• Title/Summary/Keyword: preparation technique

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Determination of Non-Steroidal Anti-Inflammatory Drugs in Human Urine Sample using HPLC/UV and Three Phase Hollow Fiber-Liquid Phase Microextraction (HF-LPME)

  • Cha, Yong Byoung;Myung, Seung-Woon
    • Bulletin of the Korean Chemical Society
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    • v.34 no.11
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    • pp.3444-3450
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    • 2013
  • Three phase hollow fiber-liquid phase microextraction (HF-LPME), which is faster, simpler and uses a more environmentally friendly sample-preparation technique, was developed for the analysis of Non-Steroidal Anti-Inflammatory Drugs (NSAIDs) in human urine. For the effective simultaneous extraction/concentration of NSAIDs by three phase HF-LPME, parameters (such as extraction organic solvent, pH of donor/acceptor phase, stirring speed, salting-out effect, sample temperature, and extraction time) which influence the extraction efficiency were optimized. NSAIDs were extracted and concentrated from 4 mL of aqueous solution at pH 3 (donor phase) into dihexyl ether immobilized in the wall pores of a porous hollow fiber, and then extracted into the acceptor phase at pH 13 located in the lumen of the hollow fiber. After the extraction, 5 ${\mu}L$ of the acceptor phase was directly injected into the HPLC/UV system. Simultaneous chromatographic separation of seven NSAIDs was achieved on an Eclipse XDB-C18 (4.6 mm i.d. ${\times}$ 150 mm length, 5 ${\mu}m$ particle size) column using isocratic elution with 0.1% formic acid and methanol (30:70) at a HPLC-UV/Vis system. Under optimized conditions (extraction solvent, dihexyl ether; $pH_{donor}$, 3; $pH_{acceptor}$, 13; stirring speed, 1500 rpm; NaCl salt, 10%; sample temperature, $60^{\circ}C$; and extraction time, 45 min), enrichment factors (EF) were between 59 and 260. The limit of detection (LOD) and limit of quantitation (LOQ) in the spiked urine matrix were in the concentration range of 5-15 ng/mL and 15-45 ng/mL, respectively. The relative recovery and precision obtained were between 58 and 136% and below 15.7% RSD, respectively. The calibration curve was linear within the range of 0.015-0.96 ng/mL with the square of the correlation coefficient being more than 0.997. The established method can be used to analyse of NSAIDs of low concentration (ng/mL) in urine.

Cobalt(III) Complex of Ethylenediamine-N,N'-di-${\alpha}$-Isobutyric Acid (Ethylenediamine-N,N'-di-${\alpha}$-Isobutyric Acid의 코발트(III) 착물)

  • Moo-Jin Jun;Chang-Yoon Han;Chang-Woo Park;Sung Rack Choi;Kwang-Ha Park
    • Journal of the Korean Chemical Society
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    • v.30 no.1
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    • pp.84-89
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    • 1986
  • A newflexible $N_2O_2$-type tetradentate ligand. Ethylenediamine-N,N'-di-${\alpha}$-isobutyric acid(eddib), has been synthesized, and dichloro cobalt(III) complex of eddib has been prepared via the air-oxidation technique. Only S-cis isomer has been yielded during the preparation of complex. Ring strain and steric hinderance are cited as the cause for the preference for the S-cis geometric configuration. On series of cobalt(III) complexes of eddib, $[Co(eddib)L]^{n+}$ $(L = Cl{\cdot}(H_2O),\;CO_3^{2-},\;(H_2O)_2)$have been prepared in situ. In their electronic absorption spectra, the absorption maxima and their intensities of the above series of complexes are on the ordinary line of the spectrochemical and hyperchromic series. Elemental analysis, IR, NMR and electronic absorption spectra have been used to characterize the complex and geometries of the complex.

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Application of Separation Technology and Supercritical Fluids Process (초임계유체 공정과 분리기술의 응용)

  • Yoon, Soon-Do;Byun, Hun-Soo
    • Clean Technology
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    • v.18 no.2
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    • pp.123-143
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    • 2012
  • Supercritical fluid technology (SFT) is recently one of the most new techniques, which has been interested various fields of related chemical industries. SFT is the most effective and practical technology with eco-friendly, energy-savings, and high efficiency as the technique using the advantages of supercritical fluid such as high solvation power, solubility, mass transfer rate, and diffusion rate. Especially, it is necessary to analyze, evaluate, and develop the potential of application techniques using SFT with these characterizations. Therefore in this review, the phase behavior in supercritical fluid at high temperature and pressure of monomers/polymers for the optimization of polymerization process are briefly described, and the preparation of molecularly imprinted polymers (MIPs) in supercritical fluid using supercritical polymerization and the performance evaluation of MIPs are introduced.

