• Title/Summary/Keyword: Two-phase extraction

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Determination of terbutaline in human plasma by coupled column chromatography (커플드칼럼크로마토그래피에 의한 사람 혈장 중 테르부탈린의 정량)

  • Ko, Mi Young;Jeon, Sang-Seol;Kim, Kyeong Ho
    • Analytical Science and Technology
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    • v.28 no.2
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    • pp.125-131
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    • 2015
  • A method was developed and fully validated for the determination of terbutaline, a β2-receptor agonist, in human plasma. Plasma samples were prepared by solid-phase extraction with Sep-Pak silica, followed by high-performance liquid chromatography (HPLC). The terbutaline was pre-separated from the interfering components in plasma on a Luna C18 (2) column, and terbutaline and salbutamol as an internal standard were resolved and determined on a Luna Silica column. The two columns were connected by a switching valve equipped with silica pre-column. The pre-column was used to concentrate the terbutaline in the eluent from the C18 column before back-flushing onto the silica column with fluorescence detection at an excitation/emission wavelength of 276/306 nm. The method was shown to be specific by testing six different human plasma sources. Linearity was established for a concentration range of 0.4-20.0 ng/mL with a correlation coefficient of 0.9999. The lower limit of quantitation was 0.4 ng/mL with a precision of 10.1% as C.V.%.

Evaluation of Sampling and Analytical Methods for the Determination of Polycyclic Aromatic Hydrocarbons in the Ambient Atmosphere (환경대기중 다환방향족탄화수소의 포집과 분석방법에 관한 연구)

  • 백성옥
    • Journal of Korean Society for Atmospheric Environment
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    • v.7 no.1
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    • pp.1-16
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    • 1991
  • In this study, sampling and analytical procedures were evaluated for the determination of ambient levels of atmospheric PAH, both in gaseous and particulate phase. The method involves low-volume sampling and Soxhlet extraction of the filters and Tenax absorbent, followed by a clean-up stage using a silica column prior to analysis by reversed-phase HPLC with wavelength programmable fluorescence and UV detection. A total of 18 PAH were identified and quantified, all of which have been of environmental concern. In order to validate the methodology and to ensure compatibility of the results, the analytical method used for the determination of PAH was evaluated with respect to the efficiencies of extraction and clean-up procedure, HPLC separation, and lower limits of detection. In addition, substrate dependency of PAH recovery was investigated for the two types of fiters, i.e. glass fiber and PTFE filters.

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Screening of Antagonistic Actinomycetes for Potato Scab Control and Isolation of Antibiotic Compound (감자 더뎅이병원균에 대해 길항활성을 갖는 방선균 탐색 및 항균 활성물질의 분리)

  • Lee, Hyang-Burm;Cho, Jong-Wun;Lim, Chi-Hwan;Kim, Chang-Jin
    • Applied Biological Chemistry
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    • v.47 no.2
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    • pp.164-169
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    • 2004
  • In the course of our screening for biocontrol agent (BCA) against Streptomyces scabiei and S. turgidiscabies causing potato scab using 5,000 actinomtcete isolates, 9 antagonistic strains were selected as BCA candidates through in vitro and in vivo assay. An antagonistic strain, A020645 was highly resistant to some pesticides and antibiotics such as dazomet and mancozeb and showed high control value in vivo. Two bioactive compounds (compound A, B) were purified by anion exchange chromatography, solid phase (ODS) extraction, TLC and reverse phase HPLC. Their chemical structures are now thought to be nucleoside derivative as determined by $^1H-NMR$ data analysis. Their full chemical structures would be elucidated through $^{13}C-NMR$, HMQC and HMBC analyses. Further studies will be focused on fitness in soil and formulation of the BCA candidates.

Effectiveness of anchorage with temporary anchorage devices during anterior maxillary tooth retraction: A randomized clinical trial

  • Barthelemi, Stephane;Desoutter, Alban;Souare, Fatoumata;Cuisinier, Frederic
    • The korean journal of orthodontics
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    • v.49 no.5
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    • pp.279-285
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    • 2019
  • Objective: This study evaluated the efficiency of anchorage provided by temporary anchorage devices (TADs) in maxillary bicuspid extraction cases during retraction of the anterior teeth using a fixed appliance. Methods: Patients aged 12 to 50 years with malocclusion for which bilateral first or second maxillary bicuspid extractions were indicated were included in the study and randomly allocated to the TAD or control groups. Retraction of the anterior teeth was achieved using skeletal anchorage in the TAD group and conventional dental anchorage in the control group. A computed tomography (CT) scan was performed after alignment of teeth, and a second CT scan was performed at the end of extraction space closure in both groups. A three-dimensional superimposition was performed to visualize and quantify the maxillary first molar movement during the retraction phase, which was the primary outcome, and the stability of TAD movement, which served as the secondary outcome. Results: Thirty-four patients (17 in each group) underwent the final analysis. The two groups showed a significant difference in the movement of the first maxillary molars, with less significant anchorage loss in the TAD group than that in the control group. In addition, TAD movement showed only a slight mesial movement on the labial side. On the palatal side, the mesial TAD movement was greater. Conclusions: In comparison with conventional dental anchorage, TADs can be considered an efficient source of anchorage during retraction of maxillary anterior teeth. TADs remain stable when correctly placed in the bone during the anterior tooth retraction phase.

