• Title/Summary/Keyword: mobile phase

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Impedance Spectroscopy Models for X5R Multilayer Ceramic Capacitors

  • Lee, Jong-Sook;Shin, Eui-Chol;Shin, Dong-Kyu;Kim, Yong;Ahn, Pyung-An;Seo, Hyun-Ho;Jo, Jung-Mo;Kim, Jee-Hoon;Kim, Gye-Rok;Kim, Young-Hun;Park, Ji-Young;Kim, Chang-Hoon;Hong, Jeong-Oh;Hur, Kang-Heon
    • Journal of the Korean Ceramic Society
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    • v.49 no.5
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    • pp.475-483
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    • 2012
  • High capacitance X5R MLCCs based on $BaTiO_3$ ceramic dielectric layers exhibit a single broad, asymmetric arc shape impedance and modulus response over the wide frequency range between 1 MHz to 0.01 Hz. Analysis according to the conventional brick-layer model for polycrystalline conductors employing a series connection of multiple RC parallel circuits leads to parameters associated with large errors and of little physical significance. A new parametric impedance model is shown to satisfactorily describe the experimental spectra, which is a parallel network of one resistor R representing the DC conductivity thermally activated by 1.32 eV, one ideal capacitor C exactly representing bulk capacitance, and a constant phase element (CPE) Q with complex capacitance $A(i{\omega})^{{\alpha}-1}$ with ${\alpha}$ close to 2/3 and A thermally activated by 0.45 eV or ca. 1/3 of activation energy of DC conductivity. The feature strongly indicate the CK1 model by J. R. Macdonald, where the CPE with 2/3 power-law exponent represents the polarization effects originating from mobile charge carriers. The CPE term is suggested to be directly related to the trapping of the electronic charge carriers and indirectly related to the ionic defects responsible for the insulation resistance degradation.

Measurement of Optical Purity for Commercially Avialable Naproxen Sold in 2013 (2013년 시판된 나프록센의 광학순도 측정)

  • Seo, Hae Chan;Song, Jung Suk;Ryoo, Sang Hyun;Lee, Sang Heon;Ryoo, Dong Hyun;Yu, Jeong Jae;Ryoo, Jae Jeong
    • Journal of the Korean Chemical Society
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    • v.58 no.2
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    • pp.179-185
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    • 2014
  • Commercial (S)-naproxen was racemized under strong basic condition. After checking the peak position of (R)- and (S)-naproxen by analysis the recemized naproxen, optical purity of 19 commercialized naproxens sold in 2013 in Korea were examined by chiral HPLC. The Chiralcel OD-H column, ChiralHyun-LE(S)-1 column and LUX-Cellulose-1 column were used as chiral stationary phases and the mixed eluent of hexane:isopropanol:acetic acid as 100:1:0.1 was used as a mobile phase with a flow rate of 1.0 mL/min. Each data was obtained from an average value of at least three different experiments for each sample and the relative standard deviation of them appeared very small. The average optical purity values obtained from three different chiral columns were very similar and the total average optical purity value (99.32%) of nineteen commercialized naproxens used in this study were larger than those of three years ago (98.17%).

Measurement of Optical Purity for Commercially Avialable Dexibuprofen and Ibuprofen Sold in 2013 (2013년도 시판된 Dexibuprofen과 Ibuprofen의 광학 순도 측정)

  • Ryoo, Sang Hyun;Lee, Sang Heon;Seo, Hae Chan;Song, Jung Suk;Ryoo, Dong Hyun;Yu, Jeong Jae;Kim, Hyun Young;Lee, Jae Hwan;Ryoo, Jae Jeong
    • Journal of the Korean Chemical Society
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    • v.58 no.3
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    • pp.277-282
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    • 2014
  • The optical purity of 11 commercial dexibuprofens and 7 ibuprofens sold in Korea in 2013 were examined by chiral HPLC. The Chiralcel OD-H column and LUX-Cellulose-1 column were used as chiral stationary phases and the mixed eluent of hexane:isopropanol:acetic acid as 100:1:0.1 was used as a mobile phase with a flow rate of 1.0 mL/min. Each data was obtained from an average value of at least three different experiments for each sample and the average value of relative standard deviation of them appeared very small, 0.19%. Average optical purity value (97.5%) of eleven commercial dexibuprofens used in this study were smaller than those of 9 years ago (99.2%), but larger than four years ago (95.6%). Enantiomeric ratios of (R)- and (S)-isomers of seven ibuprofen samples used in this experiment were achieved at about 50:50 which was different with the result (44:56) from four years ago.

