• Title/Summary/Keyword: Sample matrix

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Characterization of Korean Archaeological Artifacts by Neutron Activation Analysis (II). Multivariate Classification of Korean Ancient Glass Pieces (중성자 방사화분석에 의한 한국산 고고학적 유물의 특성화 연구 (II). 다변량 해석법에 의한 고대 유리제품의 분류 연구)

  • Chul Lee;Oh Cheun Kwun;Ihn Chong Lee;Nak Bae Kim
    • Journal of the Korean Chemical Society
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    • v.31 no.6
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    • pp.567-575
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    • 1987
  • Fourty five ancient Korean glass pieces have been determined for 19 elements such as Ag, As, Br, Ce, Co, Cr, Eu, Fe, Hf, K, La, Lu, Na, Ru, Sb, Sc, Sm, Th and Zn, and for one such as Pb by instrumental neutron activation analysis and by atomic absorption spectrometry, respectively. The multivariate data have been analyzed for the relation among elemental contents through the variance-covariance matrix. The data have been further analyzed by a principal component mapping method. As the results training set of 5 class have been chosen, based on the spread of sample points in an eigen vector plot and archaeological data. The 5 training set consisting of 36 species and a test set consisting of 9 species bave finally been analyzed for the assignment to certain classes or outliers through the statistical isolinear multiple component analysis (SIMCA). The results have showed the whole species for 5 training set and 3 species in the test set are assigned appropriately and these are in accord with the results by principal component mapping.

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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.

HPLC Determination and Steady-State Bioavailability Study of Levodropropizine Sustained-release Tablets in Dogs

  • Yan, Lin;Li, Tongling;Zhang, Rongqin;Xu, Xiaohong;Zheng, Pengcheng
    • Archives of Pharmacal Research
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    • v.29 no.6
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    • pp.514-519
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    • 2006
  • A simple HPLC method using UV detection was developed and validated for the determination of levodropropizine (LDP) In dog plasma. The sample was prepared for injection using a liquid-liquid extraction method with 1-phenypiperazine as the internal standard. The mobile phase was methanol - diethylamine solution (0.05 M) (20:80, v/v, pH adjusted to 3.0 with $H_3PO_4$) with a detection wavelength of 240 nm. The limit of quantitation (LOQ) of LDP in a biological matrix was determined to be 25.25 ng/mL. The calibration curve was linear across the concentration range of 25.25 to 2020 ng/mL. The intra-day and inter-day precision values (CV%) were within 7% and accuracy (R.E. %) was within 6% of the nominal values for medium (252.5 ng/mL) and high (2020 ng/mL) LDP concentrations. For the LDP concentration at the LOQ, the intra-day and inter-day precision and accuracy were within 20% and 10%, respectively. The average absolute recovery for LDP was 70.28%. This method was successfully used to analyze plasma samples in a steady-state bioavailability study of a newly developed sustained-release LDP tablets (SR) using immediate-release tablets (IR) as the reference. The relative bioavailability of the SR was determined to be $106.3\;{\pm}\;12.8%$ (n=6). The $C_{max}$ of the SR was significantly lower (p<0.05), and the $t_{max}$ was significantly longer than that of the IR (p<0.05). The results of ANOVA and two one-sided tests indicated that the SR exhibited acceptable sustained release properties and was bioequivalent to the IR.

Effect of Excess PbO on Grain Growth and Densification of (65)Pb(${Mg_{1/3}}{Nb_{2/3}}$)$O_3$-(35)$PbTiO_3$ Ceramics ((65)Pb(${Mg_{1/3}}{Nb_{2/3}}$)$O_3$-(35)$PbTiO_3$의 입자성장과 치밀화에 미치는 과량 PbO의 영향)

  • Lee, Jong-Bong;Hur, Tae-Moo;Lee, Ho-Yong;Choi, Kyun;Kim, Doe-Yeon
    • Journal of the Korean Ceramic Society
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    • v.37 no.7
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    • pp.673-680
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    • 2000
  • The effect of excess PbO(0, 1, 2, 4, and 8 mol%) on grain growth and densification of (65)Pb(Mg1/3Nb2/3)O3-(35)PbTiO3 [mol%] ceramics has been investigaetd. With increasing the amount of excess PbO and sintering time, densities of sintered samples decreased gradually. The samples containing less than 1 mol% of PbO showed normal grain growth behavior, however abnormal grain growth was observed to occur in the samples with more than 2 mol% of PbO. In the samples with more than 2 mol% of PbO, the number of abnormal grains decreased and thus the average grain size became smaller with increasing the amount of excess PbO. These results demonstrated that the abnormal grain growth started to occur when a critical amount of excess PbO was added to a (65)Pb(Mg1/3Nb2/3)O3-(35)PbTiO3 sample. Since PMN-PT grains in a liquid matrix were angular, the observed abnormal grain growth was explained to proceed through the two dimensional nucleation process.

