• Title/Summary/Keyword: Mobile-lP

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Preconcentration and Speciation of Trace Mercury Compounds in Water Sample Using Dithizonates Extraction and Reverse Phase Liquid Chromatography (디티존 착물 추출과 역상 액체 크로마토그래피를 이용한 물시료 중의 미량 수은 화합물의 농축 및 화학종의 분리)

  • Suh, Jung-Ki;Cho, Kyung-Haeng;Lee, Sang-Haak
    • Analytical Science and Technology
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    • v.13 no.1
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    • pp.81-88
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    • 2000
  • A rapid preconcentration method was developed for the speciation of the trace mercury compounds in water sample. The mercury compounds were extracted and preconcentrated simply as their dithizone complexes by passing through the dithizone impregnated ultra-high molecular weight polyethylene (UHMWPE) membrane solvent inlet filter following sanification in methanol solvent. The concentrated dithizonates were separated by liquid chromatography on a $C_{18}$ column. Complete resolution was obtained between methyl-, ethyl-, phenyl-, and inorganic mercury with a mobile phase of 0.05 M acetate buffer (pH=4)/THF/methanol(3:5:2). The separnted mercury chelates were detected by spectrophotometrically at 475 nm. The proposed method was successfully applied to the speciation of mercury compounds in waste water with detection limit at the subnanogram/mL level.

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Retrieval and Validation of Precipitable Water Vapor using GPS Datasets of Mobile Observation Vehicle on the Eastern Coast of Korea

  • Kim, Yoo-Jun;Kim, Seon-Jeong;Kim, Geon-Tae;Choi, Byoung-Choel;Shim, Jae-Kwan;Kim, Byung-Gon
    • Korean Journal of Remote Sensing
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    • v.32 no.4
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    • pp.365-382
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    • 2016
  • The results from the Global Positioning System (GPS) measurements of the Mobile Observation Vehicle (MOVE) on the eastern coast of Korea have been compared with REFerence (REF) values from the fixed GPS sites to assess the performance of Precipitable Water Vapor (PWV) retrievals in a kinematic environment. MOVE-PWV retrievals had comparatively similar trends and fairly good agreements with REF-PWV with a Root-Mean-Square Error (RMSE) of 7.4 mm and $R^2$ of 0.61, indicating statistical significance with a p-value of 0.01. PWV retrievals from the June cases showed better agreement than those of the other month cases, with a mean bias of 2.1 mm and RMSE of 3.8 mm. We further investigated the relationships of the determinant factors of GPS signals with the PWV retrievals for detailed error analysis. As a result, both MultiPath (MP) errors of L1 and L2 pseudo-range had the best indices for the June cases, 0.75-0.99 m. We also found that both Position Dilution Of Precision (PDOP) and Signal to Noise Ratio (SNR) values in the June cases were better than those in other cases. That is, the analytical results of the key factors such as MP errors, PDOP, and SNR that can affect GPS signals should be considered for obtaining more stable performance. The data of MOVE can be used to provide water vapor information with high spatial and temporal resolutions in the case of dramatic changes of severe weather such as those frequently occurring in the Korean Peninsula.

A Study on Optimization for Separation of Phenols and Preconcentration-Separation of Trace Phenols in Reversed-Phase Liquid Chromatography (역상 액체 크로마토그래피에서 페놀류의 분리 최적화 및 미량 페놀류의 농축-분리에 관한 연구)

  • Lee Dai Woon;Lee Sung Won;So, Min Jeong;Cho Byung Yun
    • Journal of the Korean Chemical Society
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    • v.37 no.5
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    • pp.513-522
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    • 1993
  • The purpose of this study is to optimize the selectivity of mobile phase solvents for separation of 25 phenols in reversed phase liquid chromatography and to accomplish the simultaneous preconcentration and separation of trace phenols from water samples. Phenols used in this study were classified into three groups, chloro-, methyl-, and nitrophenols. Quaternary solvent mobile phases were employed to improve the selectivity. Overlapping resolution maps(ORM) as a statistical simplex techniques was used to predict the optimum solvent system. Additional criterion such as pH and temperature were also investigated. In order to improve the resolution and decrease the analysis time, isoselective multisolvent gradient elution system was employed with ORM-Prism method. The simultaneous preconcentration and separation of trace phenols from water samples were performed by using XAD-2/Dowex 1-X8 tandem column. When the extraction efficiency was evaluated by sampling up to 1 L of distilled water, recovery of the phenols, except phenol, was above 90% and the limit of detection of the phenols was 5 ppb. The XAD-2/Dowex 1-X8 method was superior to C18 cartridge in terms of recovery and selectivity.

