• Title/Summary/Keyword: high range

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Simultaneous GC/MS Analyses of Organic acids and Amino acids in Urine using TMS-TFA derivative (TMS-TFA 유도체화를 이용한 소변여지 중 유기산과 아미노산의 GC/MS 동시분석)

  • Yoon, Hye-Ran
    • Analytical Science and Technology
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    • v.19 no.1
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    • pp.107-114
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    • 2006
  • Early diagnosis and medical intervention are critical for the treatment of patients with metabolic disorders. A rapid analytical method was developed for simultaneous quantification of organic acids and amino acids in urine without labor-intensive pre-extraction procedure showing high sensitivity and specificity. A new method consisted of simple two-step trimethylsilyl (TMS)-trifluoroacetyl (TFA) derivatization using GC/MS-selective ion monitoring (SIM). Filter paper urine specimens were dried under nitrogen after being fortified with internal standard (tropate) in a mixture of distilled water and methanol. Methyl orange was added to the residue as indicator reagent. Silyl derivative of carboxylic functional group was followed by trifluoroacetyl derivative for amino functional group. N-methyl-N-(trimethylsilyl-trifluoroacetamide) and N-methyl-bistrifluoroacetamide were consecutively added and heated for 15-20 min at $65^{\circ}C-70^{\circ}C$, for TMS-TFA derivative, respectively. This reactant was analyzed by GC/MS-SIM. Linear dynamic range showed 0.001-50 mg with the detection limit of (S/N=3) 10-200 ng, and the quantification limit of 80-900 ng in urine. Correlation coefficient of regression line was 0.994-0.998. When the method was applied to the patients 'urine, it clearly differentiated the normal from the patient with metabolic disorder. The study showed that the developed method could be the method of choices in rapid and sensitive screening for organic aciduria and amino acidopathy.

Planar microchip-based lactate biosensor (평면 소자형 락테이트 바이오센서)

  • Ha, Jeonghan;Huh, Hwang;Kang, Tae Young;Lee, Yong Seok;Yoon, Soon Ho;Shin, Jungwon;Nam, Hakhyun;Cha, Geun Sig
    • Analytical Science and Technology
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    • v.19 no.6
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    • pp.482-489
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    • 2006
  • Two electrode-based lactate biosensor was prepared by immobilizing lactate oxidase (LOD) obtained from pediococcus species in a poly(vinyl alcohol). Hydrogen peroxide ($H_2O_2$) produced by the reaction of lactate and LOD was detected on the Pt-black that was electrochemically deposited on the Au electrode. Sensors fabricated with Pt-black deposited Au electrode provided a high current of $H_2O_2$ oxidation at a substantially lowered applied potential (+300 mV vs. Ag/AgCl), resulting in reduced interferences from easily oxidizable species such as ascorbic acid, acetaminophen, and uric acid. An outer membrane is formulated by adjusting water uptake of hydrophilic polyurethane (HPU). The sensor performance was evaluated in vitro with both flow-through arrangement and static mode. The sensor showed a linear range from 0.1 mM to about 9.0 mM in 0.05 M phosphate buffer (pH 7.6) containing 0.05 M NaCl. Storing the sensors prepared in this work at $4^{\circ}C$ buffer solution while not in use, they provided same electrochemical performance for more than 25 days.

Oxidation behavior on the surface of titanium metal specimens at high temperatures (300~1000℃) (고온 (300~1000 ℃)에서 티타늄 금속시편의 표면 산화거동)

