• 제목/요약/키워드: liquid-phase standard

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HPLC Determination of Tolperisone in Human Plasma

  • Bae Jung-Woo;Park Young-Seo;Sohn Uy-Dong;Myung Chang-Sun;Ryu Byung-Kwon;Jang Choon-Gon;Lee Seok-Yong
    • Archives of Pharmacal Research
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    • v.29 no.4
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    • pp.339-342
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    • 2006
  • A simple high performance liquid chromatographic (HPLC) method was developed for the determination of tolperisone in human plasma. Tolperisone and internal standard (chlorphenesin) were isolated from 1 mL of plasma using 8 mL of dichlormethane. The organic phase was collected and evaporated under nitrogen gas. The residue was then reconstituted with 300 mL aliquot of mobile phase and a 100 mL aliquot was injected onto the $C_{18}$ reverse-phased column. The mobile phase, $45\%$ methanol containing $1\%$ glacial acetic acid and $0.05\%$ 1-hexanesulfonic acid was run at a flow rate of 1 mL/min. The column effluent was monitored using UV detector at 260 nm. The retention times for tolperisone and the internal standard were approximately 7.1 and 8.4 min, respectively. The standard curve was linear with minimal intra-day and inter-day variability. The quantification limit of tolperisone in human plasma was 10 ng/ mL. The proposed method has been applied to the determination of pharmacokinetic profile of tolperisone in Koreans. The T max of tolperisone in Koreans $(0.94{\pm}0.42\;h)$ was not significantly differ from that reported in Europeans (0.5-1 h), but the mean half-life in Koreans $(1.14{\pm}0.27\;h)$ was shorter than that in Europeans $(2.56{\pm}0.2\;h)$. The proposed HPLC method is simple, accurate, reproducible and suitable for pharmacokinetic study of tolperisone.

Effect of Additive Amount on Microstructure and Fracture Toughness of SiC-TiC Composites

  • Min-Jin Kim;Young-Wook Kim;Wonjoong Kim;Hun-Jin Lim;Duk-Ho Cho
    • The Korean Journal of Ceramics
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    • v.6 no.2
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    • pp.91-95
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    • 2000
  • Powder mixtures of $\beta$-SiC-TiC in a weight ratio of 2:1 containing 5-20 wt% additives ($Al_2O_3$-$Y_2O_3$) were liquid-phase sintered at $1830^{\circ}C$ for 1h by hot-pressing and subsequently annealed at $1950^{\circ}C$ for 6h to enhance grain growth. The annealed specimens revealed a microstructure of \"in situ-toughened composite\" as a result of the $\beta$longrightarrow$\alpha$ phase transformation of SiC during annealing. The increase of the content of additives accelerated the growth of elongated $\alpha$-SiC grains with higher aspect ratio and improved fracture toughness. The fracture toughness of SiC-TiC composite containing 20 wt% additive was 6.2 MPa.$m^{1/2}$.2}$.

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Quantitation of Flurbiprofen in Isopropyl Myristate by High Performance Liquid Chromatography (고속액체크로마토그래피를 이용한 미리스틴산이소프로필증 플루르비프로펜의 정량)

  • Kim, Hyun;Chi, Sang-Cheol
    • Journal of Pharmaceutical Investigation
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    • v.22 no.1
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    • pp.63-68
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    • 1992
  • An HPLC procedure with UV detection has been developed for the quantitation of flurbiprofen released into isopropyl myristate used as the receptor phase in an in vitro membraneless drug diffusion cell. The drug and the internal standard (oxaprozin) were extracted from isopropyl myristate with a mixture of dimethylsulfoxide:methanol:water (2:1:1) and quantitated using a reverse phase $C_{18}$ column. The chromatograms were completely free from interfering peaks, and the relative retention times of flurbiprofen and the internal standard were 4.9 and 6.8 min, respectively. Calibration plots were linear over the concentration range of $1-200\;{\mu}g/ml$ of flurbiprofen with correlation coefficients, all higher than 0.99. The mean intra-day precision and accuracy among three replicate sets of the assay in a day were 4.26 and 4.52%, respectively, whereas the mean inter-day precision and accuracy were 3.35 and 3.64%, respectively. The mean recovery of the drug was 92.5% over the calibration range. The method was simple, reliable and accurate for the quantitation of flurbiprofen in unpurified isopropyl myristate.

