• Title/Summary/Keyword: reversed phase

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Studies on the Elution Behavior and the Simultaneous Analysis of Some Metal-Dithiocarbamate Chelates by Reversed-Phase High Performance Liquid Chromatography (역상 액체 크로마토그래피에 의한 몇가지 금속-Dithiocarbamate 킬레이트의 용리거동 및 동시분석에 관한 연구)

  • Dai Woon Lee;Yun Je Kim;Hyun Chul Kim;Won Lee
    • Journal of the Korean Chemical Society
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    • v.32 no.3
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    • pp.211-226
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    • 1988
  • Liquid chromatographic behavior of several metal ions in dithiocarbamate(DTC) chelates were investigated by reversed phase high performance liquid chromatography on Novapak $C_{18}$ and ${\mu}$-Bondapak $C_{18}$ columns. The optimum conditions for the separation of DTC-metal chelate were examined with respect to the pH, shaking time, flow rate, extraction solvent, and mobile phase strength. The metal ions in mixtures at trace level, chelated with some dithiocarbamate derivatives were separated successfully on Novapak $C_{18}$ column using acetonitrile/methanol/water or acetonitril/water mixtures as mobile phases. It was found that all DTC metal chelates studied were eluted in an acceptable range of capacity factor values ($0{\leqq}log\;k'{\leqq}1$). Although several foreign metal ions were coexisted, high recovery and good precision were attained ; 97.0-106.7 % for the recovery and 0.98-3.41% for the coefficient of variation. Under the optimum analytical conditions, trace metal ions in the composite water samples were determined sucessfully with in relative error of about {\pm}$6.7 %.

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Reversed-Phase Ion-Pair High Performance Liquid Chromatographic Elution Behavior of Noble Metal-Thiacrown Ether Complexes (귀금속-티아크라운에테르 착물들의 역상 이온쌍 고성능 액체크로마토그래피 용리거동)

  • Chung, Yong Soon;Kim, Dong Won;Lee, Kang Woo;Kim, Chang Seok
    • Journal of the Korean Chemical Society
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    • v.42 no.4
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    • pp.416-421
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    • 1998
  • In the reversed-phase ion-pair high performance liquid chromatographic (RPIP-HPLC) elution behavior of noble metal-thiacrown ether complexes, the effects of the concentration of ion-pairing reagent and kind of ligands were studied. It was found that the less the number of atoms in the ring of the thiacrown ether molecule was, the larger the selectivity was, and the elution mechanism of the complexes was explained due to the formation of ion-pair when the concentration of sodium dodecyl sulfate (SDS) in mobile phase was lower than 10 mM and due to the formation of micelle when the SDS concentration was higher than 10 mM. As a conclusion, separations of the noble metal-thiacrown ether complexes in an optimum separation condition were accomplished successfully and the method was proved to be an useful one for the separation and determination of Ag (Ⅰ) ion in a black-white photographic fixing solution.

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Development of Gradient Centrifugal Partition Chromatography Method and Its Application for the Isolation of 3,5-Dimethoxyphenanthrene-2,7-diol and Batatasin-I from Dioscorea opposita