Validation on the Analytical Method of Ginsenosides in Red Ginseng

  • Cho B. G.;Nho K. B.;Shon H. J.;Choi K. J.;Lee S. K.;Kim S. C;Ko S. R.;Xie P. S.;Yan Y. Z.;Yang J. W.
    • Proceedings of the Ginseng society Conference
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    • 2002.10a
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    • pp.491-501
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    • 2002
  • A cross-examination between KT&G Central Research Institute and Guangzhou Institute for Drug Control was carried out in order to select optimum conditions for extraction, separation and determination of ginsenosides in red ginseng and to propose a better method for the quantitative analysis of ginsenosides. The optimum extraction conditions of ginsenosides from red ginseng were as follows: the extraction solvent, $70\%$ methanol; the extraction temperature, $100^{\circ}C;$ the extraction time, 1 hour for once; and the repetition of extraction, twice. The optimum separation conditions of ginsenosides on the SepPak $C_{18}$ cartridge were as follows: the loaded amount, 0.4 g of methanol extract; the washing solvents, distilled water of 25 ml at first and then $30\%$ methanol of 25 ml; the elution solvent, $90\%$ methanol of 5 ml. The optimum HPLC conditions for the determination of ginsenosides were as follows: column, Lichrosorb $NH_2(25{\times}0.4cm,$ 5${\mu}m$, Merck Co.); mobile phase, a mixture of acetonitrile/water/isopropanol (80/5/15) and acetonitrile/water/isopropanol (80/20/15) with gradient system; and the detector, ELSD. On the basis of the optimum conditions a method for the quantitative analysis of ginsenosides were proposed and another cross-examination was carried out for the validation of the selected analytical method conditions. The coefficient of variances (CVs) on the contents of ginsenoside-$Rg_{1}$, -Re and $-Rb_1$ were lower than $3\%$ and the recovery rates of ginsenosides were $89.4\~95.7\%,$ which suggests that the above extraction and separation conditions may be reproducible and reasonable. For the selected HPLC/ELSD conditions, the CVs on the detector responses of ginsenoside-Rg, -Re and $-Rb_1$) were also lower than $3\%$, the regression coefficients for the calibration curves of ginsenosides were higher than 0.99 and two adjacent ginsenoside peaks were well separated, which suggests that the above HPLC/ELSD conditions may be good enough for the determination of ginsenosides.

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Differential Interference Contrast Microscopic Module Using a Polarization Grating for Quantitative Phase Imaging (편광 격자 기반 정량적 위상 이미징을 위한 미분 간섭 현미경 모듈 개발)

  • Jin Hee Cho;Ki-Nam Joo
    • Korean Journal of Optics and Photonics
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    • v.34 no.6
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    • pp.261-268
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    • 2023
  • We propose a compact differential interference contrast microscopic module, which enables snapshot measurements for quantitative phase imaging. The proposed module adopts the lateral shearing interferometric principle, which can obtain self-interference without a reference. Due to the absence of the reference, the system is more stable than the typical interferometric systems. It uses a polarization grating to generate two laterally shifted wavefronts based on its birefringence and polarizing beam-splitting characteristics. Furthermore, the use of a polarization camera does not require sequential measurements for the phase extraction. In the experiments, we observe and measure the timely varying changes of various specimens to verify the system performance with the bright field images and phase contrast images. Because the proposed microscopic module also has the merit of being adaptable to typical microscopy instead of using an imaging camera, it can conveniently replace conventional contrast microscopy.

Design and Realization of Phase Sensitive Detector Circuitry of Two-Channel Ring-Core Flux-Gate Compass (2-체널 링-코어 플럭스-게이트 콤파스의 위상검출 회로 설계와 구현에 관한 연구)

  • Yim, Jeong-Bin
    • Journal of Navigation and Port Research
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    • v.26 no.1
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    • pp.127-136
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    • 2002
  • This paper Presents a discussion on the design and realization for the Phase Sensitive Defector (PSD) circuitry of Flu$\chi$-gate Compass that gives direction information to the Directional Frequency Analysis and Recording (DIFAR) Sonobuoy in Air Anti-Submarine Warfare. PSD circuitry is realized with Twin-T RC networked active band-pass filter. Results of a performance test the PSD circuitry shows that the effectiveness of band-pass filtering of desired $2F_0$ second harmonic signal, which is Pro- portional to the direction of earth's magnetic field. This resulted in the extraction of direction information.