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A Study on the Fabrication of p-type poly-Si Thin Film Transistor (TFT) Using Sequential Lateral Solidification(SLS) (SLS 공정을 이용한 p-type poly-Si TFT 제작에 관한 연구)

  • Lee, Yun-Jae;Park, Jeong-Ho;Kim, Dong-Hwan
    • The Transactions of the Korean Institute of Electrical Engineers C
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    • v.51 no.6
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    • pp.229-235
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    • 2002
  • This paper presents the fabrication of polycrystalline thin film transistor(TFT) using sequential lateral solidification(SLS) of amorphous silicon. The fabricated SLS TFT showed high Performance suitable for active matrix liquid crystal display(AMLCD). The SLS process involves (1) a complete melting of selected area via irradiation through a patterned mask, and (2) a precisely controlled pulse translation of the sample with respect to the mask over a distance shorter than the super lateral growth(SLG) distance so that lateral growth extended over a number of iterative steps. The SLS experiment was performed with 550$\AA$ a-Si using 308nm XeCl laser having $2\mu\textrm{m}$ width. Irradiated laser energy density is 310mJ/$\textrm{cm}^2$ and pulse duration time was 25ns. The translation distance was 0.6$\mu$m/pulse, 0.8$\mu$m/pulse respectively. As a result, a directly solidified grain was obtained. Thin film transistors (TFTs) were fabricated on the poly-Si film made by SLS process. The characteristics of fabricated SLS p -type poly-Si TFT device with 2$\mu\textrm{m}$ channel width and 2$\mu\textrm{m}$ channel length showed the mobility of 115.5$\textrm{cm}^2$/V.s, the threshold voltage of -1.78V, subthreshold slope of 0.29V/dec, $I_{off}$ current of 7$\times$10$^{-l4}$A at $V_{DS}$ =-0.1V and $I_{on}$ / $I_{off}$ ratio of 2.4$\times$10$^{7}$ at $V_{DS}$ =-0.1V. As a result, SLS TFT showed superior characteristics to conventional poly-Si TFTs with identical geometry.y.y.y.

Sensitive Determination of Pinaverium Bromide in Human Plasma by LC-ESI-MS/MS : Applicability to Oral Bioavailability Determination (LC-ESI-MS/MS를 이용한 생체시료 중 브롬화피나베리움의 고감도 분석 및 이를 이용한 생체이용률 평가)

  • Park, Seok;Lee, Ye-Rie;Kim, Ho-Hyun;Lee, Hee-Joo;Kim, Yoon-Gyoon;Youm, Jeong-Rok;Han, Sang-Beom
    • Journal of Pharmaceutical Investigation
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    • v.34 no.6
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    • pp.513-519
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    • 2004
  • A sensitive method for quantification of pinaverium bromide in human plasma was established using liquid chromatography-electrospray ionization tandem mass spectrometry(LC-ESI-MS/MS). Glimepiride was used as internal standard. Pinaverium bromide and internal standard in plasma sample were extracted using tert-butylmethylether(TBME). A centrifuged upper layer was then evaporated and reconstituted with mobile phase of acetonitrile-5 mM ammonium formate (80/20, pH 3.0). The reconstituted samples were injected into a $C_{18}$ reversed-phase column. Using MS/MS with multiple reaction monitoring (MRM) mode, pinaverium and glimepirde were detected without severe interference from human plasma matrix. Pinaverium produced a protonated precursor ion $([M+H]^+)$ at m/z 510.3 and a corresponding product ion at m/z 228.9. Internal standard produced a protonated precursor ion $([M+H]^+)$ at m/z 491.5 and a corresponding product ion at m/z 352.0. Detection of pinaverium bromide in human plasma was accurate and precise, with limit of quantitation at 0.5 ng/ml. The method has been successfully applied to bioavailability study of pinaverium bromide tablet in Korean healthy male volunteers. Pharmacokinetic parameters such as $AUC_t,\;C_{max},\;T_{max},\;K_{el}\;and\;t_{1/2}$ were calculated.

Simultaneous Analysis of Conazole Fungicides in Garlic by Q-TOF Mass Spectrometer Coupled with a Modified QuEChERS Method

