• Title/Summary/Keyword: Stability Linear Analysis

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Development and Validation of an HPLC Method for the Pharmacokinetic Study of Pentoxifylline in Human Serum (체내동태 연구를 위한 혈청 중 펜톡시필린의 HPLC 정량법 개발 및 검증)

  • Cho, Hea-Young;Kang, Hyun-Ah;Yoo, Hee-Doo;Lee, Hwa-Jeong;Moon, Jai-Dong;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
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    • v.36 no.2
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    • pp.89-95
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    • 2006
  • A selective and sensitive reversed-phase HPLC method for the determination of pentoxifylline in human serum was developed, validated, and applied to the pharmacokinetic study of pentoxifylline. Pentoxifylline and internal standard, chloramphenicol, were extracted from the serum by liquid-liquid extraction with dichloromethane and analyzed on a Luna CI8(2) column with the mobile phase of acetonitrile-0.034 M phosphoric acid (25:75, v/v, adjusted to pH 4.0 with 10 M NaOH). Detection wavelength of 273 nm and flow rate of 0.8 mL/min were used. This method showed linear response over the concentration range of 10-500 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of the serum was 10 ng/mL, which was sensitive enough for pharmacokinetic studies of pentoxifylline. The overall accuracy of the quality control samples ranged from 89.3 to 92.7% for pentoxifylline with overall precision (% C.V.) being 4.1-9.2%. The relative mean recovery of pentoxifylline for human serum was 105.8%. Stability (stock solution, short and long-term) studies showed that pentoxifylline was not stable during storage. But three freeze-thaw cycles and extracted serum samples were stable. This method showed good ruggedness (within 15% C.V.) and was successfully applied for the analysis of pentoxifylline in human serum samples for the pharmacokinetic studies of orally administered $Trental^{\circledR}$ tablet (400 mg pentoxifylline), demonstrating the suitability of the method.

Development and Validation of an HPLC Method for the Pharmacokinetic Study of Dipyridamole in Human (디피리다몰 체내동태 연구를 위한 혈청 중 디피리다몰의 HPLC 정량법 개발 및 검증)

  • Cho, Hea-Young;Kang, Hyun-Ah;Moon, Jae-Dong;Choi, Hoo-Kyun;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
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    • v.36 no.1
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    • pp.45-51
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    • 2006
  • A rapid, selective and sensitive reversed-phase HPLC method for the determination of dipyridamole in human serum was developed, validated, and applied to the pharmacokinetic study of dipyridamole. Dipyridamole and internal standard, loxapine, were extracted from human serum by liquid-liquid extraction with diethyl ether and analyzed on a Nova Pak $C_{I8}$ column with the mobile phase of 40 mM ammonium acetate:methanol:acetonitrile (35:35:30)(v/v/v, pH 7.8). Detection wavelength of 280 nm and flow rate of 1.0 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^3$ factorial design using a fixed dipyridamole concentration (50 ng/mL) with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 2-2000 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of serum was 2 ng/mL, which was sensitive enough for pharmacokinetic studies of dipyridamole. The overall accuracy of the quality control samples ranged from 103.94 to 105.86% for dipyridamole with overall precision (% C.V.) being 4.60-11.49%. The relative mean recovery of dipyridamole for human serum was 97.64%. Stability studies showed that dipyridamole was stable during storage, or during the assay procedure in human serum. The peak area and retention time of dipyridamole were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of dipyridamole in human serum samples for the pharmacokinetic studies of orally administered Dimor tablet (75 mg as dipyridamole) at three different laboratories, demonstrating the suitability of the method.

Development and Validation of HPLC Method for Pharmacokinetic Study of Promethazine in Human (염산프로메타진 체내동태 연구를 위한 혈청 중 프로메타진의 HPLC 정량법 개발 및 검증)

  • Cho, Hae-Young;Kang, Hyun-Ah;Lee, Hwa-Jeong;Choi, Hoo-Kyun;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
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    • v.36 no.1
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    • pp.23-29
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    • 2006
  • A rapid, selective and sensitive reversed-phase HPLC method for the determination of promethazine in human serum was developed, validated, and applied to the pharmacokinetic study of promethazine. Promethazine and internal standard, chlorpromazine, were extracted from human serum by liquid-liquid extraction with n-hexane containing 0.8% isopropanol and analyzed on a Capcell Pak CN column with the mobile phase of acetonitrile-0.2 M potassium dihydrogen phosphate (42:58, v/v, adjusted to pH 6.0 with 1 M NaOH). Detection wavelength of 251 nm and flow rate of 0.9 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^{3}$ factorial design using a fixed promethazine concentration (10 ng/mL) with respect to its peak area and retention time. In addition, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 1-40 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 1 mL of serum was 1 ng/mL, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the quality control samples ranged from 96.15 to 105.40% for promethazine with overall precision (% C.V.) being 6.70-11.22%. The relative mean recovery of promethazine for human serum was 63.54%. Stability (freeze-thaw and short-term) studies showed that promethazine was stable during storage, or during the assay procedure in human serum. However, the storage at $-80^{\circ}C$ for 4 weeks showed that promethazine was not stable. Extracted serum sample and stock solution were not allowed to stand at ambient temperature for 12 hr prior to injection. The peak area and retention time of promethazine were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of promethazine in human serum samples for the pharmacokinetic studies of orally administered Himazin tablet (25 mg as promethazine hydrochloride) at three different laboratories, demonstrating the suitability of the method.