One-Cycle Control Strategy for Dual-Converter Three-Phase PWM Rectifier under Unbalanced Grid Voltage Conditions

  • Xu, You;Zhang, Qingjie;Deng, Kai
    • Journal of Power Electronics
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    • v.15 no.1
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    • pp.268-277
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    • 2015
  • In this paper, a dual-converter three-phase pulse width modulation (PWM) rectifier based on unbalanced one-cycle control (OCC) strategy is proposed. The proposed rectifier is used to eliminate the second harmonic waves of DC voltage and distortion of line currents under unbalanced input grid voltage conditions. The dual-converter PWM rectifier employs two converters, which are called positive-sequence converter and negative-sequence converter. The unbalanced OCC system compensates feedback currents of positive-sequence converter via grid negative-sequence voltages, as well as compensates feedback currents of negative-sequence converter via grid positive-sequence voltages. The AC currents of positive- and negative-sequence converter are controlled to be symmetrical. Thus, the workload of every switching device of converter is balanced. Only one conventional PI controller is adopted to achieve invariant power control. Then, the parameter tuning is simplified, and the extraction for positive- and negative-sequence currents is not needed anymore. The effectiveness and the viability of the control strategy are demonstrated through detailed experimental verification.

Separation and recovery of semi-volatile substances of Cnidii Rhizoma, Aucklandiae Radix and Amomum Fructus by reduced pressure collections and GC-MS

  • Lee, In-Ho;Byun, Chang Kyu;Eum, Chul Hun;Kim, Taewook;Lee, Sam-Keun
    • Analytical Science and Technology
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    • v.33 no.1
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    • pp.11-22
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    • 2020
  • When extracting semi-volatile components of herbal medicines using hot water vapor, some substances may react with water vapor or oxygen, and some volatile substances may be lost, when using an organic solvent extraction method has the disadvantage that it may contain a non-volatile material and residual organic solvent. In addition, it is inefficient to separate semi-volatile substances from herbal medicines into each single component and conduct biological activity research for each component to determine the effective ingredient, and some components may be lost in the separation process. In this study, semi-volatile substances evaporated under two pressure-reduced conditions in Chinese herbal medicines such as Cnidii Rhizoma, Aucklandiae Radix and Amomum Fructus were separated by cooling with liquid nitrogen. Those were analyzed by gas chromatography-mass spectrometry (GC-MS) to identify the components, and this method may be used to study biological activities at the cellular level. The substances separated under reduced pressure, essential oil obtained by simultaneous distillation extraction (SDE) method and substances by using solid phase micro-extraction (SPME) from Cnidii Rhizoma, Aucklandiae Radix and Amomum Fructus were analyzed by GC-MS. In the case of Cnidii Rhizoma and Aucklandiae Radix, there were some differences among the essential oil components obtained by SDE and those identified by low temperature capture (CT) and SPME method, these were believed to be produced by some volatiles reacting with water or oxygen at the boiling point temperature of water.

Analysis of Polycyclic Aromatic Hydrocarbons in Agricultural Waterways in Chungbuk and Gyeongbuk Provinces in Korea

  • Kim, Leesun;Lee, Jong-Hwa;Kim, Jeong-Han;Lee, Sung-Eun
    • Korean Journal of Environmental Biology
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    • v.36 no.3
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    • pp.345-351
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    • 2018
  • An efficient, quick and low-cost extraction and clean up method for the determination of 14 polycyclic aromatic hydrocarbons (PAHs) in the agricultural water samples was optimized using gas chromatography-tandem mass spectrometry (GC-MS/MS). The extraction of the target compounds in water sample was carried out with acetonitrile, followed by partitioning promoted by the addition of salt. As a clean-up procedure, dispersive solid phase extraction was employed to purify the analytes of interest for GC-MS/MS analysis. This method was successfully applied for the quantification of PAHs in real water samples collected for the purpose of monitoring from the waterways located in Chungbuk (15 sites) and Gyeongbuk (6 sites), S. Korea. Phenanthrene (0.54 to $2.53{\mu}gL^{-1}$) was detected in all the water samples collected from both the sites. Fluoranthene was detected in the water samples collected from the two sites in Gyeongbuk province, but other PAHs were not determined in these water sampling sites. Based on these results, the determined PAHs were conducted using an environmental risk assessment. The risk characterization ratios (RCRs) for phenanthrene ranged from 0.37 to 3.21. These RCR values referred to as risk was not controlled because RCR values of some sites were greater than 1. In conclusion, it is proposed that the optimized method in combination with GC-MS/MS could be successfully employed for the determination of PAHs in any environmental samples including water samples.