Preparation of Magnetic Chitosan Microsphere Particles (나노 크기의 마그네타이트 입자를 이용한 자성 키토산 미소구체의 제조)

  • Ko, Sang-Gil;Cho, Jun-Hee;Ahn, Yang-Kyu;Song, Ki-Chang;Choi, Eun-Jung
    • Journal of the Korean Magnetics Society
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    • v.16 no.1
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    • pp.66-70
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    • 2006
  • Magnetite nanoparticles, which have been extensively used in many fields, were encapsulated with a natural polymer, chitosan, to improve their biocompatibility. We have synthesized magnetite $(Fe_3C_4)$ nanoparticles using chemical coprecipitation technique with sodium oleate as surfactant. Nanoparticle size can be varied from 1.2 to 7.4nm by controlling the sodium oleate concentration. Magnetite phase nanoparticles could be observed from X-ray diffraction. Magnetic colloid suspensions containing particles with sodium oleate and chitosan have been prepared. High magnetic property chitosan-microsphere particles were prepared from oleate-coated magnetite suspension using spray method. The surftce, and tile morphology of the magnetic chitosan microsphere particles were characterized using optical microscope and scanning electron microscope. Magnetic hysteresis measurement were performed using a superconducting quantum interference device (SQUID) magnetometer at room temperature to investigate the magnetic properties of the chitosan microspheres including magnetite nanoparticles. The SQUID measurements revealed superparamagnetism of nanoparticles.

Preparation and Characterization of Antioxidant Peptides from Fermented Goat Placenta

  • Hou, Yinchen;Zhou, Jiejing;Liu, Wangwang;Cheng, Yongxia;Wu, Li;Yang, Gongming
    • Food Science of Animal Resources
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    • v.34 no.6
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    • pp.769-776
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    • 2014
  • The goat placenta was fermented by Bacillus subtilis and the optimal fermentation parameters of strongest antioxidant capacity of peptides were obtained using response surface methodology (RSM). The effects of fermentation time, initial pH value and glucose content on the 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging capacity of the goat peptides were well fitted to a quadric equation with high determination coefficients. According to the data analysis of design expert, the strongest DPPH radical scavenging capacity value was obtained with the following conditions: content of glucose was 2.23%, initial pH value was 7.00 and fermentation time was 32.15 h. The DPPH radical scavenging capacity commonly referring antioxidant activity showed a concentration dependency and increased with increasing peptide concentration. The effects of temperature and pH were assessed to determine the stability of antioxidant peptides prepared from goat placenta. Antioxidant peptides showed good stabilities when temperature was lower than $70^{\circ}C$. However, the antioxidant peptides lost antioxidant activities rapidly under alkaline and excessive acid condition. Ultrafiltration technique was performed to separate fermentation broth with different Mw (molecular weight). It was found that peptides in the range of < 3 KDa mainly accounted for the antioxidant activities.

Preparation of Gel Polymer Electrolyte Membranes of Polyvinyl Alcohol and Poly (acrylic acid) for Zn Air Batteries (아연공기전지를 위한 Polyvinyl Alcohol과 Poly (acrylic acid)의 블랜드를 이용한 겔 고분자 전해질막의 제조)

  • Kim, Chanhoon;Koo, Ja-Kyung
    • Membrane Journal
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    • v.22 no.3
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    • pp.208-215
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    • 2012
  • Gel polymer electrolyte membranes were prepared from blends of polyvinyl alcohol (PVA) and poly (acrylic acid) (PAA), by solution-cast technique. The PAA content in the blend varied from 30 to 80 wt%. With the gel polymer electrolyte membranes, Zn air batteries were fabricated. The gel polymer electrolyte membranes were characterized by means of stress-strain test, impedance test. The Zn air batteries were tested by current interrupt method and galvanostatic discharge method. The tensile strength and tensile modulus decreased with increasing PAA content in the gel polymer electrolyte membrane. On the other hand, the ionic conductivity increased with increasing PAA content. The effect of ionic conductivity trend of the gel polymer electrolyte membrane in the Zn air battery was confirmed through current interrupt method and galvanostatic discharge method experiments. The battery with higher PAA content gel polymer electrolyte membrane showed lower IR drop and higher discharge capacity.

Preparation and characterization of nanoporous monolith with high thermal insulation performance (나노 기공성 단열 실리카 모노리스 제조 및 특성 연구)

  • Choi, Hyun-Muk;Kim, Seong-Woo
    • Journal of the Korean Applied Science and Technology
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    • v.31 no.1
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    • pp.83-91
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    • 2014
  • In this study, we synthesized two different silica monoliths by using sol-gel, solvent exchange, surface modification, ambient pressure drying processes, and surfactant-based templating technique followed by calcination process. All of the prepared two silica monoliths showed crack-free appearance with fairly good transparency, and furthermore were confirmed to have extremely high porosity, specific surface area, and mean pore size below 30 nm. The silica aerogel sample exhibited finer and more homogeneous nano-sized pore structure due to spring back effect caused by surface modification, which resulted in better thermal insulation performance. Based on measured thermal conductivities and theoretical relationship, multi-layered glass window system in which silica monolith prepared in this study was inserted as a middle layer was revealed to have superior thermal insulation performance compared to conventional air-inserted glass window system.

