• Archives of Pharmacal Research
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• 제12권2호
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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.

• Bulletin of the Korean Chemical Society
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• 제31권12호
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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.

• Bulletin of the Korean Chemical Society
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• 제33권3호
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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.

• 약학회지
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• 제39권4호
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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.

• 대한화학회지
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• 제43권6호
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• pp.644-650
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• 1999

본연구에서 유기 침전제를 사용하여 수용액중의 코발트를 on-line으로 연속 침전시켜 선농축하는 방법을 연구하였다. 침전제로 1-nitroso-2-naphthol을 사용하여 라인내에서 직접 침전시킨 뒤 MlBK(Methyl lsobutyl Ketone)로 용해시켜 불꽃 원자흡수 분광기로 보내어 분석하였다. 최적조건을 구하고 농축배율을 연구한 결과 대개 0.5 ppm의 코발트 시료 1.0 mL를 사용하였을 때 13배의 농축율을 얻었으며 시료 처리 속도는 시간당 I0개 정도 이었다. 부피를 10.0 mL로 증가시키면 시료의 처리속도는 늦어지지만 농축비를 68배로 높일 수 있었다. 본 연구의 정확성을 알기 위해 합성된 준 표준 생체시료를 분석한 결과 4%의 상대 표준편차를 가지고 예상치에 근접하는 좋은 결과를 얻을 수 있었다.

• Archives of Pharmacal Research
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• 제17권5호
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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%.

• 대한환경공학회지
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• 제31권1호
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• pp.42-50
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• 2009

2008년 1월에 대구지하철 1호선 총 30개 역사에 대해 각 역사별로 공기여과장치에서 포집된 먼지를 채취하여 100 ${\mu}m$ 이하로 체거름하고 산추출한 후 ICP로 14개 원소를 분석하였다. 농축계수를 이용한 미량원소성분의 발생원을 평가한 결과, Ca, Fe, K, Mg, Mn, Na, V 성분은 암석풍화, 토양재비산 등과 관련된 자연적인 발생원의 영향을 받았고, Cd, Cr, Cu, Ni, Pb, Zn 성분은 연료연소, 폐기물소각 등과 관련된 인위적인 발생원의 영향을 받고 있는 것으로 추정되었다. 미량원소성분의 농도는 자연적인 발생원에서 유래되는 성분이 높았고, 인위적인 발생원에서 유래되는 성분이 낮았다. 인위적인 발생원 성분의 기여도는 실내먼지가 실외먼지에 비해 높았다. 오염지수를 이용한 중금속성분의 오염도를 평가한 결과, 실내먼지는 실외먼지에 비해 중금속으로부터 오염된 것으로 추정되었다. 미량원소성분의 상관성을 분석한 결과, 실내와 실외먼지에서 공통적으로 자연적-인위적발생원 성분간, 인위적-인위적발생원 성분간, 자연적-자연적발생원 성분간의 순으로 유의하게 양호하였다. 그리고 실외먼지는 실내먼지에 비해 미량원소성분간의 유의한 상관성이 많았다. 또한 지하깊이, 이용객수, 실외먼지 등이 실내먼지의 성분에 미치는 영향을 분석한 결과, 실내먼지는 지하깊이나 이용객수의 영향보다는 실외먼지의 직접적인 영향을 많이 받고 있는 것으로 추정되었다.