• Title/Summary/Keyword: reversed phase

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Quantification of Vitamin $D_3$ and Its Derivatives in Marine Animal Foods by HPLC (HPLC에 의한 동물성 수산식품 중의 Vitamin $D_3$와 그 관련물질 정량에 관한 연구)

  • Kim, Seong-Jin;Kim, Ji-Soo;Joh, Yong-Goe
    • Journal of the Korean Applied Science and Technology
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    • v.10 no.2
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    • pp.11-18
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    • 1993
  • Contents of vitamin $D_3$ and 25-OH-vitamin $D_3$ in marine animal products(20 species) were determined by HPLC. The isomers of vitamin D, $D_2$ and $D_3$, were not clearly separated on a reversed phase, ${\mu}$ Bonda Pak, with 20% methanol-acetonitrile, and on a normal phase, Zorbax SIL. with 0.4% isopropanol-hexane, but 25-OH-vitamin $D_2$ and-$D_3$ were separated on either ${\mu}$ Bonda Pak with 10% methanol-acetonitrile, or on Zorbax SIL with 2.2% isopropanol-hexane, respectively. Although levels of vitamin $D_3$ and 25-OH-vitamin $D_3$ varied remarkably according to species, their average value(fish : $l,l87{sim}36,007$ I.U/sample 100g, mussel : $58{\sim}1,706$ I.U/sample 100g, pickle: $1,208{\sim}79,358$ I.U/sample 100g) was greatly higher than that of meat($80{\sim}100$ I.U/sample 100g) and dairy products($400{\sim}800$ I.U/sample 100g). Fatty tissues of fish and pickled fish intestines contained high level of vitamin $D_3$ and 25-OH-vitamin $D_3$, while the clam and mussel known to have various kinds of sterol including ${\Delta}^7$-sterol showed very low levels of vitamin $D_3$ and its derivative.

Collisionless Magnetic Reconnection and Dynamo Processes in a Spatially Rotating Magnetic Field

  • Lee, Junggi;Choe, G.S.;Song, Inhyeok
    • The Bulletin of The Korean Astronomical Society
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    • v.41 no.1
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    • pp.45.1-45.1
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    • 2016
  • Spatially rotating magnetic fields have been observed in the solar wind and in the Earth's magnetopause as well as in reversed field pinch (RFP) devices. Such field configurations have a similarity with extended current layers having a spatially varying plasma pressure instead of the spatially varying guide field. It is thus expected that magnetic reconnection may take place in a rotating magnetic field no less than in an extended current layer. We have investigated the spontaneous evolution of a collisionless plasma system embedding a rotating magnetic field with a two-and-a-half-dimensional electromagnetic particle-in-cell (PIC) simulation. In magnetohydrodynamics, magnetic flux can be decreased by diffusion in O-lines. In kinetic physics, however, an asymmetry of the velocity distribution function can generate new magnetic flux near O- and X-lines, hence a dynamo effect. We have found that a magnetic-flux-reducing diffusion phase and a magnetic-flux-increasing dynamo phase are alternating with a certain period. The temperature of the system also varies with the same period, showing a similarity to sawtooth oscillations in tokamaks. We have shown that a modified theory of sawtooth oscillations can explain the periodic behavior observed in the simulation. A strong guide field distorts the current layer as was observed in laboratory experiments. This distortion is smoothed out as magnetic islands fade away by the O-line diffusion, but is soon strengthened by the growth of magnetic islands. These processes are all repeating with a fixed period. Our results suggest that a rotating magnetic field configuration continuously undergoes deformation and relaxation in a short time-scale although it might look rather steady in a long-term view.

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Nonlinear Adsorption Isotherm of Single and Multi-Components of 2'-Deoxyribonucleosides (2'-deoxyribonucleosides의 단일 및 다성분계의 비선형 흡착평형식)

  • Jin, Long Mei;Han, Soon Koo;Choi, Dae-Ki;Row, Kyung Ho
    • Korean Chemical Engineering Research
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    • v.43 no.2
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    • pp.230-235
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    • 2005
  • Reversed-phase high-performance liquid chromatography (RP-HPLC) was used to determine the equilibrium isotherm of single and multi-components of dUrd(2'-deoxyuridine), dGuo(2'-deoxyguanosine), and dAdo(2'-deoxyadenosine) of 2'-deoxyribonucleosides by dynamic method. The composition of mobile phase was 90/10 vol.% (water/MeOH). With an increase in the injection volumes, the retention times were shorter and the peak shapes were triangle-shaped, so Langmuir-type isotherm was assumed. The Langmuir adsorption parameters were estimated by PIM (pulsed-input method), and the competitive Langmuir adsorption isotherm was further utilized. For the sample of the dUrd and dGuo whose retention times were relatively short, the agreement of between the calculated value and experimental data was fairly good in both single and multi-components, but for the dAdo, the last eluting component, some deviations were caused by non-linear and non-ideal properties.

