• Title, Summary, Keyword: selected ion monitoring

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Selected ion monitoring analysis of conjugated metabolites of methadone using biosynthetic internal standards for the study of methadone-diazepam interaction

  • Kang, Gun-Il
    • Archives of Pharmacal Research
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    • v.6 no.1
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    • pp.7-16
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    • 1983
  • A methadone-diazepam interaction study in rats was performed in which conjugated metabolites of methadone were analyzed using deuterated biosynthetic internal standards. Diazepam (5mg/kg) was given to rats through a cannulate djugular vein and a subcutaneous dose of methadone (10mg/kg) was given. Bile was collecte through the cannulate dbile duct over a period of 24 hours. The deuterium label of the internal standards was found to be stable under conditions of the prolonged incubation. There was no significant difference in the excretion of the metabolites between the control and the diazepam treated rats. Feasibility of using biosynthetic internal standards with selected ion monitoring was established for the drug metabolism and kinetic studies.

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Determination of 11 Phenolic Endocrine Disruptors using Gas Chromatography/Mass Spectrometry-Selected Ion Monitoring in Five Selected Wastewater Influents

  • Kim, Hyub
    • Environmental Engineering Research
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    • v.13 no.4
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    • pp.216-223
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    • 2008
  • An efficient method for the simultaneous determination of eleven phenolic endocrine-disrupting chemicals (EDCs) present in wastewater influent samples was described. The 11 phenolic EDCs including alkylphenols, chlorophenols, and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) following two work-up methods for comparison; isobutoxycarbonyl (isoBOC) derivatization and tert-butyldimethylsilyl (TBDMS) derivatization. The wastewater influent samples containing the 11 EDCs were adjusted to pH 2 with $H_2SO_4$ and then cleaned up with n-hexane. Next, they were subjected to solid-phase extraction (SPE) with XAD-4 resin and subsequently converted to isoBOC or TBDMS derivatives for sensitivity analysis with gas chromatography/mass spectrometry-selected ion monitoring (GC/MSSIM). Following isoBOC derivatization and TBDMS derivatization, the recoveries were 86.6-105.2% and 97.6-142.7%, the limits of quantitation (LOQ) for the 11 phenolic EDCs for SIM was 0.001-0.050 ng/mL and 0.003-0.050 ng/mL, and the SIM responses were linear with the correlation coefficient varying by 0.9717-0.9995 and 0.9842-0.9980, respectively. When these methods were applied to five selected wastewater influent samples, for isoBOC derivatization and TBDMS derivatization the ranges of concentration detected were 0.2-99.6 ng/mL and 0.4-147.4 ng/mL, respectively.

Application and Optimization of the IsoButoxycarbonyl Derivatization method to the Analysis of Trace Level Phenols in Environmental Samples (환경시료로부터 미량 페놀류의 분석을 위한 isoButoxycarbonyl 유도체화 분석방법 적용 및 최적화)

  • Kim, Hyub;Hong, Jong-Ki;Kim, Yong-Hwa;Kim, Kyoung-Rae
    • Environmental health and toxicology
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    • v.17 no.1
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    • pp.37-51
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    • 2002
  • Eleven phenols including two chlorophenols, eight alkylphenols and bisphenol A were derivatized with isobutylchloroformate to form their isobutoxycarbonyl derivatives. Standard phenol mixture was concentrated for the isobutoxycarbonyl (isoBOC) derivatization and analysed by gas chromatography/mass spectrometry (GC/MS). The recoveries of the derivatization method of alkylphenols, chlorophenols, and bisphenol A were calculated by gas chromatography/mass spectrometry-selected ion monitoring mode using two work-up methods for comparison; shaking and heating method. The linear detector responses were obtained in the concentration range of 5∼400 ng, with correlation coefficients varying from 0.9755∼0.9981. Recoveries of the alkylphenols, chlorophenols, and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring mode using two work-up methods for comparison ; the US-EPA method and the isoBOC derivatization method, Eleven phenols in water samples were extracted with dichloromethane and then concentrated. Also, solid-phase extraction (SPE) with XAD-4 and subsequent conversion to isobutoxycarbonyl derivatives for sensitive analysis with the selected ion-monitoring (SIM) mode. The recoveries were 85.1∼109.9% and 90.3∼126.6% for the US-EPA method and the isoBOC.

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
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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 Benzophenone in Sediment and Soil by Gas Chromatography/Mass Spectrometry (기체크로마토그래피/질량분석기에 의한 저질 및 토양시료 중 벤조페논의 분석법 연구)

  • 권오승;김은영;류재천
    • Environmental health and toxicology
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    • v.16 no.3
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    • pp.121-126
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    • 2001
  • Analytical method of benzophenone (BP) in sediment and soil was developed by gas chromatography/mass selective detector/selected ion monitoring (GC/MSD/SIM). The ultrasonic extraction of US EPA (method 3550B) method and liquid-liquid extraction for sediment and soil samples were used for the analysis of BP from sediment and soil. BP was extracted with n-hexane. Organic layer was washed with 5% sodium chloride solution. 1∼2 l of the concentrated solution of organic layer was applied to GC/MSD. The retention time of BP peak was 11.10 min. Recovery (%) of BP by ultrasonication from sediment and soil samples was 96.0∼100.6% and 40.0∼83.0%, respectively. Recovery of BP by liquid-liquid extraction was 51∼59% in soil samples. The detection limit of BP in sediment and soil samples were determined to 0.1 ng/g.

