• Title/Summary/Keyword: reversed phase

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UV-HPLC Determination of Carbowyl Group Using 2-Bromoacetyltriphenylene as a Pre-labeling Reagent - The isolative determination of prostaglandin $E_2$ and $F_2{\alpha}$ by HPLC (2-Bromoacetyltriphenylene 유도체화제를 이용한 카르복실기 함유성분의 분석법 (I) - 프로스타글란딘 $E_2$$F_2{\alpha}$ 혼합물의 HPLC에 의한 분리정량)

  • 이왕규;정해수;김박광
    • YAKHAK HOEJI
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    • v.30 no.6
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    • pp.311-316
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    • 1986
  • A new UV labeling reagent was developed and used in HPLC for the determination of prostaglandin $E_2$ which have weak UV light-absorbing property. This reagent, 2-bromoacetyltriphenylene, was synthesized by the bromination of 2-acetyltriphenylene which was obtained from triphenylene by Friedel-Crafts reaction. The wave length maximum (${\lambda}_{max}^{CH_3CN}$ of this reagent was 268nm. Prostaglandin E$_2$ was extracted from prostaglandin E$_2$-$\beta$-cyclodextrin using a Sep-pak $C_{18}$ cartridge. The prostaglandin E$_2$ was labeled with 2-bromoacetyl-triphenylene in aectonitrite using 18-crown-6-ether as catalyst. Derivatized prostaglandins were separated on a reversed-phase column (Radial-pak) $\mu$-Bondapak $C_{18}$ using acetonitrile: water=60:40 as mobile phase. The effluent was monitored by UV detector at 254nm filter kit. Linearity of calibration curve was obtained between 30ng and 140ng, and the lower limit of detection was 5ng.

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Determination and Ethylene Oxide(EO) Separation of Polysorbates by RP-HPLC (역상 HPLC에 의한 polysorbates의 산화에틸렌(EO) 분리 및 정량분석)

  • Lee, Yong-Hwa
    • Journal of the Korean Applied Science and Technology
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    • v.29 no.4
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    • pp.585-593
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    • 2012
  • The EO separation and quantitative determination of polysorbate 20, polysorbate 40, polysorbate 60 and polysorbate 80 was carried out by reversed phase HPLC. The water/acetonitrile was used for the mobile phase of gradient conditions. An YMC Pack Ph ($250mm{\times}4.6mm$ i.d., $5{\mu}m$) and Phenomenex C4 ($250mm{\times}4.6mm$ i.d., $5{\mu}m$) and the selected ELSD detector was applied. The analysis results of HPLC showed good linearity with correlation coefficient of $r^2$=0.997 in the rage of $180.2{\sim}980.5{\mu}g/mL$ and detection limit.

Simultaneous determination of sunscreen agents in cosmetics by HPLC (HPLC를 이용한 화장품 중의 자외선 차단제 동시분석방법 연구)

  • Lee, Yong-Hwa;Yang, Jae-Chan
    • Journal of the Korean Applied Science and Technology
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    • v.29 no.4
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    • pp.577-584
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    • 2012
  • The simultaneous analysis of sun screen agents in commercial cosmetic samples was carried out by High Perfomance Liquid Chromatography(HPLC). The cosmetic samples are directly dissolved in Tetrahydrofurane(THF) and filtered using $0.45{\mu}m$ filter. The water/methanol/THF was used for the mobile phase of gradient conditions. An Extend C18 reversed-phase column and the selected UV/Visible detector was applied. The analysis results of HPLC showed good linearity with correlation coefficient of $r^2$=0.9992 in the rage of $50{\sim}800{\mu}g/mL$ and detection limit of $0.01{\mu}g/mL$.

Simplified HPLC Method for the Determination of Mirtazapine in Human Plasma and Its Application to Single-dose Pharmacokinetics

  • Gwak Hye-Sun;Lee Na-Young;Chun In-Koo
    • Biomolecules & Therapeutics
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    • v.14 no.1
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    • pp.40-44
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    • 2006
  • Mirtazapine is an antidepressant agent with dual action on both the noradrenergic and serotonergic neurotransmitter systems. A simple high performance liquid chromatographic method has been developed and validated for the quantitative determination of mirtazapine in human plasma. A reversed-phase Cl8 column was used for the determination of mirtazapine with a mobile phase composed of 0.01M ammonium acetate solution (pH 4.2) and acetonitrile (75:25, v/v%) at a flow rate of 1.2 mL/min. Terazosin hydrochloride was used as an internal standard. The fluorescence detector was set at excitation and emission wavelengths of 290 and 350 nm, respectively. Intra- and inter-day precision and accuracy were acceptable for all quality control samples including the lower limit of quantification of 3 ng/mL. Mirtazapine was stable in human plasma under various storage conditions. This method was used successfully for a pharmacokinetic study using plasma samples after oral administration of a single 30 mg dose as mirtazapine base to 8 healthy volunteers. The maximum plasma concentration of mirtazapine was $64.1{\pm}28.0ng/mL$ at 1.8 h, and the area under the curve and elimination half-life were calculated to be $674.1{\pm}218.5ng\;h/mL\;and\;23.4{\pm}3.8h$, respectively.