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Three-Phase Eulerian Computational Fluid Dynamics (CFD) of Air-Water-Oil Separator with Coalescer (유적 합체기가 포함된 공기-물-기름 분리 공정에 대한 3상 Eulerian 전산유체역학)

  • Lim, Young-Il;Le, Thuy T.;Park, Chi-Kyun;Lee, Byung-Don;Kim, Byung-Gook;Lim, Dong-Ha
    • Korean Chemical Engineering Research
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    • v.55 no.2
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    • pp.201-213
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    • 2017
  • Water is removed from crude oil containing water by using oil separator. This study aims to develop a three-dimensional (3D) Eulerian computational fluid dynamics (CFD) model to predict the separation efficiency of air-water-oil separator. In the incompressible, isothermal and unsteady-state CFD model, air is defined as continuous phase, and water and oil are given as dispersed phase. The momentum equation includes the drag force, lift force and resistance force of porous media. The standard k-${\varepsilon}$ model is used for turbulence flow. The exit pressures of water and oil play an important role in determining the liquid level of the oil separator. The exit pressures were identified to be 6.3 kPa and 5.1 kPa for water and oil, respectively, to keep a liquid level of 25 cm at a normal operating condition. The time evolution of volume fractions of air, water and oil was investigated. The settling velocities of water and oil along the longitudinal separator distance were analyzed, when the oil separator reached a steady-state. The oil separation efficiency obtained from the CFD model was 99.85%, which agreed well with experimental data. The relatively simple CFD model can be used for the modification of oil separator structure and finding optimal operating conditions.

A Study on Quantitative Method of Piperine in Pure Ground Black Pepper (후추중의 Piperine 정량법에 관한 연구)

  • 고종명
    • Journal of Food Hygiene and Safety
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    • v.10 no.3
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    • pp.169-174
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    • 1995
  • Piperine, component of pure ground black pepper, has strong stimulative and hot. Analytical method for piperine was developed by high performance liquid chromatography. Analytical conditions are as follows, mobile phase is 70% methanol, detector UV 343 nm (0.05 AuFs), column is Novapak 5 C18 (15 cm $\times$ 4.6mm), flow rate is 1.0ml/min, chart speed is 0.25 cm/min and injection volume is 20 ul. Analytical results are as follows that relative standard deviation is 1.15%, calibration curve is y=170473.1x-7848.5 (R2=0.999) that shows good linearity. Standard solution of piperine is stable up to 10 hr and content of piperine in pureground black pepper is 4.97$\pm$0.86% Retention time of piperine in HPLC method is about 7 min. Therefore, the developed HPLC method including simple pretreatment of sample will be contribute to quality mangement.

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Development of a high-performance liquid chromatographic method for the determintion of levosulpiride in plasma

  • Ban, Eun-Mi;Jang, Dong-Jin;Kim, Adele;Park, Jeong-Sook;Kim, Chong-Kook
    • Proceedings of the PSK Conference
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    • 2002.10a
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    • pp.400.3-401
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    • 2002
  • Levosulpiride is the levo-enantiomer from of racemic sulpride. abenzamide derivative selectively inhibition doparninergic D2 receptos at the trigger zone both in the central nervous system and in the gastrointestinal tract. We report a rapid and sensitive HPLC method using reverse phase C 18 column with fluorescence detection for separation and quantitation of levosulpiride in plasma. Tiapride was used as an internal standard. After adding an internal standard. levosulpiride in 800 ${\mu}l$ of plasma was extracted under basic conditions with ethyl acetate and methylene chloride. (omitted)

