• Bulletin of the Korean Chemical Society
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• 제25권6호
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• pp.900-906
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• 2004

An RPLC-postcolumn detection method has been developed for the fluorimetric determination of dichloroacetamide (DCAD) in water. After ammonia and DCAD were separated on a $C_{18}$ nonpolar stationary phase with 2.5% methanol-0.02 M phosphate buffer at pH 3, the column eluant was reacted with post column reagents, o-phthaldialdehyde (OPA) and sulfite ion at pH 11.5, to produce a highly fluorescent isoindole fluorophore, which was measured with a fluorescence detector ( ${\lambda}_{ex}$ = 363 nm, ${\lambda}_{em}$ = 425 nm). With the optimized conditions for RPLC and the postcolumn derivatization, the calibration curve was found to be linear in the concentration ranges of 0.5 and 20 ${\mu}$M for DCAD, and the detection limit for DCAD was 0.18 ${\mu}$M (23${\mu}$g/L). This corresponded to 18 pmol per 100 ${\mu}$L injection volume for a signal-to-noise ratio of 3, and the repeatability and reproducibility of this method were 1.0% and 2.5% for five replicate analyzes of 2 ${\mu}$M DCAD, respectively. The degradation yields DCAD to ammonia were 94 and 99%, and the percent recoveries of DCAD from 4 and 6 ${\mu}$M DCAD-spiked tap water were shown mean more than 97%.

• Bulletin of the Korean Chemical Society
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• 제32권10호
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• pp.3603-3609
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• 2011

A novel sampling method of the headspace poly(dimethylsiloxane) (PDMS) mini-disk extraction (HS-PDE) was developed, optimized, validated and applied for the GC/MS analysis of spices flavors. A prototype PDMS mini-disk (8 mm outer diameter, 0.157 mm thickness, 9.4 mg weight) has been designed and fabricated as a sorption device. The technique uses a small PDMS mini-disk and very small volume of organic solvent and less sample size than the solvent extraction. This new HS-PDE method is very simple to use, inexpensive, rapid, requires less labor. Linearities of calibration curves for ${\alpha}$-pinene, ${\beta}$-pinene, limonene and ${\gamma}$-terpinene by HS-PDE combined with GC/MS were excellent having $r^2$ values greater than 0.99 at the dynamic range of 6.06~3500 ng/mL. The limit of detection (LOD) and the limit of quantitation (LOQ) showed very low values. This method exhibited good precision and accuracy. The overall extraction efficiency of this method was evaluated by using partition coefficients ($K_p$) and concentration factors (CF) for several characteristic components from nutmeg and mace. Partition coefficients were in the range from $2.04{\times}10^4$ to $4.42{\times}10^5$, while CF values were 0.88-15.03. HS-PDE was applied successfully for the analysis of flavors compositions from nutmeg, mace and cumin. The HS-PDE method is a very promising sampling technique for the characterization of volatile flavors.

• Bulletin of the Korean Chemical Society
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• 제25권1호
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• pp.79-84
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• 2004

The existing technological schemes for processing rhenium-containing raw materials involve the recovery of Re from solutions, which can be effectively achieved by anion exchange method. The application of anion exchange also allows to study rhenium state in aqueous solutions and to develop analytical control methods. The present work is focused on investigation of ion exchange equilibrium in the analytical system Re(VII)-HCl-$SnCl_2$-KSCN-anion exchanger by means of sorption-desorption method as well as by electron, IR- and diffuse reflection spectroscopy. It was shown that rhenium can be quantitatively recovered from this system. It is proposed to use the sorption-spectroscopic method for Re(VII) determination in aqueous solutions. The calibration curve is linear in the concentration range of 0.5-20.0 mg/L (sample volume is 25.0 mL) and the detection limit is 0.05 mg/L. The presence of Mo(VI), Cu(II), Fe(II, III), Ni(II), Zn(II) as well as $K^+,\;Na^+$ do not hinder the solid-phase determination of rhenium. Rhenium (VII) determination by diffuse reflection spectroscopy was carried out in model solutions as well as in samples of river-derived water and in solutions obtained after the dissolution of spent catalysts.