Column-switching High Performance Liquid Chromatographic Determination of Fluconazole in Human Plasma (컬럼 스위칭 고속액체크로마토그라프법을 이용한 혈장 중 플루코나졸의 분석)

  • Jee, Jun-Pil;Jin, Sook;Lee, Mi-Kyung;Kim, Yang-Bae;Kim, Chong-Kook
    • Journal of Pharmaceutical Investigation
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    • v.30 no.1
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    • pp.51-54
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    • 2000
  • A column-switching high performance liquid chromatographic method has been developed for the determination of a fluconazole in human plasma. Each plasma sample was centrifuged for 10 min at 5000 g. After an aliqout of the supernatant was taken to nylon microcentrifuge filter, these samples were centrifuged for 10 min at 5000 g. An aliqout of the supernatant was injected directly onto the HPLC column. Deionized water was run for 2 min at a flow rate of 1.0 ml/min to retain fluconazole in an extration column, while proteins and endogenous interferences were eluted to the waste. The analyte was then back-flushed onto an analytical column, $C_{18}$ reversed-phase column. The mobile phase for analytical column, 0.01 M sodium acetate (pH 5.0)-methanol (65:35, v/v), was run at a flow rate of 1.0 ml/min. The column effluent was monitored by ultraviolet detection at 261 nm. The retention time for fluconazole was 11.76 min in human plasma. The detection limit for fluconazole in human plasma was $0.2\;{\mu}g/ml$. No interference from endogenous substances was observed.

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Parameter Estimation of Perillyl Alcohol in RP-HPLC by Moment Analysis

  • Row Kyung Ho;Lee Chong Ho;Kang Ji Hoon
    • Biotechnology and Bioprocess Engineering:BBE
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    • v.7 no.1
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    • pp.16-20
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    • 2002
  • Parameter estimations were made for the reversed-phase adsorption of perillyl alcohol (POH), a potent anti-cancer agent, on octadecylsilyl-silica gel (ODS). The average particle diameter of ODS was about $15\;{\mu}m$, and the particles were packed in the column $(3.9\;\times\;300mm)$. The mobile phase used was a mixture of acetonitrile and water, in which the acetonitrile ranged between 50 and $70\;(v/v\;\%)$. The first absolute moment and the second central moment were determined from the chromatographic elution curves by moment analysis. Experiments were carried out using POH solutions within the linear adsorption range. The fluid-to-particle mass transfer coefficient was estimated using the Wilson-Geankoplis equation. The axial dispersion coefficient and the intra particle diffusivity were determined from the slope and intercept of a plot of H vs $1/u_0$, respectively. The contributions of each mass-transfer step were axial dispersion, fluid-to-particle mass transfer, and intraparticle diffusion.

Synthesis of Periodic Mesoporous Organosilica by Microwave Heating

  • Yoon, Sang-Soon;Son, Won-Jin;Biswas, Kalidas;Ahn, Wha-Seung
    • Bulletin of the Korean Chemical Society
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    • v.29 no.3
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    • pp.609-614
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    • 2008
  • A periodic mesoporous organosilica material was synthesized by microwave heating (PMO-M) using 1,2-bis(trimethoxysilyl)ethane as a precursor in a cationic surfactant solution, and textural properties were compared with those of the product produced by conventional convection heating (PMO-C). These synthesized materials were characterized using XRD, TEM/SEM, N2 adsorption isotherm, 29Si and 13C NMR, and TGA, which confirmed their good structural orders and clear arrangements of uniform 3D-channels. Synthesis time was reduced from 21 h in PMO-C to 2-4 h in PMO-M. PMO-M was made of spherical particles of 1.5-2.2 m m size, whereas PMO-C was made of decaoctahedron-shaped particles of ca. 8.0 m m size. Effect of synthesis temperature, time, and heating mode on the PMO particle morphology was examined. The particle size of PMO-M could be controlled by changing the heating rate by adjusting microwave power level. PMO-M demonstrated improved separation of selected organic compounds compared to PMO-C in a reversed phase HPLC experiment. Ti-grafted PMO-M also resulted in higher conversion in liquid phase cyclohexene epoxidation than by Ti-PMO-C.