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Separation Characteristics of Mandelic Acid in Kromasil HPLC Column (Kromasil HPLC 칼럼에서 Mandelic Acid의 분리특성)

  • Kim, Byung Lip;Kim, Jong Min;Kim, Woo Sik;Kim, In Ho
    • Korean Chemical Engineering Research
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    • v.46 no.4
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    • pp.681-685
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    • 2008
  • Chiral separation of racemic mandelic acid was achieved on a Kromasil KR100-5CHI-TBB column. Some chromatographic parameters (resolution, number of theoretical plates, capacity factor) are calculated under different separation conditions such as changes of mobile phase compositions (hexane/t-BME = 85/15 - 10/90) as well as formic acid concentrations for adjusting pH (0.1, 0.5, 1.0 v/v%). Flow rate versus number of theoretical plates was compared to evaluate column efficiency. To determine the adsorption isotherms, PIM (Pulse Input Method) was carried out. At the concentrations of racemic mandelic acid between 0.1 and 0.3 mg/ml, L- and D-mandelic acids have the same retention times of 8.8 and 9.4 min respectively. Mandelic acid isotherms show a linear form under the concentrations of 0.3 mg/ml with eluent (hexane/t-BME = 75/25). As the concentrations of mandelic acids increase, nonlinear Langmuir isotherms were observed as $C_{S,L}=3.358C_{M,L}/(1+0.0897C_{M,L})$ for L-mandelic acid and, $C_{S,D}=3.692C_{M,D}/(1+0.1457C_{M,D})$ for D-mandelic acid.

Validation of a Simple HPLC Method for Determination of Nicardipine in Human Plasma and Its Application to Single-dose Pharmacokinetics (인체 혈장 중 니카르디핀의 정량을 위한 HPLC 분석법 검증 및 단일 용량 투여에 의한 약물동태 연구)

  • Im, Ho-Taek;Cho, Sung-Hee;Lee, Heon-Woo;Park, Wan-Su;Rew, Jae-Hwan;Choi, Young-Wook;Yong, Chul-Soon;Lee, Kyung-Tae
    • Journal of Pharmaceutical Investigation
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    • v.35 no.6
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    • pp.461-465
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    • 2005
  • A simple HPLC method with ultraviolet detection of nicardipine in human plasma was developed and validated. After drug extraction with solid phase extraction (SPE) method, chromatographic separation of nicardipine in plasma was achieved at $30^{\circ}C$ with a $C_{18}$ column and acetonitrile-0.02% phosphate buffer mixture (with 0.02% triethylamine, final pH 7.0), as mobile phase. Quantitative determination was performed by ultraviolet detection at 254 nm. The method was specific and validated with a limit of quantification of 5 ng/mL. The intra- and inter-day precision and accuracy were acceptable for all quality control samples including the lower limit of quantification. The applicability of the method was demonstrated by analysis of plasma after oral administration of a single 40 mg dose to 8 healthy subjects. From the plasma nicardipine concentration versus time curves, the mean $AUC_{t}$, was $134.04{\pm}59.72\;ng\;hr/mL$ and $C_{max}$ of $108.65{\pm}69.17\;ng/mL$ reached 1.5 hr after administration. The mean biological half-life of nicardipine was $3.93{\pm}0.82\;hr$. Based on the results, this simple and validated assay method could readily be used in any pharmacokinetic or bioequivalence studies using human.