  • Yoon, Kee-Dong;Yang, Min-Hye;Chin, Young-Won;Kim, Yoen-Jun;Kim, Hye-Ryung;Choi, Ki-Ri;Park, Ju-Hyun;Kim, Jin-Woong
    • Natural Product Sciences
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    • v.15 no.3
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    • pp.144-150
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    • 2009
  • Gradient centrifugal partition chromatography (GCPC) method was developed and applied to isolate 3,5-dimethoxyphenanthrene-2,7-diol (DMP) and batatasin-I (BA-I) from the dichloromethane soluble extract of Dioscorea opposita. In this method, the lower phase of n-hexane-methanol-water system (HMW, 10 : 9 : 1, v/v) was used as a mobile phase A (MpA) and water was used as a mobile phase B (MpB). This gradient CPC method is comparable to that of reversed-phase HPLC method in that the stationary upper-phase of HMW (10 : 9 : 1 v/v) works as if it were reversed-phase silica gel due to its hydrophobic property, while the lower phase (MpA) and water (MpB) functioned as hydrophilic mobile phases. The initial condition of the mobile phase was 20% MpA/80% MpB and maintained for 150 min to obtain DMP (1.2 mg), and then MpA was increased up to 50% to elute BA-I (1.7 mg). The purities of DMP and BA-I were 94.1% and 98.3% with the recovery yields of 83% and 86%, respectively. Similar results were obtained by linear-gradient CPC. The CPC peak fractions were identified by comparing their retention time to those of authentic samples of DMP and BA-I and their spectroscopic data ($^1$H NMR and $^{13}$C NMR) to those of literature values.

Determination of Aloesin in Plasma by High-Performance Liquid Chromatography as Fluorescent 9-Anthroyl Derivative

  • Kim, Kyeong-Ho;Lee, Jin-Gyun;Park, Jeong-Hill;Shin, Young-Geun;Lee, Seung-Ki;Cho, Tae-Hyung
    • Archives of Pharmacal Research
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    • v.21 no.6
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    • pp.651-656
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    • 1998
  • A sensitive high-performance liquid chromatographic (HPLC) method for the determination of aloesin in plasma was developed. After solid-phase extraction from plasma and derivatization of aloesin and compound AD-1, which was prepared from aloesin as a internal standard, with 9-anthroylnitrile in the presence of quinuclidine, the derivatives were separated on a Inertsil ODS-3 column using acetonitrile/methanol/water (3:1:6) as a mobile phase, and detected fluorimetrically at 460nm with excitation at 360nm. The detection limit of aloesin was 3.2ng/ml in plasma (S/N=3).

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Resolution of Salbutamol Enantiomers in Human Urine by Reversed-phase High Performance Liquid Chromatography after Derivatization with (S)-(-)-${\alpha}$-methylbenzyl isocyanate

  • Kim, Kyeong-Ho;Kim, Tae-Kyun;Kwon, Young-Hee;Sohn, Young-Teak
    • Archives of Pharmacal Research
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    • v.20 no.5
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    • pp.486-490
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    • 1997
  • A stereospecific HPLC method has been developed for the resolution of the enantiomers of salbutamol in human urine. After solid-phase extraction and derivatization with (S)-(-)-${\alpha}$-methyl-benzyl isocyanate, the diastereomeric derivatives were resolved $(R_s=1.59)$ on $5{\mu}M$ octadecylsilan column using 47% methanol as a mobile phase with fluorescence detection. The detection limit of each enantiomer was 10 ng/ml (S/N=3).

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Liquid Chromatography of Aromatic Sulfonic Acids by Tetramethylammonium Bromide (Tetramethylammonium Bromide를 이용한 방향족 술폰산들의 액체크로마토그래피)

  • Oh, Hae-Beom
    • Journal of the Korean Chemical Society
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    • v.37 no.9
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    • pp.793-799
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    • 1993
  • Ion-pair model was predominated over ion-interaction model in the retention mechanism of analytes when tetramethylammonium bromide (TMAB) was used as a counter-ion in the investigation of aromatic sulfonic acids on the reversed-phase liquid chromatography by $C_{18}$ column as a stationary phase. The capacity factors of analytes were influenced by the type and concentration of counter-ions, concentrations of methanol and co-anion, types and position of functional group, and the pH mobile phase. Components of analyte mixture could be separated under the optimum conditions by this method.