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Determination of tiropramide in human plasma by LC/MS/MS

  • Lee, Hye-Won;Ji, Hye-Young;Kim, Hee-Hyoun;Kim, Hae-Kyoung;Lee, Yong-Bok;Lee, Hye-Suk
    • Proceedings of the PSK Conference
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    • 2003.04a
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    • pp.277.2-278
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    • 2003
  • A liquid chromatography-tandem mass spectrometric (LC/MS/MS) method for the determination of tiropramide in human plasma was developed. Tiropramide and internal standard, cisapride were extracted from human plasma with MTBE at basic pH. A reverse-phase LC separation was performed on Luna C8 column with the mixture of acetonitrile-ammonium formate (10 mM, pH 4.5) (5:5, v/v) as mobile phase. (omitted)

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Analysis of the Coumarin Constituents in Peucedanii Radix (식방풍중의 Coumarin성분의 확인 및 정량)

  • Shin, Kuk-Hyun;Kang, Sam-Sik;Chi, Hyung-Joon
    • Korean Journal of Pharmacognosy
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    • v.23 no.1
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    • pp.20-23
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    • 1992
  • A new method for the analysis of coumarin constituents in the roots of Peucedanum japonicum by high performance liquid chromatography was established. Among two coumarin constituents identified, peucedanol was confirmed to be applicable to a standard compound. A reversed phase system with a ${\mu}Bondapak$ C_{18}$, column using $H_2O-MeOH=5\;:\;4$ as a moble phase was developed. Peucedanol and a minor constituent, umbelliferone were detected at 333nm and the analysis was successfully carried out within 20 min.

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Simultaneous Determination of Cinnamaldehyde and Coumarin in Oryeong-san using HPLC with Photodiode Array Detector

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Herbal Formula Science
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    • v.18 no.2
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    • pp.251-257
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    • 2010
  • Objectives : To develop and validate High-performance liquid chromatography-photodiode array methods for simultaneous determination of two constituents in Oryeong-san(ORS). Methods : Reverse-phase chromatography using a Gemini C18 column operating at $40^{\circ}C$, and photodiode array(PDA) detection at 280 nm, were used for quantification of the two marker components of ORS. The mobile phase using a gradient flow consisted of two solvent systems. Solvent A was $H_2O$ and solvent B was acetonitrile. Results : Calibration curves were acquired with correlation coefficient ($r^2$)>0.9999, and the relative standard deviation(RSD) values(%) for intra- and inter-day precision were not exceed 1.0%. The recovery rate of each compound was in the range of 93.01-104.16%, with an RSD less than 2.0%. The contents of two compounds in ORS were 1.10-3.72 mg/g. Conclusions : The established HPLC method will be helpful to improve quality control of ORS.

Determination of Terbutaline Enantiomers in Human Plasma by Coupled Achiral-Chiral High Performance Liquid Chromatography

  • Kim, Kyeong-Ho;Kim, Hyun-Ju;Hong, Seon-Pyo;Shin, Sang-Deok
    • Archives of Pharmacal Research
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    • v.23 no.5
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    • pp.441-445
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    • 2000
  • Achiral-chiral column switching HPLC assay was developed to allow the separation and quantification of the enantiomers of terbutaline in human plasma by means of fluorescence detection. Plasma samples were prepared by solid-phase extraction with sep-pak silica, followed by HPLC assay. The enantiomers of terbutaline and the internal standard were separated from the biological matrix on a silica column, and the two enantiomers were resolved and quantified on a Sumichiral OA-4900 column. The two columns were connected by a switching valve equipped with silica trap column, The trap column was used to concentrate the terbutaline in the eluent from the achiral column before back flushing onto the chiral phase. For each enantiomers, the assay was linear between 2.5-125 ng/$m\ell$ (r=0.9999) and detection limit was 1.0 ng/$m\ell$ .

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