• 대한화학회지
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• 제37권3호
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• pp.309-316
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• 1993

전도도법을 이용하여 물과 에탄올 혼합 용매에서 LiCl, NaCl, KCl 및 KBr의 한계 당량전도도를 측정한 후, TATB법을 이용하여 염을 구성하는 이온들의 한계 당량전도도를 구했다. 이온의 한계 당량전도도와 혼합 용매의 점성도의 항으로 이루어진 식을 사용하여 이온의 Stokes 반지름을 얻었으며, Nightgale법을 사용하여 이온의 보정반지름을얻었다. 또한 이온의 보정 반지름과 결정 반지름으로 부터 이온에 용매화된 용매의 부피를 구하고, 간단한 가정을 이용하여 이온의 여러가지 용매화수를 얻었다. 이들 중에서 가장 타당한 용매화수 (h$_{H_2O}$ ＋ h$_0$)를 구하고, 등용매화점으로부터 물과 메탄올 혼합 중에서 메탄올의 조성이 바뀜에 따라 이온에 선택적 용매화를 하는 용매를 알았다.

• 대한의용생체공학회:학술대회논문집
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• 대한의용생체공학회 1996년도 춘계학술대회
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• pp.22-26
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• 1996

In this paper, we designed 4-channel electrolyte analyzer that can measure simultaneousely the 4 electrolytes - pH, $pNa^{+}$, $pCa^{2+}$, and $pK^{+}-$ using 2-point calibration and implemented it. Developed electrolyte analyzer consists of singal processing part, actuator part and control unit for sample flow system. To implement reliable instrument, design considerations are emphasized on flow system and sample chamber that requires small sample volume and prevent air contact with sample solution. In addition to the hardware design, we developed system software which controls full measuring process. After system developed, we verified the system performance by the test measurement for pH, $pNa^{+}$, $pCa^{2+}$, and $pK^{+}$ value.

• Nuclear Engineering and Technology
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• 제25권4호
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• pp.548-551
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• 1993

원자력 산업의 변환공정에서 발생하는 폐수용액중의 우라늄 농도를 레이저 유발형광법을 사용하여 쉽게 측정할 수 있는 새로운 분석방법을 개발하였다. 실험 결과 시료의 약 10배 이상의 부피로 4M-인산용액을 첨가함으로써 효율적으로 형광 quencher의 영향을 배제시킬 수 있었으며, 폐액 시료에서의 우라늄 농도 3.0$\times$$10^{-6}$－6.0$\times$$10^{-5}$ M U $O_2$$^{2＋}$의 범위에서 농도에 대한 형광강도의 직선성이 우수하였다.

• Mass Spectrometry Letters
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• 제10권3호
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• pp.88-92
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• 2019

A sensitive analytical method of rhodanthpyrone A in rat plasma was developed using a liquid chromatography-tandem mass spectrometry (LC-MS/MS). Rhodanthpyrone A and rhodanthpyrone B (internal standard) in rat plasma were extracted by a liquid-liquid extraction method with ethyl acetate. This extraction method gave results in high and reproducible extraction recovery in the range of 73.75-79.90% with no interfering peaks around the peak elution time of rhodanthpyrone A and B. The standard calibration curves for rhodanthpyrone A ranged from 0.5 to 2000 ng/mL were linear with $r^2$ > 0.994 and the inter- and intra-day accuracy and precision and the stability were within acceptance criteria. Using this validated analytical method, pharmacokinetics of rhodanthpyrone A following intravenous and oral administration of rhodanthpyrone A at doses of 2 mg/kg and 30 mg/kg, respectively, were investigated. Rhodanthpyrone A in rat plasma showed multi-exponential elimination pattern with high clearance and volume of distribution values. The absolute oral bioavailability of this compound was calculated as 3.7%. Collectively, the newly developed sensitive LC-MS/MS analytical method of rhodanthpyrone A could be successfully applied to investigate the pharmacokinetic properties of this compound and would be useful for the further studies on the efficacy, toxicity, and biopharmaceutics of rhodanthpyrone A.