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Quantitation and Validation of Atorvastatin using HPLC-UV

  • Heine, Daniel;Yong, Chul-Soon;Kim, Jung-Sun
    • Journal of Pharmaceutical Investigation
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    • v.37 no.3
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    • pp.187-192
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    • 2007
  • A reversed phase HPLC analysis of atorvastatin (AS) standard solution was performed using diclofenac (DF) as internal standard. Column oven temperature, flow rate and the composition of the mobile phase were varied in order to determine a practical system setup using a C18 column and UV detector. Two C18 columns of different length were compared regarding their influence on the AS peak shape. Based on these preliminary experiments a validation study was performed utilizing a C18 column at $62^{\circ}C$ with a mobile phase consisting of sodium phosphate buffer (0.05 M, pH 4.0), methanol and acetonitrile (40:50:10, v/v/v). The detection limit for AS was $0.1{\mu}g/ml$ and inter- and intra-day calibration curves were linear over a concentration range of $0.2-50{\mu}g/ml$. Accuracy and precision were satisfactory in the AS concentration range of $0.5-50{\mu}g/ml$.

Resolution of Salbutamol Enantiomers in Human Urine by Reversed-Phase High Performance Liquid Chromatography after Derivatization with 2,3,4,6-Tetra-O-acetyl-${\beta}$-D-glucopyranosyl Isothiocyanate

  • Kim, Kyeong-Ho;Kim, Tae-Kyun
    • Archives of Pharmacal Research
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    • v.21 no.2
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    • pp.217-222
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    • 1998
  • A stereospecific HPLC method has been developed for the resolution of the enantiomers of salbutamol in human urine. After solid-phase extraction and derivatization with 2,3,4,6-tetra-O-acetyl-$\beta$-D-glucopyranosyl isothiocyanate, the diastereomeric derivatives were resolved (Rs=1.83) on $5{\mu}m$ octadecylsilan column using 35% acetonitrile in 0.05M ammonium acetate buffer (pH=6) as a mobile phase with electrochemical detection. The diastereomeric derivatives were formed within 30 min. The detection limit of each enantiomer was 20 ng/ml (S/N=3).

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Quantitative Determination of Salidroside and Tyrosol from the Underground Part of Rhodiola rosea by High Performance Liquid Chromatography

  • Linh, Pham-Tuan;Kim, Young-Ho;Hong, Seon-Pyo;Jian, Jiang-Ji;Kang, Jong-Seong
    • Archives of Pharmacal Research
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    • v.23 no.4
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    • pp.349-352
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    • 2000
  • A reversed-phase high performance liquid chromatographic method was developed to determine salidroside and tyrosol simultaneously in the Rhodiola rosea. The optimum condition was Nova-pak $C_18$as stationary phase, 6.5% methanol in water as mobile phase and detection at UV 225 nm. The identification was carried out by comparing the retention time and LC/MS spectrum of the relevant peaks with those of isolated standards. The contents of salidroside and tyrosol in the samples gathered from various area in China were ranged over 1.3-11.1 ${m}g/g$ and 0.3-2.2 ${m}g/g$, respectively.

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Adaptive SLM Scheme Based on Peak Observation for PAPR Reduction of OFDM Signals (OFDM PAPR 감소를 위한 피크 신호 관찰 기반의 적응적 SLM 기법)

  • Yang, Suck-Chel;Shin, Yoan
    • Proceedings of the IEEK Conference
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    • 2006.06a
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    • pp.15-16
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    • 2006
  • In this paper, we propose an adaptive SLM scheme based on peak observation for PAPR reduction of OFDM signals. The proposed scheme is composed of three steps: peak scaling, sequence selection, and SLM procedures. In the first step, the peak signal samples in the IFFT outputs of the original input sequence are scaled down. In the second step, the sub-carrier positions where power difference between the original input sequence and the FFT outputs of the scaled signal is large, are identified. Then, the phase sequences which have the maximum number of phase-reversed sequence words only for these positions, are selected. Finally, only using the selected phase sequences, the generic SLM procedure is performed for the original input sequence. Simulation results reveal that the proposed adaptive SLM remarkably reduces the complexity in terms of IFFT and PAPR calculations than the conventional SLM, while maintaining the PAPR reduction performance.

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