Liquid Chromatography Quadrupole Time-Of-Flight Tandem Mass Spectrometry for Selective Determination of Usnic Acid and Application in Pharmacokinetic Study

  • Fang, Minfeng;Wang, Hui;Wu, Yang;Wang, Qilin;Zhao, Xinfeng;Zheng, Xiaohui;Wang, Shixiang;Zhao, Guifang
    • Bulletin of the Korean Chemical Society
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    • v.34 no.6
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    • pp.1684-1688
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    • 2013
  • A rapid and sensitive method for determining usnic acid of Lethariella cladonioides in rat was established using high performance liquid chromatography (HPLC) quadrupole time-of-flight (QTOF) tandem mass (MS/MS). Rat plasma was pretreated by mixture of acetonitrile and chloroform to precipitate plasma proteins. Chromatographic separation was achieved on a column ($50{\times}2.1$ mm, $5{\mu}m$) with a mobile phase consisting of water (containing $5{\times}10^{-3}$ M ammonium formate, pH was adjusted to 3.0 with formic acid) and acetonitrile (20:80, v/v) at a flow rate of 0.3 mL/min. A tandem mass spectrometric detection with an electrospray ionization (ESI) interface was conducted via collision induced dissociation (CID) under negative ionization mode. The MS/MS transitions monitored were m/z 343.0448 ${\rightarrow}$ m/z 313.2017 for usnic acid and m/z 153.1024 ${\rightarrow}$ m/z 136.2136 for protocatechuic acid (internal standard). The linear range was calculated to be 2.0-160.0 ng/mL with a detection limit of 3.0 pg/mL. The inter- and intra-day accuracy and precision were within ${\pm}7.0%$. Pharmacokinetic study showed that the apartment of usnic acid in vivo confirmed to be a two compartment open model. The method was fully valid and will probably be an alternative for pharmacokinetic study of usnic acid.

Simultaneous determination of illegal galactagogue adulterants in supplement diets by LC-MS/MS

  • Lee, Ji Hyun;Cho, So-Hyun;Park, Han Na;Park, Hyoung Joon;Kim, Nam Sook;Park, Sung Kwan;Kang, Hoil
    • Analytical Science and Technology
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    • v.31 no.4
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    • pp.171-178
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    • 2018
  • Recently, for successful lactation, many breastfeeding mothers seek various products, including herbal medicine, dietary supplements, and prescribed medicines, to improve milk production. As demand for galactogogues grows, it is highly possible that pharmaceutical galactogogues may be adulterated with illegal products to maximize their efficacy. For continuous control and supervision of illegal products, we developed and validated a simple and sensitive LC-MS/MS method capable of simultaneously determining five galactogogues. Chromatographic separation was conducted using an Agilent Poroshell $120SB-C_{18}$ column with a mobile phase consisting of 20 mM ammonium formate (pH 5.4) and 100 % acetonitrile. The total run time was 13 min per analyte. The proposed method was performed according to the guidelines of the International Conference of Harmonization and it produced reliable results. This method showed high sensitivity and specificity, with a limit of detection (LOD) and limit of quantitation (LOQ) of 0.01-0.82 ng/mL and 0.02-2.45 ng/mL, respectively, for the solid- and liquid-type samples. Specificity was evaluated by analyzing matrix-blank samples spiked with the target compounds at LOQ levels, which provided a good separation of all peaks without interference. Additionally, the repeatability and intermediate precision were typically <15 %, whereas the recovery was 80-120 % of the values obtained using blank samples. Thus, we concluded that this method could be used for the identification and quantification of galactogogues in food or herbal products.