Rapid Determination of Imatinib in Human Plasma by Liquid Chromatography-Tandem Mass Spectrometry: Application to a Pharmacokinetic Study

  • Yang, Jeong Soo;Cho, Eun Gi;Huh, Wooseong;Ko, Jae-Wook;Jung, Jin Ah;Lee, Soo-Youn
    • Bulletin of the Korean Chemical Society
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    • v.34 no.8
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    • pp.2425-2430
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    • 2013
  • A simple, fast and robust analytical method was developed to determine imatinib in human plasma using liquid chromatography-tandem mass spectrometry with electrospray ionization in the positive ion mode. Imatinib and labeled internal standard were extracted from plasma with a simple protein precipitation. The chromatographic separation was performed using an isocratic elution of mobile phase involving 5.0 mM ammonium formate in water-5.0 mM ammonium formate in methanol (30:70, v/v) over 3.0 min on reversed-stationary phase. The detection was performed using a triple-quadrupole tandem mass spectrometer in multiple-reaction monitoring mode. The developed method was validated with lower limit of quantification of 10 ng/mL. The calibration curve was linear over 10-2000 ng/mL ($R^2$ > 0.99). The method validation parameters met the acceptance criteria. The spiked samples and standard solutions were stable under conditions for storage and handling. The reliable method was successfully applied to real sample analyses and thus a pharmacokinetic study in 27 healthy Korean male volunteers.

Retention Behavior of the Phenols on the Binary and Ternary Mobile Phases in Reversed-Phase Liquid Chromatography (역상 액체크로마토그래피에 있어서 이성분과 삼성분 이동상에 대한 페놀류의 머무름 거동)

  • Dae Sub Oh;Sun Haing Lee;Soo Han Kim;Sang Tae Kim
    • Journal of the Korean Chemical Society
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    • v.30 no.4
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    • pp.352-358
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    • 1986
  • An extensive experimental survey on the retention behaviors of phenols in the binary solvent system such as methanol-water, acetonitrile-water and tetrahydrofuran-water as well as the ternary solvent system such as methanol-acetonitrile-water and methanol-tetrahydrofuran-water is presented. A linear equation, which describes the capacity factor as a function of the solvent composition in the mobile phase and is able to predict the retention behaviors of phenols, was obtained. The iso-eluotropic lines for the binary and ternary solvent system are based on the equal strength of the methanol-water solvent which shows an optimum separation of the phenols used. The specific effect of each solute in the binary solvent system appeared to be larger than those in the ternary system.

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Determination of Boron by Ion Pair Liquid Chromatography with Chromotropic Acid (Chromotropic Acid를 착화제로 이용한 이온쌍 액체 크로마토그래피에 의한 붕소의 분리와 정량)

  • Yun, Young Ja;Yu, Gu Yong
    • Journal of the Korean Chemical Society
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    • v.39 no.4
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    • pp.288-293
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    • 1995
  • The separation and determination of boron with chromotropic acid (1,8-Dihydroxynaphthalene-3,6-disulfonic acid) as a complex agent has been studied using ion pair liquid chromatography. The use of tetrabutylammonium bromide added as an ion pair reagent to mobile phase (MeOH 61%, phosphate buffer 39% pH=8.5) allowed good separation of boron-chromotrophic acid complex anion and chromotrophic acid on poly(styrene-divinylbenzene) based reversed phase column (PRP-1, 15 $cm{\times}4.6$ mm i.d.). The complex formation between boric acid and chromotrophic acid was enhanced in the presence of 0.1 M tetrabutylammonium bromide, resulting in high sensitivity. The linear calibration was achieved over the boron concentration range of 0.5∼1000 ${\mu}g/L.$ The detection limit was 0.5 ${\mu}g/L$ (S/N=2). The proposed method was applied to the determination of boron in commercially available chemicals, $Na_2SO_4$, NaOH, KCl.

