• Title/Summary/Keyword: Liquid-Solid Flow

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Simultaneous determinations of anthracycline antibiotics by high performance liquid chromatography coupled with radial-flow electrochemical cell (고성능 액체 크로마토그래피/방사흐름 전기화학전지를 이용한 안트라사이클린계 항생제의 동시 정량)

  • Cho, Yonghee;Hahn, Younghee
    • Analytical Science and Technology
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    • v.20 no.4
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    • pp.308-314
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    • 2007
  • The analytical method of HPLC with the radial-flow electrochemical cell (RFEC) has been developed to determine doxorubicin, epirubicin, nogalamycin, daunorubicin and idarubicin simultaneously by employing a reversed-phase chromatography. Anthracyclines were detected at -0.74 V vs. a Ag/AgCl (0.01 M NaCl) reference electrode, a potential of diffusion current plateau in the mobile phase. At a $V_f$ of 1.0 mL/min doxorubicin, epirubicin, daunorubicin and idarubicin appeared at a retention time ($t_r$) of 6.4 min, 7.4 min, 12.7 min and 18.4 min, respectively, while at a $V_f$ of 0.6 mL/min, doxorubicin, epirubicin, nogalamycin, daunorubicin and idarubicin appeared at a $t_r$ of 9.9 min, 11.5 min, 13.5 min, 19.6 min and 28.7 min, respectively. The linearity between each anthracycline injected ($2.40{\times}10^{-7}M{\sim}1.42{\times}10^{-5}M$) and peak area (charge) was excellent with the square of the correlation coefficient ($R^2$) higher than 0.999. The detection limits were $1.0{\times}10^{-8}M{\sim}1.5{\times}10^{-7}M$ for the five anthracyclines. Within-day precision for the five anthracyclines were in reasonable relative standard deviations less than 3 % ($1.00{\times}10^{-6}M{\sim}1.42{\times}10^{-5}M$) except the lower concentrations less than $0.7{\mu}M$. Solid phase extractions of $1.00{\times}10^{-5}M$ epirubicin, $0.48{\times}10^{-5}M$ nogalamycin and $1.52{\times}10^{-5}M$ daunorubicin from human serum with a $C_{18}$ cartridge resulted in 97 %, 100 % and 90 % of recoveries, respectively.

Simultaneous Determination of Penicillin Antibiotics in Meat using Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS를 이용한 육류 중 페니실린계 항생제 8종의 동시분석 및 적용성 검증)

  • Kim, Myeong-Ae;Yoon, Su-Jin;Kim, MeeKyung;Cho, Yoon-Jae;Choi, Sun-Ju;Chang, Moon-Ik;Lee, Sang-Mok;Kim, Hee-Jeong;Jeong, Jiyoon;Rhee, Gyu-Seek;Lee, Sang-Jae
    • Journal of Food Hygiene and Safety
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    • v.29 no.2
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    • pp.131-140
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    • 2014
  • The objective of this study was to develop a simultaneous method of 8 penicillin antibiotics including amoxicillin, ampicillin, cloxacillin, dicloxacillin, nafcillin, oxacillin, penicillin G and penicillin V in meat using LC-MS/MS. The procedure involves solid phase extraction with HLB cartridge and subsequent analysis by LC-MS/MS. To optimize MS analytical condition of 8 compounds, each parameter was established by multiple reaction monitoring in positive ion mode. The chromatographic separation was achieved on a $C_{18}$ column with a mobile phase of 0.05% formic acid and 0.05% formic acid in acetonitrile at a flow rate of 0.2 mL/min for 20 min with a gradient elution. The developed method was validated for specificity, linearity, accuracy and precision in beef, pork and chicken. The recoveries were 71.0~106%, and relative standard deviations (RSD) were 4.0~11.2%. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.003~0.008 mg/kg and 0.01~0.03 mg/kg, respectively, that are below maximum residue limit (MRL) of the penicillins. This study also performed survey of residual penicillin antibiotics for 193 samples of beef, pork and chicken collected from 9 cities in Korea. Penicillins were not found in all the samples except a sample of pork which contained cloxacillin (concentration of 0.08 mg/kg) below the MRL (0.3 mg/kg).

A Rheological Study on Creep Behavior of Clays (점토(粘土)의 Creep 거동(擧動)에 관한 유변학적(流變學的) 연구(研究))

  • Lee, Chong Kue;Chung, In Joon
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.1 no.1
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    • pp.53-68
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    • 1981
  • Most clays under sustained load exhibit time-dependent deformation because of creep movement of soil particles and many investigators have attempted to relate their findings to the creep behavior of natural ground and to the long-term stability of slopes. Since the creep behavior of clays may assume a variety of forms depending on such factors as soil plasticity, activity and water content, it is difficult and complicated to analyse the creep behavior of clays. Rheological models composed of linear springs in combination with linear or nonlinear dashpots and sliders, are generally used for the mathematical description of the time-dependent behavior of soils. Most rheological models, however, have been proposed to simulate the behavior of secondary compression for saturated clays and few definitive data exist that can evaluate the behavior of non-saturated clays under the action of sustained stress. The clays change gradually from a solid state through plastic state to a liquid state with increasing water content, therefore, the rheological models also change. On the other hand, creep is time-dependent, and also the effect of thixotropy is time-function. Consequently, there may be certain correlations between creep behavior and the effects of thixotropy in compacted clays. In addition, the states of clay depend on water content and hence the height of the specimen under drained conditions. Futhermore, based on present and past studies, because immediate elastic deformation occurs instantly after the pressure increment without time-delayed behavior, the factor representing immediate elastic deformations in the rheological model is necessary. The investigation described in this paper, based on rheological model, is designed to identify the immediate elastic deformations and the effects of thixotropy and height of clay specimens with varing water content and stress level on creep deformations. For these purposes, the uniaxial drain-type creep tests were performed. Test results and data for three compacted clays have shown that a linear top spring is needed to account for immediate elastic deformations in the rheological model, and at lower water content below the visco-plastic limit, the effects of thixotropy and height of clay specimens can be represented by the proposed rheological model not considering the effects. Therefore, the rheological model does not necessitate the other factors representing these effects. On the other hand, at water content higher than the visco-plastic limit, although the state behavior of clays is visco-plastic or viscous flow at the beginning of the test, the state behavior, in the case of the lower height sample, does not represent the same behavior during the process of the test, because of rapid drainage. In these cases, the rheological model does not coincide with the model in the case of the higher specimens.

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