  • Park, Yang-Soon;Han, Sun-Ho;Song, Kyuseok
    • Analytical Science and Technology
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    • v.22 no.6
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    • pp.464-470
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    • 2009
  • For the investigation of the oxidation behavior for titanium metal at various temperatures, titanium specimens were heated for 2 hours in the range of $300{\sim}1000^{\circ}C$, individually. And then X-ray diffraction(XRD), scanning electron microscopy (SEM)/energy dispersive spectroscopy (EDS) and attenuated total reflection-Fourier transform infrared (ATR-FTIR) spectroscopic analyses were carried out. At $300^{\circ}C$, infrared absorption bands on the surface of the titanium specimen were shown in a spectrum by the oxygen uptake of titanium metal(hexagonal). At increased temperature, not only infrared absorption bands but also X-ray diffraction peaks for the titanium oxide were grown and shifted to low wave number ($cm^{-1}$) and angle($^{\circ}$) due to the more oxygen diffusion into titanium metal. At $700^{\circ}C$, $Ti_3O$ (hexagonal phase) was identified by X-ray diffractometer. $TiO_2$ (rutile, tetragonal phase) layer was produced on the surface of the specimen below $1{\mu}m$ in thickness at $600^{\circ}C$, and grown about $2{\mu}m$ at $700^{\circ}C$ and with $110{\mu}m$ in thickness at $1000^{\circ}C$. Above $900^{\circ}C$, (110) plane of the crystal on the surface of rutile-$TiO_2$ layer was grown.

Bioequivalence of pioglitazone tablet to Actos® tablet (Pioglitazone 30 mg) (액토스정®(피오글리타존 30 mg)에 대한 염산피오글리타존정의 생물학적동등성)

  • Yeom, Hyesun;Lee, Tae Ho;Youm, Jeong-Rok;Song, Jin-Ho;Han, Sang Beom
    • Analytical Science and Technology
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    • v.22 no.1
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    • pp.101-108
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    • 2009
  • The bioequivalence of two pioglitazone tablets, Actos$^{(R)}$ tablet (Takeda Chemical Industries, reference drug) and Pioglitazone tablet (Boryung Company, test drug) was evaluated according to the guidelines of Korea Food and Drug Administration. Twenty-eight healthy male Korean volunteers received each medicine (pioglitazone dose of 30 mg) in a $2{\times}2$ crossover study with one week washout interval. After drug administration, blood samples were collected at specific time intervals from 0-36 hours. The plasma concentrations of pioglitazone were determined by high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). The total chromatographic run time was 5 min and calibration curves were linear over the concentration range of 5-2000 ng/mL for pioglitazone. The method was validated for selectivity, sensitivity, linearity, accuracy and precision. The pharmacokinetic parameters were determined from the plasma concentration-time profiles of both formulations. The primary calculated pharmacokinetic parameters were compared statistically to evaluate bioequivalence between the two preparations. The 90% confidence intervals of the $AUC_t$ ratio and the $C_{max}$ ratio for Pioglitazone tablet and Actos$^{(R)}$ tablet were log0.9422~log1.1040 and log0.9200~log1.1556, respectively. Based on the statistical considerations, we can conclude that the test drug, Pioglitazone tablet was bioequivalent to the reference drug, Actos$^{(R)}$ tablet.

Compositions and pollution characteristics of total suspended particles (TSP) at 1100 Site of Mt. Halla (한라산 1100 고지 총부유분진(TSP)의 조성 및 오염 특성)

  • Kim, Won-Hyung;Kang, Chang-Hee;Jung, Duk-Sang;Go, Hui-Jeong;Lee, Won
    • Analytical Science and Technology
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    • v.21 no.4
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    • pp.304-315
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    • 2008
  • The total suspended particles (TSP) collected at the 1100 site of Mt. Halla have shown higher compositions for the anthropogenic components followed by marine and soil originated ones. The concentrations of the soil originated nss-$Ca^{2+}$, Al, Fe, Ca components have been increased in spring, and the anthropogenic $NH{_4}^+$, $K^+$, nss-$SO{_4}^{2-}$ components showed high concentrations in June. Meanwhile, the concentration of $NO{_3}^-$ as same as nss-$Ca^{2+}$ was higher in spring. It's likely due to the influence of its long-range transport from China. Compared to the non-Asian Dust periods, the concentrations of nss-$Ca^{2+}$, Al, Ca, and Fe have been increased 7.2~9.5 times in Asian Dust storm periods, and those of nss-$SO{_4}^{2-}$ and $NO{_3}^-$ were 1.3 and 3.8 times, respectively. From the factor analysis, the TSP compositions were influenced mainly by anthropogenic emission sources, followed by oceanic and soil sources. The backward trajectory analysis has shown that the concentrations of the anthropogenic and soil components were increased when the air parcels had been moved into Jeju island via China in a northwesterly wind.