  • Bong, Min-Sun;Yang, Si-Young;Lee, Seung-Ho;Seo, Jung-Mi;Kim, In-Seon
    • Korean Journal of Environmental Agriculture
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    • v.30 no.3
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    • pp.323-329
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    • 2011
  • BACKGROUND: The conazoles, difenoconazole, diniconazole, hexaconazole, penconazole and tetraconazole are a large class of synthetic fungicides used extensively for foliage and seed treatments in agricultural crops. The extensive use of conazoles has brought concerns on the potentiality of environmental contamination and toxicity. Thus studies on the development of methods for monitoring the conazoles are required. METHODS AND RESULTS: A modified quick, easy, effective, rugged and safe (QuEChERS) method was involved in sample preparation. Quadrapole time of flight mass spectrometer (Q-TOF MS) in electron spray ionization (ESI) mode was employed to determine conazoles in garlic samples. The limit of detection (LOD) and limit of quantification (LOQ) of conazoles by Q-TOF-MS ranged from 0.001 to 0.002 mg/L and 0.002 to 0.005 mg/L, respectively. Q-TOF-MS analysis exhibited less than 2.6 ppm error of accurate mass measurements for the detection of conazoles spiked at 0.05 mg/L in garlic matrix. Recovery values of conazoles fortified in garlic samples at 0.02, 0.05 and 0.1 mg/L were between 79.2 and 106.2% with a maximum 11.8% of standard deviation. No detectable conazoles were found in the domestic market samples by using the Q-TOF-MS method. CONCLUSION(s): High degree of confirmation for conazoles by accurate mass measurements demonstrated that Q-TOF-MS analysis combined with a QuEChERS method may be applicable to simultaneous determination of conazoles in garlic samples.

Determination of trace actinide (Am, Pu, Th, U) using alpha spectrometry and neutron activation analysis (알파분광법과 중성자방사화분석법에 의한 극미량의 악티늄계원소 (Am, Pu, Th, U)분석연구)

  • Yoon, Yoon Yeol;Lee, Kil Yong;Cho, Soo Young;Kim, Yongjai;Lee, Myong Ho
    • Analytical Science and Technology
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    • v.17 no.4
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    • pp.302-307
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    • 2004
  • Determination of actinides in the environmental sample requires separation of each element. This procedure is tedious and time consuming. And also, the detection limits of some nuclides using alpha spectrometry are rather higher. To overcome the lower detection limit and complicated separation procedure, a simple analytical technique for the determination of actinide isotopes in the environmental samples was developed and applied to IAEA and NIST reference sediment samples. For the separation of actinides from matrix, anion exchange resin and TRU-spec extraction chromatography resin were used and chemical yields were obtained using natural uranium, thorium, $^{242}Pu$ and $^{243}Am$ tracers. For overcoming the higher detection limits of U and Th in alpha spectrometry, neutron activation analysis was applied. Using combined method, the detection limit was increased about 10 times. The activity values of each isotope were consistent with the reference values reported by IAEA and NIST.

Measurement uncertainty for QC/QA applied to the chemical analysis (화학 분석 결과의 QA/QC를 위한 측정 불확도)

  • Woo, Jin-Chun;Oh, Sang-Hyub;Kim, Byoung-Moon;Bae, Hyun-Kil;Kim, Kwang-Sub;Kim, Young-Doo
    • Analytical Science and Technology
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    • v.18 no.6
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    • pp.475-482
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    • 2005
  • The expression of uncertainty applied to the chemical analysis is highly recommended with increasing demands upon the systematic quality assurance and control(QA/QC) with ISO 17025. For the quantification of quality source, 7 major common sources of uncertainty, normally contributing to the quality of the chemical analysis, were selected from QA/QC literatures of chemical analysis. They were classified into repeatability, drift, uncertainty in standards, linearity of calibration, homogeneity, stability of sample, and matrix effect. And, the quantification of the sources by means of measurement uncertainty was proposed as a prerequisite steps for QA/QC. Examples applied to the quantification procedures of modelling, combination and expression of standard uncertainty for the 7 major common sources were presented as a reference guide for QA/QC in chemical analysis.

Development of the Planar Active Phased Array Radar System with Real-time Adaptive Beamforming and Signal Processing (실시간으로 적응빔형성 및 신호처리를 수행하는 평면능동위상배열 레이더 시스템 개발)

  • Kim, Kwan Sung;Lee, Min Joon;Jung, Chang Sik;Yeom, Dong Jin
    • Journal of the Korea Institute of Military Science and Technology
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    • v.15 no.6
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    • pp.812-819
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    • 2012
  • Interference and jamming are becoming increasing concern to a radar system nowdays. AESA(Active Electronically Steered Array) antennas and adaptive beamforming(ABF), in which antenna beam patterns can be modified to reject the interference, offer a potential solution to overcome the problems encountered. In this paper, we've developed a planar active phased array radar system, in which ABF, target detection and tracking algorithm operate in real-time. For the high output power and the low noise figure of the antenna, we've designed the S-band TRMs based on GaN HEMT. For real-time processing, we've used wavelenth division multiplexing technique on fiber optic communication which enables rapid data communication between the antenna and the signal processor. Also, we've implemented the HW and SW architecture of Real-time Signal Processor(RSP) for adaptive beamforming that uses SMI(Sample Matrix Inversion) technique based on MVDR(Minimum Variance Distortionless Response). The performance of this radar system has been verified by near-field and far-field tests.