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Determination of Glimepiride in Human Plasma by Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry

  • Kim, Ho-Hyun;Chang, Kyu-Young;Lee, Hee-Joo;Han, Sang-Beom
    • Bulletin of the Korean Chemical Society
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    • v.25 no.1
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    • pp.109-114
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    • 2004
  • A sensitive method for quantitation of glimepiride in human plasma has been established using liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS). Glipizide was used as an internal standard. Glimepiride and internal standard in plasma sample was extracted using diethyl etherethyl acetate (1 : 1). A centrifuged upper layer was then evaporated and reconstituted with the mobile phase of acetonitrile-5 mM ammonium acetate (60:40, pH 3.0). The reconstituted samples were injected into a $C_{18}$ reversed-phase column. Using MS/MS in the multiple reaction monitoring (MRM) mode, glimepiride and glipizide were detected without severe interference from human plasma matrix. Glimepiride produced a protonated precursor ion ([M+H]$^+$) at m/z 491 and a corresponding product ion at m/z 352. And the internal standard produced a protonated precursor ion ([M+H]]$^+$) at m/z 446 and a corresponding product ion at m/z 321. Detection of glimepiride in human plasma by the LC-ESI/MS/MS method was accurate and precise with a quantitation limit of 0.1 ng/mL. The validation, reproducibility, stability, and recovery of the method were evaluated. The method has been successfully applied to pharmacokinetic studies of glimepiride in human plasma.

Design and Fabrication of 5.5GHZ SSB optical modulator with polarization reversed structure (LiINbO3 기판의 분극반전을 이용한 5.5 GHz 대역 SSB 광변조기의 설계 및 제작)

  • Jeong, W.J.;Kim, W.K.;Yang, W.S.;Lee, H.M.;Lee, H.Y.;Kwon, S.W.
    • Korean Journal of Optics and Photonics
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    • v.17 no.2
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    • pp.175-180
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    • 2006
  • A single sideband(SSB) modulator operating at 5.5 GHz was fabricated by polarization inversion techniques. The dimension of domain inversion in a $LiINbO_3$ Mach-Zehnder structure was precisely controlled so that the RF signal applied on two Mach-Zehnder arms gives rise to $90^{\circ}$ effective phase difference. The single sideband suppression was maximized by optimization of the polarization status of the optical input and by the DC bias value. The fabricated device showed the center frequency of 5.8 GHz and the maximum sideband suppression of 33dB, where the bandwidth of 15 dB sideband suppression ranged over a 2.5 GHz span. The optical phase delay could be regulated by the DC bias voltage, fur example, the enhanced optical modulation sideband was distinctively switched from the upper sideband to the lower sideband by changing the DC bias voltage from 1.9 V to -10.6 V.

High Performance Liquid Chromatographic Assay of a New Fluoroquinolone, LB20304, in the Plasma of Rats and Dogs

  • Seo, Mi-Kyeong;Jeong, Yi-Na;Kim, Hoon-Joo;Kim, In-Chull;Lee, Yong-Hee
    • Archives of Pharmacal Research
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    • v.19 no.6
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    • pp.554-558
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    • 1996
  • High-performance liquid chromatographic method was developed for the determination or LB 20304 (compound 1) in the plasma of rats and dogs. The analyte was deproteinized with 1 volume of methanol and 1/2 volume of 10% zinc sulfate, and the supernatant was injected onto a reversed-phase HPLC column. The mobile phase was a mixture of 24 parts of acetonitrile and 76 parts of 0.1% trifluoroacetic acid. The flow rate was 1 ml/min, and the effluent was monitored by fluorescence detector at an excitation wavelength of 337 nm and an emission wavelength of 460 nm. The retention time of compound 1 was 6.3 min. The assay of compound 1 was linear over the concentration range of 0.2-100.mu.g/ml in the plasma of rats and dogs. The lower limit of quantification was 0.2.mu.g/ml using 100.mu.l of plasma with a 97-99% accuracy and a 12-14% precision. In the 0.5, 5, and 50.mu.g/ml quality control samples, the intra- and inter-day accuracy were 88-95% and 88-97%, whereas intra- and interday precision were 0.5-6.6% and 0.2-9.3%, respectively, in the plasma of rats and dogs. The recoveries were 68-71% independent of concentration and species in the plasma. No interferences from endogenous substances were observed. Taken together, the above HPLC assay method by deproteinization and fluorescence detection was suitable for the determination of compound 1 in the preclinical pharmacokinetics.

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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.