Thermodynamic Study of Poly(dimethylsiloxane)-Solvents Systems Using Inverse Gas Chromatography (Inverse Gas Chromatography를 이용한 Poly(dimethylsiloxane)-Solvent계의 열역학적 연구)

  • Cho, Joung-Mo;Kang, Choon-Hyoung
    • Applied Chemistry for Engineering
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    • v.10 no.5
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    • pp.718-725
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    • 1999
  • In order to investigate the interaction characteristics of poly(dimethylsiloxane) (PDMS) with various solvents such as water, ethanol, and iso-propanol, Inverse Gas Chromatography(IGC) at finite concentration, which is a very fast, accurate, and thus promising technique in thermodynamic study of polymer systems, is employed. By measuring the specific retention volumes of the probes, the interaction parameters are calculated by means of the Flory-Huggins equation. From the results, the interaction parameters of the probes are, as expected due to the hydrophobicity of the polymer, found to be of large positive values (2$2.0{\times}10^{-3}mol/g$. For the linear PDMS, interpretation of the space distribution of molecules is performed by the Kirkwood-Buff-Zimm(KBZ) integrals, which give intuitive information about physical properties. From the KBZ integrals, water does not show the tendency of preferential solvation with the PDMS but formed self-cluster. The larger solvent molecules show a stronger tendency to distribute more randomly in the mixture.

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Quantitative analysis of cholesterol in infant formula by isotope dilution liquid chromatography-tandem mass spectrometry (동위원소희석 액체크로마토그래피 질량분석법에 의한 분유 내 콜레스테롤의 정량)

  • Ahn, Eun Jeong;Lee, Hwa Shim;Kim, Byung Joo;Lee, Gae Ho
    • Analytical Science and Technology
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    • v.28 no.6
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    • pp.460-466
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    • 2015
  • An isotope dilution liquid chromatography tandem mass spectrometry was developed as a primary method for the quantitative analysis of cholesterol in infant formula. Cholesterol-d4 was used as an internal standard and spiked into the infant formula sample. In order to release cholesterol out of cholesteryl ester, which is cholesterol bound to fatty acids in infant formula, saponification was carried out. Saponification conditions were optimized with heating temperature, reaction time and the concentration of KOH. The optimum conditions were as follows; heating temperature was 70 ℃, reaction time was 180 min and the concentration of KOH was 0.8 mL of 8 M KOH for about 0.1 g infant formula sample. Extraction of cholesterol out of sample solution was carried out with hexane uisng liquid-liquid extraction. Chromatographic analysis was carried out using Phenomenex Kinetex C18 column. Mobile phase was 0.1% acetic acid in methanol/water (v/v, 99/1) and flow rate was 0.3 mL/min. Cholesterol and cholesterol-d4 were monitored at mass transfer m/z 369/259 and 373/263 respectively. Reproducibility of the method was evaluated to be 0.23% of the measurement result. The expanded uncertainty of the measurement result of cholesterol in infant formula was approximately 1.9% at a 95% confidence level. NIST standard reference material having certified values of cholesterol in infant formula, was analyzed in order to verify this method. The ID-LC/MS/MS results were well agreed with the certified values of NIST SRM within the uncertainty.

Determination of Fructooligosaccharides and Raffinose in Infant Formula by High Performance Liquid Chromatography with Evaporative Light Scattering Detector (HPLC-ELSC를 이용한 조제분유 중 fructooligosaccharides 및 raffinose 분석)

  • Shin, Man-Sub;Park, Jae-Woo;Cho, Mi-Ran;Song, Sung-Ok;Kim, Chun-Sun;Choi, Chun-Bae;Lee, Seoung-Won;Lee, Ki-Woong;Chang, Chi-Hoon;Kwak, Byung-Man
    • Korean Journal of Food Science and Technology
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    • v.38 no.6
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    • pp.725-729
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    • 2006
  • A method was developed for the determination of fructooligosaccharides and raffinose contents in infant formula. The samples were extracted and analyzed by liquid chromatography equipped with carbohydrate column and evaporative light scattering detector. The mobile phase used for the gradient mode was water-acetonitrile, at a flow rate of 1.0mL/min. The method showed a mean recovery of 95-99%, the relative standard deviation obtained in the precision study was 0.774-8.982%, the quantification and detection limits were 25-50mg/L.

