• Title/Summary/Keyword: on-line trace enrichment

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On-line Trace Enrichment in High Performance Liquid Chromatography Using XAD-2 Precolumn for the Determination of Lonazolac in Human Plasma

  • Lee, Hye-Suk;Kim, Eun-Joo;Zee, Ok-Pyo;Lee, Yoon-Joong
    • Archives of Pharmacal Research
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    • v.12 no.2
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    • pp.108-113
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    • 1989
  • A new column-switching high performance liquid chromatographic method was developed for the determination of lonazolac in plasma. This method was based on the on-line trace enrichment of lonazolac using a precolumn packed with Amberlite XAD-2. The analysis was complete in 20 min. between injections and the limit of detection was $0.1{\mu}g/ml$ using $100{\mu}l$ of plasma. The method was linear in range of $0.1-10{\mu}g/ml$ with a correlation coefficient of 0.9991. Absolute recovery of lonazolac from the spiked plasma samples ranged from 95.6% to 97.1%. The method was shown to be reproducible over the concentration range studied.

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On-line SPE-HPLC Method using Alumina Filtering to Selectively Extract Phenolic Compounds from Environmental Water

  • Lee, Sung-Kwang
    • Bulletin of the Korean Chemical Society
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    • v.31 no.12
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    • pp.3755-3759
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    • 2010
  • A on-line SPE (solid phase extraction)-HPLC preconcentration method was developed for the determination of phenolic compounds at trace levels in environmental water sample. XAD-4 and Dowex 1-X8 were used as sorbent in the on-line SPE-HPLC method for the selective enrichment of nine phenolic compounds, which are included in the priority pollutants list of the US EPA. Also alumina prefiltering considerably reduced the amount of interfering peaks due to humic substances that could accumulated due to the preconcentration step and prevent quantification of polar phenolic compounds in environmental water samples. This method was used to determine the phenolic compounds in tap and river water and superiority to the US EPA 625 method in its enrichment factor, pretreatment time, recoveries, and detection limit. The limits of detection were in the range of $0.3-0.9\;{\mu}g/L$ in tap water sample.

Isotachophoretically Assisted On-Line Complexation of Trace Metal Ions in a Highly Saline Matrix for Capillary Electrophoresis

  • Kim, Ji-Hye;Choi, Ki-Hwan;Cho, Sun-Young;Riaz, Asif;Chung, Doo-Soo
    • Bulletin of the Korean Chemical Society
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    • v.33 no.3
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    • pp.790-794
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    • 2012
  • Trace metal ions such as $Cd^{2+}$, $Ni^{2+}$, and $Zn^{2+}$ in a highly saline sample were subjected to on-line complexation with 4-(2-thiazolylazo) resorcinol (TAR) dissolved in a background electrolyte (BGE) under transient isotachophoresis (TITP) conditions. A long plug of the saline sample, containing the trace metal ions but devoid of TAR, was injected into a coated capillary filled with a BGE composed of 150 mM 2-(cyclohexylamino) ethanesulfonic acid (CHES) and 110 mM triethylamine (TEA) at pH 9.7. Since the electrophoretic mobility of TAR fell between the mobilities of the anionic leading electrolyte ($Cl^-$ in the sample) and the anionic terminating background electrolyte ($CHES^-$), a highly concentrated zone of TAR from the BGE was formed at the rear of the sample matrix and then the metal cations toward the cathode were swept by isotachophoretically assisted on-line complexation (IAOC) between the metal ions and the isotachophoretically stacked TAR. As a result, anionic metal-TAR complexes were formed efficiently, which satisfy the TITP conditions between $Cl^-$ and $CHES^-$. The enrichment factors of metal ions including $Cd^{2+}$ were up to 780-fold compared to a conventional CZE mode using absorbance detection. The detection limits were 17 nM, 15 nM, and 27 nM for $Ni^{2+}$, $Zn^{2+}$, and $Cd^{2+}$ in a 250 mM NaCl matrix, respectively. Our method was successfully applied to the analysis of urine samples without desalting.

Optimization for the Solid-Phase Extraction of Trace Clobazam from Biological Samples (생체시료로부터 미량 크로바잠의 고상추출을 위한 최적화)

  • Kim, Kyoung-Rae;Kim, Jeong-Ho;Kim, Hyub;Yoon, Hye-Ran
    • YAKHAK HOEJI
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    • v.39 no.4
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    • pp.395-400
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    • 1995
  • The sorption and desorption properties of four adsorbents were evaluated for the trace enrichment of clobazam from biological samples. Graphitized carbon black(GCB) gaved the highest dynamic adsorption coefficient. Among the six organic solvents examined, acetone gave the highest desorption coefficient for the clobazam adsorbed on GCB. Using the GCB column, the optimum elution volume of the eluting solvent was evaluated from the on-line monitored breakthrough curve for clobazam. When GCB as the solid adsorbent and acetone as the eluting solvent were used for the solidphase extraction of clobazam from serum, the recoveries were higher than 83% with good reproducibility in the concentration range of 20-50 $\mu\textrm{g}$/ml.