Qunatitative analysis of liquiritin and glycyrrhizin in glycyrrhizae radix by HPLC-MS/MS (HPLC-MS/MS에 의한 감초의 liquiritin과 glycyrrhizin의 분석)

  • Yu, Young-Beob;Kim, Mi-Jung;Huang, Dae Sun;Ha, Hye-Kyeong;Ma, Jin-Yeul;Shin, Hyeun-Kyoo
    • Analytical Science and Technology
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    • v.20 no.4
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    • pp.331-338
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    • 2007
  • Licorice, Glycyrrhizae Radix is widely used as a herbal medicines and a dietary supplements in East Asia. We employed high performance liquid chromatography electrospray ionization tandem mass spectrometry to determine liquiritin and glycyrrhizin in the Glycyrrhizae Radix. Liquiritin and glycyrrhizin in Glycyrrhizae Radix were ionized by positive ion pneumatically assisted electrospray and detected by HPLC-MS/MS in the multiple-reaction monitoring (MRM) mode using precursor ${\rightarrow}$ product ion combinations at m/z $436.2{\rightarrow}257.0$ and $823.4{\rightarrow}453.4$, respectively. The assay had a calibration range from 10 to 3,000 ng/mL. The limits of detection (LOD) of the liquiritin and glycyrrhizin were 0.4 ng/mL and 0.01 ng/mL, respectively. The reproducibility and repeatability (relative standard deviation) at different analyte concentrations varied from 103 to 113 % and 0.95 to 1.8 %, respectively. According to the above results, HPLC-MS/MS method permits assignment of tentative structures such as liquiritin and glycyrrhizin in the Glycyrrhizae Radix.

Study on Changes of Street Furniture in Digital Environment (디지털 환경에서 가로시설물의 변화에 관한 연구)

  • In, Chiho;Kim, Hyunsoo
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.28 no.1D
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    • pp.129-136
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    • 2008
  • Along with the development in cutting-edge digital technology, the street space is also being changed. Mobile telecommunication units and internet give a big change in a human being's lifestyle. And the ubiquitous computing is proceeding with expanding its application range from the indoor space to the street space. As the street furniture is the convenient facility that allows a human being's life in street space to be abundant, it is getting advanced. First of all, in terms of such phenomenon, this study analyzed the cases of a research on application of street space and the actual condition of a change in the number of individuals for the street furniture, through a literature research of ubiquitous. Also, it researched into the realities of using the street furniture of the walking-desired streets at Daehac-ro and Hongdae district, where are two representative places related to digital generation. The next was carried out FGI (Focus Group Interview) with users of the street space in front of Hongik University and managers of the street furniture, and was researched into the use & management behavior, and recognition level on the street furniture. Thus, the key elements were extracted such as interchange of information for cultural activities, automation for interaction variability in function. Finally the core elements for future vision of street furniture in this digital era were extracted in 3I, namely, Information, Intellectualization, and Integration. This is considered to be applied to the establishment of direction in the process of high-tech digitalization in street furniture related to information hereafter.

Target Reliability Indices of Static Design Methods for Driven Steel Pipe Piles in Korea (국내 항타강관말뚝 설계법의 목표 신뢰도지수)