• 약학회지
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• 제58권3호
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• pp.158-164
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• 2014

Dangguisu-san is a well-known traditional Korean herbal medicine prescription and has been widely used to treat ecchymosis, blood stagnation, and pain resulting from physical shock in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometer method was established for the simultaneous determination of the 17 biomarker components in Dangguisu-san. All analytes were separated on an UPLC BEH $C_{18}$ ($100{\times}2.1$ mm, $1.7{\mu}m$) column and maintained at $45^{\circ}C$. The mobile phase consisted of two solvent systems, 0.1% (v/v) formic acid in water (A) and acetonitrile (B) by gradient flow. The injection volume was $2.0{\mu}l$ and the flow rate was 0.3 ml/min with detection at mass spectrometer. Calibration curves of the 17 biomarker components were acquired with $r^2$ values ${\geq}0.9951$. The values of limit of detection and quantification of all analytes were 0.02~6.32 ng/ml and 0.05~18.95 ng/ml, respectively. The amounts of the 17 components in Dangguisu-san sample were $3.17{\sim}13,224.50{\mu}g/g$.

• 분석과학
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• 제35권2호
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• pp.60-68
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• 2022

In this study, we developed and validated a sensitive analytical method to quantify baphicacanthin A in mouse plasma using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The standard calibration curves for baphicacanthin A ranged from 0.5 to 200 ng/mL and were linear, with an r² of 0.985. The inter- and intra-day accuracy and precision and the stability fell within the acceptance criteria. Besides, we investigated the pharmacokinetics of baphicacanthin A following its intravenous (5 mg/kg) and oral administration (30 mg/kg). Intravenously injected baphicacanthin A showed biphasic elimination kinetics with high clearance and volume of distribution values. Furthermore, baphicacanthin A showed a rapid absorption but low aqueous solubility (182.51±0.20 mg/mL), resulting in low plasma concentrations and low oral bioavailability (2.49 %). Thus, we successfully documented the pharmacokinetic properties of baphicacanthin A using this newly developed sensitive LC-MS/MS quantification method, which could be used in future lead optimization and biopharmaceutic studies.

• 한국해안·해양공학회논문집
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• 제24권4호
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• pp.257-268
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• 2012

경기만과 한강하구를 유기적으로 연결한 고해상도 격자시스템의 EFDC수치모델을 이용하여 한강하구 수로별 순 수송량을 연구하였다. 수치모델의 모의기간은 2009년 5월부터 8월까지 총 124일 동안 모의하였으며, 담수 유입량은 모의 기간 동안 실제 한강과 임진강의 담수량을 입력자료로 사용하였다. 수치모델 결과는 관측된 조석 조화상수를 이용하여 보정 작업을 수행하였고 조류 관측자료를 이용하여 검증하였다. 강화 북쪽수로와 염하수로에서 평수기 담수량이 유입되는 30일 동안의 순 수송량을 계산하면, 염하수로와 강화 북쪽수로를 통해서 경기만으로 유출되는 수송량은 56:44의 비율로 나타났다. 평수기 30일 동안에 염하수로로 유입된 순 수송량의 방향은 세어도 인근 지역까지 하류 방향이고, 인천항 전면과 영종대교 인근 지역의 순 수송량은 상류 방향으로 나타났다. 영종대교 인근 해역에서 하류와 상류 방향에서 유입된 순 수송량의 수렴대가 형성되고 강화도와 영종도 사이의 수로를 통해서 서쪽으로 유출된다. 염하수로의 대 소조기 변동에 따른 순 수송량의 변화를 비교하기 위하여, 대 소조기 각 4 조석주기 동안의 결과를 분석하였다. 외해에서 유입되는 순 수송량과 하구 상류에서 유출되는 순 수송량의 수렴대 위치가 대 소조기 변동에 따라서 상류 또는 하류로 이동되며, 서쪽으로 유출되는 위치가 다르게 나타난다. 대조기에 비하여 소조기 때 수렴대의 위치가 상류 방향으로 이동되는 이유는 1)대조기 때 수위의 증가에 의한 강화도와 영종도 사이의 수로를 통한 유출량 증가, 2)대조기 때 상류와 하류의 해수면 차이에 의한 하류 방향으로 순압력 증가, 3)소조기 때 혼합 작용의 감소에 의한 주 수로의 상류 방향으로의 경압력 증가라고 판단된다.