Quantitative Determination of Amitriptyline and Its Metabolite in Rat Plasma by Liquid Chromatography-tandem Mass Spectrometry

  • Chae, Jung-Woo;Baek, In-Hwan;An, Jung-Hwa;Kim, Eun-Jung;Kwon, Kwang-Il
    • Bulletin of the Korean Chemical Society
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    • v.33 no.7
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    • pp.2163-2167
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    • 2012
  • A rapid, specific, and reliable LC-MS/MS-based bioanalytical method was developed and validated in rat plasma for the simultaneous quantitation of amitriptyline and its metabolite nortriptyline. Chromatographic separation of these analytes was achieved on a Gemini C18 column ($50{\times}4.60mm$, $5{\mu}m$) using reversed-phase chromatography. The mobile phase was an isocratic solvent system consisting of 1% formic acid in water and methanol (10:90, v/v), at a flow rate of 0.2 mL/min. The analytical range was set as 0.1-500 ng/mL for amitriptyline and 0.08-500 ng/mL for nortriptyline using a $200{\mu}L$ plasma sample. The accuracy and precision of the assay were in accordance with FDA regulations for the validation of bioanalytical methods. The validated method was successfully applied to a pharmacokinetic study in six rats after oral administration of amitriptyline (15 mg/kg). This method allows laboratory scientists to rapidly determine amitriptyline and nortriptyline concentrations in plasma.

Quantitation of Mevinolinic Acid in Human Plasma by HPLC (고속액체크로마토그래피를 이용한 사람 혈장중 메비놀린 산의 정량)

  • Oh, Han-Suk;Park, Dong-Young;Seo, Sung-Hoon;Kim, Young-Gwan;Hong, Seon-Pyo;Choi, Young-Wook;Lee, Kyung-Tae
    • Journal of Pharmaceutical Investigation
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    • v.30 no.4
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    • pp.279-282
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    • 2000
  • Simple and precise high-performance liquid chromatographic (HPLC) assay was developed and validated for the determination of a HMG-CoA reductase inhibitor, $lovastatin^{TM}$ and its active metabolite (mevinolinic acid) in human plasma. The method involved solid phase extraction of mevinolinic acid and internal standard using Sep-Pak Cartridge. Samples were analyzed by reversed-phase HPLC using $Capcell-Pak\;C_{18}$ column with ultraviolet detection at 238 nm. The quantitation limit of mevinolinic acid was 2 ng/ml and the calibration curve was linear over the range of 2-50 ng/ml $(r^2>0.999)$ with human plasma. The analyses of quality control samples indicated that the normal values could be predicted with an accuracy >97%. The intra- and inter-day coefficients of variation for the analyses were <10%. The average recoveries were similar (79%) for mevinolinic acid and methylmevinolinic acid. The method described has been successfully applied to the quantification of mevinolinic acid in about 1,000 human plasma samples over six-month period.

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Spatial and Temporal Electrodynamics in Acuzones: Test-Induced Kinematics and Synchronous Structuring. Phenomenological Study

  • Babich, Yuri F.;Babich, Andrey Y.
    • Journal of Acupuncture Research
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    • v.38 no.4
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    • pp.300-311
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    • 2021
  • Background: So far there is no confidence in the basics of acupoint/meridian phenomena, specifically in spatial and temporal electrical manifestations in the skin. Methods: Using the skin electrodynamic introscopy, the skin areas of 32 × 64 mm2 were monitored for spectral electrical impedance landscape with spatial resolution of 1 mm, at 2 kHz and 1 MHz frequencies. The detailed baseline and 2D test-induced 2 kHz-impedance phase dynamics and the 4-parameter time plots of dozens of individual points in the St32-34 regions were examined in a healthy participant and a patient with mild gastritis. Non-thermal stimuli were used: (1) (for the sick subject), microwaves and ultraviolet radiation applied alternately from opposite directions of the meridian; and (2) (for the healthy one) microwaves to St17, and cathodic/anodic stimulation of the outermost St45, alternately. Results: In both cases, the following phenomena have been observed: emergence of in-phase and/or antiphase coherent structures, exceeding the acupoint conditional size of 1 cm; collective movement along the meridian; reversible with a reversed stimulus; counter-directional dynamics of both whole structures and adjacent points; local abnormalities in sensitivity and dynamics of the 1 MHz and 2 kHz parameters indicating existence of different waveguide paths. Conclusion: It is assumed that these findings necessitate reconsideration of some basic methodological issues regarding neurogenic/acupuncture points as spatial and temporal phenomena; this requires development of an appropriate approach for identifying the acuzones patterns. These findings may be used for developing new approaches to personalized/controlled therapy/treatment.