A STUDY ON THE SHAPE OF A CANAL PREPARED WITH PROFILES IN A CURVED CANAL (PROFILE을 이용한 만곡 근관 형성시 근관의 형태에 관한 연구)

  • Park, Han-Soo;Lee, Min-Koo;Kim, Jong-Jin;Lee, Jong-Yeop
    • Restorative Dentistry and Endodontics
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    • v.24 no.4
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    • pp.633-638
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    • 1999
  • The purpose of our study is to evaluate the ability of nickel-titanium(NiTi) files in maintaining the original curvature of a curved root canal during canal preparation. Curved canals on translucent resin blocks were prepared with Profiles and stainless steel files and they were placed at the platform which can reproduce the same position. The unprepared and prepared canal forms were accurately compared by double exposure technique of photography. The results were as follows : 1 NiTi files made a canal comparatively taper, but stainless steel files didn't make a canal taper, wicest at midportion and comparatively wide at a apical portion. 2. Canals preparations with no. 25 Profile.06 up to the working length were most excellent in taperness and in maintaining the original curvature. Canals prepared with no 30 Profile.06 up to the working length made a little outer transportation at a apical portion, but not severe. 3. Canal preparations with Profile GT were excellent in taperness and in maintaining the original curvature, but made more enlargement toward the inner side at the starting portion of the curvature. 4. Canal preparations with stainless steel files were not tapered and provided the largest transportation.

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Comparison between the liquid-liquid partition method and modified QuEChERS method for the analysis of pesticide residues in beef fat (소지방 중 잔류농약분석을 위한 액-액분배법과 modified QuEChERS법 비교)

  • Kim, Yoen-Joo;Choi, Yoon-Hwa;Shin, Bang-Woo;Lee, Jung-Hark
    • Korean Journal of Veterinary Service
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    • v.34 no.4
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    • pp.429-439
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    • 2011
  • This article described the comparison of a quick, easy, cheap, effective, rugged and safe (QuEChERS) sample preparation and the classical method established by National Veterinary Research and Quarantine Service (NVRQS) for the determination of pesticide residues in livestock products using GC-tandem mass spectrometry. The classical method by NVRQS used liquid-liquid partioning followed by evaporizing. The modified QuEChERS entailed extraction of 2 g sample with 15 ml acetonitrile containing 1% acetic acid followed by addition of 6 g anhydrous magnesium sulfate and 1.5 g sodium acetate. After centrifugation, 6 ml of the extract underwent a cleanup step (in a technique known as column-based solid phase extraction) using 400 mg each of $C_{18}$ and primary secondary amine sorbents plus 1,200 mg magnesium sulfate. The quantitation of individual pesticides by both methods was based on tissue standard calibration curves with a correlation coefficient in excess of 0.98 for the 24 pesticides. The detection limits by the classical method were ranged 1.3~5.0 ${\mu}g$/kg, with mean recoveries between 76.2% and 114.3% except aldrin (59.3%) and deltamethrin (63.6%). The detection limits by modified QuEChERS were ranged 0.3~6.2 ${\mu}g$/kg, with mean recoveries between 68.0% and 114.3% except dimethipin (152.6%), chlorfenvinphos (138.1%), 4,4-DDT (61.5%), aldrin (60.4%) and chinomethionate (30.3%).

Preparation and characterization of water-soluble polyaniline/carbon nanotube composites (수용성 폴리아닐린/탄소나노튜브 복합재료의 제조 및 물성분석)

  • Lee, Jea-Uk;Jo, Won-Ho;Lee, Won-Oh;Byun, Joon-Hyung
    • Composites Research
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    • v.24 no.6
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    • pp.1-6
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    • 2011
  • A new water-soluble and self-doped poly(styrenesulfonic acid-graft-aniline), PSSA-g-PANI, for dispersing carbon nanotubes (CNTs) in water was synthesized and its ability to stabilize aqueous CNT dispersions was examined. It was observed that the PANI in PSSA-g-PANI, which has benzoid and quinoid structure, was strongly adsorbed onto the nanotube surface via a strong ${\pi}-{\pi}$ interaction, and thus only gentle sonication causes exfoliation of CNT ropes to small bundles and the long-term stability of their resulting dispersions was much better than commercial surfactants. Furthermore, when thin films of PSSA-g-PANI/CNT are prepared from aqueous dispersion and their electrical conductivities are measured by the four probe technique, it is observed that their conductivities are in the range of 1.5-2.5 S/cm.