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Comparative Studies on Two Types Derivatives of Gibberellins for the Gibberellin Analysis by Gas Chromatography-Selected Ion Monitoring (GC-SIM에 의한 두종의 gibberellin유도체의 분석)

  • Park, Keun-Hyung
    • Applied Biological Chemistry
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    • v.28 no.2
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    • pp.82-87
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    • 1985
  • Aiming at the improvement of accuracy and sensitivity of gibberellin analysis by gas chromatography-selected ion monitoring (GC-SIM), the mass spectra of two types of 29 gibberellin derivatives, methyl ester-trimethylsilyl ethers and trimethylsilyl ester-trimethylsilyl ethers, were obtained and their advantages and disadvantages in GC-SIM analysis are discussed.

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Simultaneous Analysis of Semi-Volatile Organic Acid Priority Pollutants in Soil (토양 중의 비휘발성 산성 유기 Priority Pollutants 동시분석에 관한 연구)

  • Lee, Seung Seok;Park, Gyo Beom;Lee, Seong Geun
    • Journal of the Korean Chemical Society
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    • v.38 no.3
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    • pp.246-253
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    • 1994
  • The simultaneous analysis of 11 semi-volatile organic acid compound which are listed as priority pollutants by EPA, were performed by GC/MS-SIM(selected ion monitoring). Two extraction procedures, sonication extraction and Soxhlet extraction, were studied as an extraction and concentration method for priority pollutants in soil. Accurecy and precision of the methods were measured by the calculation of mean recovery, mean relative standard deviation, and method detection limit. Finally, limitations and prospects were discussed.

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Simultaneous Analysis of Semi-Volatile Organic Base/Neutral Priority Pollutants in Soil (토양 중의 비휘발성 염기/중성 유기 Priority Pollutants 동시 분석에 관한 연구)

  • Lee, Seung Seok;Park, Gyo Beom;Lee, Seok Geun
    • Journal of the Korean Chemical Society
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    • v.38 no.6
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    • pp.418-426
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    • 1994
  • This study was aimed at the detection of 40 semi-volatile organic base/neutral compounds from soil among 129 priority pollutants listed by EPA. Two extraction procedures, sonication extraction and Soxhlet extraction, were studied as a extraction and concentration method for priority pollutants in soil. Extracts were analyted by GC/MS-SIM(selected ion monitoring). The analytical methods were tested by standard compounds spiked into blank soil. Accuracy and precision of the methods were measured by calculation of mean recovery and mean relative standard deviation. And the method detection limits were estimated.

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Analysis of Ginsenosides by Thermospray LC/MS (열분무 LC/MS에 의한 인삼사포닌의 분석)

  • Park, Man-Ki;Park, Jeong-Hill;Hwang, Gwi-Seo;Lee, Mi-Young;Park, In-Jeong
    • Journal of Ginseng Research
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    • v.19 no.2
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    • pp.134-137
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    • 1995
  • Ginseng saponins were analyzed by thermospray (TSP) LCMS method using ODS column and with acetonitrile/ammonium acetate solution. Optimal condition for TSP Lchfs was found as follows: capillary temperature: 33$0^{\circ}C$ repelled voltage: 200 V, and concentration of ammonium acetate: 0. 05 M. Panaxadiol and panaxatriol type saponins showed characteristic fragment ions. The calibration curve of ginseng saponin showed good linearity with a correlation coefficient of 0.99. Detection limits using selected ion monitoring (SIM) technique were improved by 10~200 times compared to conventional HPLCnnr detection method.

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Enantioseparation of Flurbiprofen and Ketoprofen in Patches and in Urine Excretions by Achiral Gas Chromatography

  • Paik, Man-Jeong;Nguyen, Duc-Toan;Kim , Kyoung-Rae
    • Archives of Pharmacal Research
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    • v.27 no.12
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    • pp.1295-1301
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    • 2004
  • The enantiomeric composition tests on flurbiprofen and ketoprofen present in patch products and in urine excretions following patch applications were performed as diastereomeric (R)-(+)- 1-phenylethylamides by achiral gas chromatography and by gas chromatography-mass spectrometry in selected ion monitoring mode. The method for determination of (R)- and (S)-enantiomers in the range from 0.1 to 5.0 ${\mu}$g was linear (r ${\ge}$ 0.9996) with acceptable precision (% RSD ${\le}$5.2) and accuracy (% RE = 0.6 ~ -2.4). The enantiomeric compositions of flurbiprofen in one patch product and of ketoprofen in five different products were identified to be racemic with relatively good precision (${\le}$ 6.4%). The urinary excretion level of (R)-flurbiprofen was two times higher than its antipode, while the comparable excretion levels of (R)- and (S)-enantiomers for ketoprofen were observed.