  • Kwak, Kiseok;Huh, Jungwon;Kim, Kyung Jun;Park, Jae Hyun;Lee, Juhyung
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.28 no.1C
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    • pp.19-29
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    • 2008
  • As a part of study to develop LRFD (Load and Resistance Factor Design) codes for foundation structures in Korea, reliability analyses for driven steel pipe piles are performed and the target reliability indices are selected carefully. The 58 data sets of static load tests and soil property tests conducted in the whole domestic area were collected and analyzed to determine the representative bearing capacities of the piles. The static bearing capacity formula and the Meyerhof method using N values are applied to calculate the expected design bearing capacity of the piles. The resistance bias factors were evaluated for the two static design methods by comparing the representative bearing capacities with the design values. Reliability analysis was performed by two types of advanced methods: First Order Reliability Method (FORM), and Monte Carlo Simulation (MCS) method using resistance bias factor statistics. The static bearing capacity formula exhibited relatively small variation, whereas the Meyerhof method showed relatively high inherent conservatism in the resistance bias factors. Reliability indices for safety factors in the range of 3 to 5 were evaluated respectively as 1.50~2.89 and 1.61~2.72 for both of the static bearing capacity formula and the Meyerhof method. The target reliability indices are selected as 2.0 and 2.33 for group pile case and 2.5 for single pile case, based on the reliability level of the current design practice and considering redundancy of pile group, acceptable risk level, construction quality control, and significance of individual structure.

Pseudo-DC Resistivity Survey for Site Investigation at Urban Areas with Ambient Electrical Noises (전기잡음 간섭이 있는 도심지 지역 탐사를 위한 유사직류 전기비저항 기법)

  • Joh, Sung-Ho;Kim, Bong-Chan
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.30 no.1C
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    • pp.37-44
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    • 2010
  • Recently, urban retrofit and extension, development of new buildings and facilities, and construction of underground structures like subway tunnels in urban areas give rise to significance of site investigation at urban areas. However, ambient electric noises, traffic vibrations, embedded objects work as obstacles to high-quality and accuracy in site investigation at urban areas. In this paper, a new technique called the pseudo-DC resistivity survey (in brief, PDC-R) was proposed to minimize the adverse effect of ambient electrical noises in resistivity survey. PDC-R technique utilizes an AC current with frequency range of 0.1 to 1.0 Hz rather than DC current, which is used for conventional resistivity survey. The motivation of using low-frequency AC current is to avoid 60-Hz components or its multiples in the resistivity survey which ambient noises are mostly composed of. The implementation of PDC-R technique also included the parametric study on skin effect, frequency effect and current-level effect, which led to the determination of optimal values of frequency and current level for PDC-R survey. The reliability and feasibility of PDC-R technique was verified through field tests, accompanied by the comparison with DC resistivity survey and CapSASW tests.

Properties on the Strength of Polymer Concrete Using Nano MMT-UP Composite (나노 MMT-폴리머 복합체를 이용한 폴리머 콘크리트의 강도 특성)

  • Jo, Byung-Wan;Moon, Rin-Gon;Park, Seung-Kook
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.26 no.4A
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    • pp.761-766
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    • 2006
  • Polymer composite are increasingly considered as structural components for use in civil engineering, on account of their enhanced strength-to-weight ratios. Unsaturated polyester (UP) resin have been widely used for the matrix of composites such as FRP and polymer composite, due to its excellent adhesive. Polymer nanocomposites are new class of composites derived from the nano scale inorganic particles with dimensions typically in the range of 1 to 1000 nm that are dispersed in the polymer matrix homogeneously. Owing to the high aspect ratio of the fillers, mechanical, thermal, flame, retardant and barrier properties are enhanced without significant loss of clarity, toughness or impact strength. To prepare the MMT (Montmorillonite)-UP exfoliated nanocomposites, UP was mixed with MMT at $60^{\circ}C$ for 3 hours by using pan mixer. XRD (X-ray diffraction) pattern of the composites and TEM (Transmission Electron Micrographs) showed that the interlayer spacing of the modified MMT were exfoliated in polymer matrix. The mechanical properties also supported these findings, since in general, tensile strength, modulus with modified MMT were higher than those of the composites with unmodified MMT. The thermal stability of MMT-UP nanocomposite is better than that of pure UP, and its glass transition temperature is higher than that of pure UP. The polymer concrete made with MMT-UP nanocomposite has better mechanical properties than of pure UP. Therefore, it is suggested that strength and elastic modulus of polymer concrete was found to be positively tensile strength and tensile modulus of the MMT-UP nanocomposites.