Analysis of Related Compounds from Commercial Atenolol Raw Materials and Preparations by High-Performance Liquid Chromatography (HPLC를 이용한 시판 아테놀롤 원료 및 제품 중 유연물질의 분석)

  • Dong, Nguyen Thanh;Kang, Ji-Youn;Jung, Young-Hee;Lim, Eun-Hee;Hwang, Gwi-Seo;Kang, Chan-Soon;Kim, Eun-Jung;Kang, Jong-Seong
    • Journal of Pharmaceutical Investigation
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    • v.34 no.6
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    • pp.453-457
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    • 2004
  • Atenolol and related compounds found in raw materials and commercial products were analyzed by reversed-phase high-performance liquid chromatography. A mixed solution of phosphate buffer (3.4 g/l, pH 3.0), tetrahydrofurane and methanol (800:20:180, v/v/v) including sodium octanesulfonate (1 g/l) and tetrabutylammonium-hydrogensulfate (0.4 g/l) was used as mobile phase at the flow rate of 0.25 ml/min. Detection was carried out at UV 226 nm. Atenolol related compounds, such as bis ether, tertiary amine and blocker acid were identified by comparing the retention time of the standard. The within-day and between-day precisions of the separated compounds were less than 1.2% and 3.4%, respectively. The contents of related compounds of the tested samples were under the limit prescribed in the European Pharmacopoeia. The pattern of the related compounds showed that atenolol raw materials and products could be classified in three different groups, indicating that the materials originated from different source or treated in different way.

Development of Method for Analysis of Four Sulfonylurea Pesticides, Rimsulfuron, Ethametsulfuron-methyl, Tribenuron-methyl, Chlorimuron-ethyl Residues by High-Performance Liquid Chromatography with Diode-Array Detection (HPLC/DAD를 이용한 림술푸론, 에타메트설푸론메틸, 트리베누론메칠, 클로리무론에칠 4종 성분의 잔류농약 분석법 개발)

  • Koo, Yun-Chang;Yang, Sung-Yong;Wang, Zeng;An, Eun-Mi;Heo, Kyoung;Kim, Hyeng-Kook;Shin, Han-Seung;Lee, Jin-Won;Lee, Kwang-Won
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.39 no.8
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    • pp.1231-1235
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    • 2010
  • The method for residue analysis of four sulfonylurea pesticides, rimsulfuron, ethametsulfuron-methyl, tribenuron-methyl and chlorimuron-ethyl was examined and analyzed by HPLC with ODS column ($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$ diameter particle size) which was maintained at $35^{\circ}C$. Mobile phase consisted of solvent A (20 mM $KH_2PO_4$, pH 2.5) and solvent B (acetonitrile). Isocratic elution of the column with 45% solvent A and 55% solvent B at a flow rate of 1 mL/min resulted in retention times of 5.92, 6.54, 9.28, and 14.35 min for rimsulfuron, ethametsulfuron-methyl, tribenuron-methyl, and chlorimuron-ethyl, respectively. All injection volumes were $20\;{\mu}L$. The limit of quantitation was 0.02, 0.01, 0.001, and 0.004 mg/kg for rimsulfuron, ethametsulfuron-methyl, tribenuron-methyl, and chlorimuron-ethyl, respectively. Recovery rate test was performed with three farm products, rice, apple and soybean. Four sulfonylurea pesticides were spiked at concentrations of 0.05, 0.1 and 0.5 mg/kg. The recovery rates were ranged from 86.12% to 116.26% and the standard deviations of all experiments were within 10%.

Quantification of Entacapone in Human Plasma by HPLC Coupled to ESI-MS/MS Detection: Application to Bioequavalence Study (체외에서 ESI-MS/MS 탐지에 연결된 HPLC에 의한 Entacapon의 수량화: 생물학적 동등성 연구에 적용)