Validated HPLC Method for the Pharmacokinetic Study of Atenolol and Chlorthalidone Combination Therapy in Korean Subjects

  • Kang, Hyun-Ah;Kim, Hwan-Ho;Kim, Se-Mi;Yoon, Hwa;Cho, Hea-Young;Oh, Seaung-Youl;Choi, Hoo-Kyun;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
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    • v.36 no.5
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    • pp.331-338
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    • 2006
  • A rapid, selective and sensitive reverse-phase HPLC methods for the determination of atenolol and chlorthalidone in human serum and whole blood were validated, and applied to the pharmacokinetic study of atenolol and chlorthalidone combination therapy. Atenolol and an internal standard, pindolol, were extracted from human serum by liquid-liquid extraction, and analyzed on a $\mu$-Bondapak C18 $10-{\mu}$ column in a mobile phase of methanol-0.01 M potassium dihydrogenphosphate(30:70, v/v, adjusted to pH 3.5) and fluorescence detection(emission: 300 nm, excitation: 224 nm). Chlorthalidone and an internal standard, probenecid, were extracted form human whole blood by liquid-liquid extraction, and analyzed on a Luna C18 $5-{\mu}$ column in a mobile phase of acetonitrile containing 77% 0.01 M sodium acetate and UV detection at 214 nm. These analysis were performed at three different laboratories using the same quality control(QC) samples. The chromatograms showed good resolution, sensitivity, and no interference by human serum and whole blood, respectively. The methods showed linear responses over a concentration range of 10-1,000 ng/mL for atenolol and 0.05-20 ${\mu}g/mL$ for chlorthalidone, with correlation coefficients of greater than 0.999 at all the three laboratories. Intra- and inter-day assay precision and accuracy fulfilled international requirements. Stability studies(freeze-thaw, short-, long-term, extracted sample and stock solution) showed that atenolol and chlorthalidone were stable. The lower limit of quantitation of atenolol and chlorthalidone were 10 ng/mL and 0.05 ${\mu}g/mL$, respectively, which was sensitive enough for pharmacokinetic studies. These methods were applied to the pharmacokinetic study of atenolol and chlorthalidone in human volunteers following a single oral administration of Hyundai $Tenoretic^{\circledR}$ tablet(atenolol 50 mg and chlorthalidone 12.5 mg) at three different laboratories.

Construction of Correlation between Basic Soil Properties and Deformation Modulus of Trackbed Soils Based on Laboratory and Field Mechanical Tests (역학적 실내외 시험에 의한 철도궤도 상부노반용 흙재료의 기본물성과 변형계수 상관성 평가)

  • Park, Jae Beom;Choi, Chan Yong;Ji, Sang Hyun;Lim, Sang Jin;Lim, Yu Jin
    • Journal of the Korean Society for Railway
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    • v.19 no.2
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    • pp.204-212
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    • 2016
  • The soils used as trackbed in Korea are selected using USCS utilizing basic soil properties such as Grain Size Distribution(GSD), % passing of #200 sieve ($P_{200}$), % passing of #4 sieve ($P_4$), Coefficient of uniformity ($C_u$), and Coefficient of curvature ($C_c$). Degree of compaction of the soils adapted in the code by KR should be evaluated by maximum dry density (${\gamma}_{d-max}$) and deformation modulus $E_{v2}$. The most important influencing factor that is critical to stability and deformation of the compacted soils used as trackbed is stiffness. Thus, it is necessary to construct a correlation between the modulus and the basic soil properties of trackbed soil in order to redefine a new soil classification system adaptable only to railway construction. To construct the relationship, basic soil test data is collected as a database, including GSD, maximum dry unit weight (${\gamma}_{d-max}$), OMC, $P_{200}$, $P_4$, $C_u$, $C_c$, etc.; deformation modulus $E_{v2}$ and $E_{vd}$ are obtained independently by performing a Repeated Plated Bearing Test (RPBT) and Light Weight Deflectometer Test (LWDT) for ten different railway construction sites. A linear regression analysis is performed using SPSS to obtain the relationship between the basic soil properties and the deformation modulus $E_{v2}$ and $E_v$. Based on the constructed relationship and the various obtained mechanical test data, a new soil classification system will be proposed later as a guideline for the design and construction of trackbed foundation in Korea.

