeong Mok;Rhu, Chan Joo;Kim, Jong Won;Lee, Seok Ki
    • Analytical Science and Technology
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    • v.31 no.1
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    • pp.23-30
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    • 2018
  • Twenty-two allergy-induced aromatics in children were analyzed using a gas chromatography flame ionization detector (GC-FID) and gas chromatography mass spectrometer (GC-MSD). Analytes were extracted using an automatic Soxhlet extractor and centrifuged for 10 min in a fast freezing centrifuge, and the supernatant was transferred into a 2 mL vial and injected in split mode. Under the established conditions, the calibration curve showed linearity with a correlation coefficient of 0.996 or more. A wide range of sensitivity of 6.7 to 1,859,839 depending on the device characteristics and detector used was shown. The detection limit of the device was 0.0032 to $0.0335{\mu}g/mL$, and the maximum detection limit was less than $0.1{\mu}g/mL$. The detection limit of the method ranged from 0.0033 to $0.1161{\mu}g/mL$. In addition, the limit of quantification ranged from 0.0100 to $0.5422{\mu}g/mL$, with a level of precision ranging from 0.21 % to 4.89 % and a degree of accuracy ranging from 89 % to 111 %. The analytical method developed in this study was applied to commercial products.

Feasibility study of membrane interface for gas chromatograph-mass spectrometry (기체크로마토그래프-질량분석기의 실리콘 분리막 인터페이스의 유용성 연구)

  • Kang, Gil Seon;Lee, Dong Soo;Lee, Hwa Sim;Park, Chang Joon
    • Analytical Science and Technology
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    • v.21 no.6
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    • pp.495-501
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    • 2008
  • Agilent 5973 GC-MS instrument was modified so that the capillary direct interface was removed and that a silicone membrane was installed between GC and MS. Feasibility study of the membrane interface GC-MS has been carried out. Vacuum of the mass spectrometer was not affected by the carrier gas flow rate up to $4.7m{\ell}/min$. As the carrier flow rate was increased, peak tailing was reduced and chromatogram peaks appeared earlier. Chromatogram peaks showed better separation and higher sensitivity as the membrane thickness was reduced from $127{\mu}m$ to $75{\mu}m$, and also as the interface temperature was increased. However, the membrane interface GC-MS had drawbacks such as background ions at 73 and 147 m/z and poor peak separation due to peak tailing.

Determination of chlorophenols from the industrial wastewater by GC/MS (GC/MS를 이용한 산업폐수중의 염화페놀류 분석)

  • Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.18 no.4
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    • pp.320-328
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    • 2005
  • The most common five chlorophenols (4-chloro-3-methylphenol, 2,4,5-trichlorophenol, 2,4,6-trichlorophenol, 2,3,4,6-tetrachlorophenol, pentachlorophenol) were determined from the industrial wastewater by GC/MS. The samples were collected from the petrochemical company, textile company and leather making company. The developed analytical method was modified by USEPA Method 3510. The samples were extracted with dichloromethane under pH 2 and pH 5-6, and determined by the GC/MS with SIM mode. There were good linearities (above $R^2=0.9943$) on e ranges of the 0.1 ng/mL~10 ng/mL and 0.5 ng/mL~10 ng/mL, and the limit of detection were between 0.1 ng/mL and 0.5 ng/mL. The absolute recoveries were measured at the concentration of 1, 5, and 10 ng/mL, and the recovery was 71.6~98.9% except for PCP. The relative standard deviation (RSD) was 1.2~14.3% and it gave a good reproducibility for the assay. The bias, which shows the accuracy, was a good although it was a little high values (11.3~22.1%) at the low concentration (1 ng/mL).