Rapid and Simple Method for the Determination of Pregabalin in Human Plasma using Liquid Chromatography-tandem Mass Spectrometry (LC-MS/MS): Application to a Bioequivalence Study of Daewoong Pregabalin Capsule To Lyrica® Capsule (Pregabalin 150 mg)

  • Jang, Ki-Ho;Seo, Ji-Hyung;Yim, Sung-Vin;Lee, Kyung-Tae
    • Journal of Pharmaceutical Investigation
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    • v.41 no.4
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    • pp.255-262
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    • 2011
  • Method using liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was developed and validated for the determination of pregabalin in plasma samples. Acquisition was performed by monitoring the transitions: m/z 160.1${\rightarrow}$142.2 for pregabalin and m/z 423.2${\rightarrow}$207.1 for losartan (as an internal standard). After cold acetonitrileinduced protein precipitation of the plasma samples, separation was performed with C18 column by isocratic mobile phase consisted of 10 mM ammonium acetate and acetonitrile (15:85, v/v). Results were linear over the concentration ranged from 0.1 to $10{\mu}g$/mL and the correlation coefficients (r) were $\geq0.99$. Intra- and inter-day precisions were $\leq6.02$ and $\leq11.04%$, respectively, and intra- and inter-day accuracies were 96.60-101.09 and 98.10-102.60%, respectively. This validated method was successfully applied to a bioequivalence study of two formulations of pregabalin, Daewoong pregabalin capsule (Daewoong Pharm. Co., Ltd.) and Lyrica$^{(R)}$ capsule (Pfizer Korea Ltd.) in twenty eight healthy Korean volunteers. The subjects received a single oral dose of each formulation (150 mg as pregabalin) in a randomized $2{\times}2$ crossover study and plasma samples were obtained from each subject at predetermined time intervals. Then, the pharmacokinetic parameters ($AUC_{0-t}$, $C_{max}$ and $T_{max}$) were calculated and statistically analyzed to assess the differences between two formulations. The 90% confidence intervals for the log-transformed data were acceptable range of log 0.8-log 1.25 (e.g., log 1.0048-log 1.0692 for AUC0-t, log 0.9142-log 1.0421 for $C_{max}$). Thus, $AUC_{0-t}$ and $C_{max}$ met the criteria of the Korea Food and Drug Administration (KFDA) for bioequivalence test indicating that Daewoong pregabalin capsule was bioequivalent to Lyrica$^{(R)}$ capsule.

Petrology of the Chaeyaksan basaltic rocks and application of hornblende geobarometer (채약산 현무암질암류의 암석학적인 특징 및 각섬석 지질압력계의 적용)

  • 김상욱;황상구;양판석;이윤종;고인석
    • The Journal of the Petrological Society of Korea
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    • v.8 no.2
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    • pp.92-105
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    • 1999
  • The Cretaceous Chaeyaksan basaltic rocks consist mainly of basaltic tuffs intercalating three layers of basalt. Stratigraphically, the rocks are located between the upper Songnaedong Formation and the lower Geoncheonri Formation and contain plagioclase, augite, hornblende, and a few olivine phenocrysts. Geochemically, they show calc-alkaline characteristics in some immobile element content, but show the alkaline suite feature in the mobile major element composition. The basalts are widely spilitized but some of them is altered to shoshonitic rocks with more calcic plagioclase, calcite, and chlorite, and adularia veinlets are common in the rocks. It is supposed that the post-eruption alteration of the rocks is done through alkali-replacement by hydrothermal solution or vapor rather than by low grade regional metamorphism. It is considered that A1 in hornblende will be available for estimating the pressure of the pre-eruption magma in the reservoir although the plagioclase of the rocks are highly albitized. The crystallization pressure was calculated as 5.7Kb by the equation of Johnson and Rutherford(l989) incorporating of the effect of overestimate of .41T in hornblende in the case of quartz-free rocks. Application of the estimated temperature, pressure and the constituent of phenocrysts of the rocks to the experimental P-T phase diagram for basalts established by Green(1982) indicates the crystallization course and succession of growth of the phenocrysts during of rising and cooling of the magma reservoir; augite + augite and olivine + augite, olivine, and hornblende -+ augite and hornblende+ augite, hornblende, and plagioclase. Such evolution course of the magma may include crystal fractionation by the phenocrysts crystallization and contamination by country rock in lower crust.

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