  • Balasekhara Reddy., Ch.;Baburao., Ch.;Chandrasekhar., K.B.;Kanchanamala., K.;RihanaParveen., S.K.;Ravikumar., Konda
    • Journal of the Korean Chemical Society
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    • v.54 no.5
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    • pp.523-532
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    • 2010
  • The proposed method is simple, sensitive and specific Liquid chromatography-tandem mass spectrometry (LCESI-MS/MS) method for the quantification of Entacapone (EA) in human plasma using Entacapone-d10 (EAD10) as an internal standard (IS). Chromatographic separation was performed on Zorbax SB-C18, $2.1{\times}50\;mm$, $5\;{\mu}m$ column, mobile phase composed of 10 mM Ammonium formate (pH 3.0): Acetonitrile (60:40 v/v), with a flow-rate of 0.7 mL/min, followed by Liquid-liquid extraction. EA and EAD10 were detected with proton adducts at m/z $306.1{\rightarrow}233.1$ and $316.3{\rightarrow}233.0$ in multiple reaction monitoring (MRM) positive mode respectively. The method was validated over a linear concentration range of 1.00 - 2000.00 ng/mL with correlation coefficient ($r^2$) $\geq$ 0.9993. Intra and inter-day Precision within 3.60 to 7.30 and 4.20 to 5.50% and Accuracy within 97.30 to 104.20 and 98.30 to 105.80% proved for EA. This method is successfully applied in the bioequivalence study of healthy Indian human volunteers.

Inverse HPLC approach for the evaluation of repulsive interaction between ionic solutes and a membrane polymer

  • Kiso, Yoshiaki;Kamimoto, Yuki;Hosogi, Katsuya;Jung, Yong-Jun
    • Membrane and Water Treatment
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    • v.6 no.2
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    • pp.127-139
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    • 2015
  • Rejection of ionic solutes by reverse osmosis (RO) and nanofiltration (NF) membranes is controlled mainly by electrochemical interaction as well as pore size, but it is very difficult to directly evaluate such electrochemical interaction. In this work, we used an inverse HPLC method to investigate the interaction between ionic solutes and poly (m- phenylenediaminetrimesoyl) (PPT), a polymer similar to the skin layer of polyamide RO and NF membranes. Silica gel particles coated with PPT were used as the stationary phase, and aqueous solutions of the ionic solutes were used as the mobile phase. Chromatographs obtained for the ionic solutes showed features typical of exclusion chromatographs: the ionic solutes were eluted faster than water (mobile phase), and the exclusion intensity of the ionic solute decreased with increasing solute concentration, asymptotically approaching a minimum value. The charge density of PPT was estimated to be ca. 0.007 mol/L. On the basis of minimum exclusion intensity, the exclusion distances between a salt and neutralized PPT was examined, and the following average values were obtained: 0.49 nm for 1:1 salts, 0.57 nm for 2:1 salts, 0.60 nm for 1:2 salts, and 0.66 nm for 2:2 salts. However, $NaAsO_2$ and $H_3BO_3$, which are dissolved at neutral pH in their undissociated forms, were not excluded.

Characteristics of Source and Concentration of VOCs in Daegu (대구지역 대기 중 VOCs 농도 및 발생원 특성)

  • Gu Min-Jung;Choi Sung-Woo
    • Journal of Environmental Science International
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    • v.14 no.6
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    • pp.543-553
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    • 2005
  • In recent days, photochemical smog due to the rapid industry development and vehicle increasement has become a critical pollutant in the metropolitan area and the number of ozone alarm signal has increased every year. This research was performed to evaluate VOCs emission source characteristics and concentration of VOCs in Daegu. The site average concentration was observed in the following order: industrial area > commercial area > residential area. Most of the VOCs species except toluene showed variations with higher concentration during nighttime, and lower concentration during the daytime. The major VOCs of stationary emission source were BTEX(benzene, toluene, ethylbenzene. xylene) and methylene chloride, trichloroethene and styrene. Also, those of automobile exhaust were toluene and benzene. Also, the major VOCs concentration emited by the vehicle fuel was observed in the following order: gasoline > light oil > liquefied petroleum gas (L.P.G). Correlation coefficients values were estimated between major VOCs such as toluene, ethylbenzene, m,p-xylene, o-xylene. Results showed that correlation coefficient values were significant magnitude above 0.76. Also, there showed highly significant correlations among ethyl benzene, m,p-xylene, and o-xylene concentration(Pearson correlation coefficients, r=0.868-0.982). Calculated correlation coefficients among commercial area,industrial area and residential area were 0.934-0.981, they showed high correlation. There showed highly correlation between stationary emission source and industrial area, compared with commercial area and residential area. Also, calculated correlation coefficients among commercial area, industrial area, residential area and automobile exhaust were 0.732, 0.725, 0.777, respectively.