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Quantitative Analysis of Cobalt with Continuous Flow Preconcentration Using 1-Nitroso-2-naphthol as an Organic Precipitant (1-Nitroso-2-naphthol 침전제를 사용한 연속흐름 선농축법에 의한 코발트의 정량분석)

  • Im, Kab Soo;Pak, Yong Nam
    • Journal of the Korean Chemical Society
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    • v.43 no.6
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    • pp.644-650
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    • 1999
  • Trace amount of cobalt in water samples was preconcentrated continuously with an organic precipitant and determined by flame atomic absorption spectrometry. The flow injection technique was used to preconcentrate cobalt by on-line direct precipitation with 1-nitroso-2-naphthol. The precipitation was dissolved with methyl isobutyl ketone (MlBK) and was sent to the flame. The optimum conditions for cobalt determination were determined and used to analyze Co samples. For 1.0 mL of sample, the enrichment factor was 13 and the sample throughput was about lO per hour for 0.5 ppm Co solution. The enrichment factor was increased to 68 fold for 10.0 mL. A semi-reference biologicaI sample was prepared and analyzed. The result was in good agreement with the expected value with RSD of 4%.

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On-line Trace Enrichment for the Determination of Insulin in Biological Samples Using Reversed-Phase High Performance Liquid Chromatography with Column Switching

  • Lee, Jung-Sook;Lee, Heeyong;Lee, Hye-Suk;Lee, Kang-Choon
    • Archives of Pharmacal Research
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    • v.17 no.5
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    • pp.360-363
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    • 1994
  • Column--swtiching technique with a reversed-phase high performance liquid chromatographic method has been developed for the routine analysis of radioiodinated insulin and its degadation products in biological fluids. The diluted biological samples were loaded onto a precolumn packed with LiChrosorb RP-8 $(25-40{\;}{\mu}m)$ using 0.1% trifuoroacetic acid (TFA) in water as a washing solvent. After valve switching, the concentrated insulins were eluted in the back-flush mode and separated by a W-Porex $C_{18}$ column with a gradient of 0.1% TFA in water and 0.1% TFA in acetonitrile as the mobile phase. The method showed good precision, accuracy and speed with the detection limit of 20 pg/ml. Total analysis time per sample was about 40 min and the coefficients of variation were less than 8, 2%.

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Characteristic Assessment of Heavy Metals in Dusts Collected by the Air Filtration System at Subway Stations in Daegu, Korea (대구지역 지하철역사 공기여과필터 포집먼지에 함유된 중금속성분의 특성평가)

  • Do, Hwa-Seok;Song, Hee-Bong;Shin, Dong-Chan;Kwak, Jin-Hee;Lee, Myoung-Sook;Yoon, Ho-Suk;Kang, Hye-Jung;Phee, Young-Gyu
    • Journal of Korean Society of Environmental Engineers
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    • v.31 no.1
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    • pp.42-50
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    • 2009
  • Samples of subway dust were collected by the air filter system of 30 subway stations on Daegu subway line 1 in January 2008. Samples were sieved below 100 ${\mu}m$, and 14 elements were analyzed using ICP after acid extraction. Results obtained from the source assessment of trace elements using enrichment factor showed that Ca, Fe, K, Mg, Mn, Na, V were influenced by natural sources such as weathered rock and resuspended soil, while Cd, Cr, Cu, Ni, Pb and Zn were influenced by anthropogenic sources such as fuel combustion and waste incineration. Concentrations were remarkably higher in components from natural sources than in components from anthropogenic sources. Anthropogenic sources were significantly affected by indoor dusts than outdoor dusts. Results of pollution indices of heavy metals indicated that indoor dusts were more contaminated with heavy metal ions than outdoor dusts. The correlation analysis among trace elements indicated that components were much correlated in the order of natural sources-anthropogenic sources, anthropogenic sources-anthropogenic sources, natural sources-natural sources in both indoor and outdoor dusts. Trace element components of outdoor dusts were largely correlated than those of indoor dusts. In addition, indoor dusts were significantly affected by outdoor dusts rather than depth from the surface or the average daily number of subway passengers.