A Basic Study on Non-aqueous Electrolysis of Neodymium for Room-temperature Metallurgy (상온제련을 위한 네오디뮴의 비수계 전해 기초연구)

  • Park, Jesik;Lee, Churl Kyoung
    • Resources Recycling
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    • v.27 no.4
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    • pp.29-35
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    • 2018
  • In this study, the electrochemical redox behavior of neodymium in non-aqueous electrolytes was investigated to confirm the possibility of neodymium metallurgy at room temperature. The non-aqueous electrolytes include ionic liquids such as $[C_4mim]PF_6$, $[C_4mim]Cl$, and $[P_{66614}]PF_6$, ethanol which are highly soluble in neodymium salts, and mixed electrolytes based on carbonate with highly electrochemical stability. The electrochemical redox properties of neodymium were better than those of other electrolytes in the case of the mixed electrolyte based on ethylene carbonate (EC)/di-ethylene carbonate (DEC). Ethanol was added to improve the physical properties of the mixed electrolyte. Thorough the analysis about ionic conductivity of EC/DEC ratio, ethanol content and $NdCl_3$ concentration, the best electrolyte composition was 50 vol% content of ethanol and 0.5 M of $NdCl_3$. Using cyclic voltametry and linear sweep voltametry, a current peak estimated at -3.8 V (vs. Pt-QRE) was observed as a limiting current of neodymium reduction. Potentiostatic electrolysis for 18 hours at room temperature at -6 V (vs. Pt-QRE) confirmed that metallic neodymium was electrodeposited.

Comparative Analysis of Annual Tropospheric Delay by Season and Weather (계절과 날씨에 따른 연간 대류권 지연오차량 변화)

  • Lim, Soo-Hyeon;Kim, Ji-Won;Park, Jeong-Eun;Bae, Tae-Suk;Hong, Sungwook
    • Journal of the Korean Society of Surveying, Geodesy, Photogrammetry and Cartography
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    • v.37 no.1
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    • pp.1-7
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    • 2019
  • In this study, we estimated the tropospheric delay of GNSS (Global Navigation Satellite System) signals during passing through the atmosphere in relation to weather and seasonal factors. For this purpose, we chose four CORS (Continuously Operating Reference Station) stations from inland (CCHJ and PYCH) and on the coast (GEOM and CHJU). A total of 48 days for each station (one set of data for each week) were downloaded from the NGII (National Geographic Information Institute) and processed it using the scientific GNSS software. The average tropospheric delays in winter are less than 2,400 mm, which is about 200 mm less than those in summer. The estimated tropospheric delay shows a similar pattern from all stations except the absolute bias in magnitude, while a large delay was observed for the station located on the coast. In addition, the delay during the day was relatively stable in winter, and the average tropospheric delay was strongly related to the orthometric height. The inland stations have tropospheric delays by the precipitation rather than humidity due to dry weather and difference in temperature. On the contrary, it was primarily caused by the humidity on the sea. The correlation between temperature and water vapor pressure is 0.9 or larger for all stations, and the tropospheric delay showed a high linear relationship with temperature. It is necessary to analyze the GNSS data with higher temporal resolution (e.g. all RINEX data of the year) to improve the stability and reliability of the correlation results.

Estimation and Analysis of the Vertical Profile Parameters Using HeMOSU-1 Wind Data (HeMOSU-1 풍속자료를 이용한 연직 분포함수의 매개변수 추정 및 분석)

  • Ko, Dong-Hui;Cho, Hong-Yeon;Lee, Uk-Jae
    • Journal of Korean Society of Coastal and Ocean Engineers
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    • v.33 no.3
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    • pp.122-130
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    • 2021
  • A wind-speed estimation at the arbitrary elevations is key component for the design of the offshore wind energy structures and the computation of the wind-wave generation. However, the wind-speed estimation of the target elevation has been carried out by using the typical functions and their typical parameters, e.g., power and logarithmic functions because the available wind speed data is limited to the specific elevation, such as 2~3m, 10 m, and so on. In this study, the parameters of the vertical profile functions are estimated with optimal and analyzed the parameter ranges using the HeMOSU-1 platform wind data monitored at the eight different locations. The results show that the mean value of the exponent of the power function is 0.1, which is significantly lower than the typically recommended value, 0.14. The values of the exponent, the friction velocity, and the roughness parameters are in the ranges 0.0~0.3, 0~10 (m/s), and 0.0~1.0 (m), respectively. The parameter ranges differ from the typical ranges because the atmospheric stability condition is assumed as the neutral condition. To improve the estimation accuracy, the atmospheric condition should be considered, and a more general (non-linear) vertical profile functions should be introduced to fit the diverse profile patterns and parameters.

Free Vibration Analysis of Circular Arches Considering Effects of Midsurface Extension and Rotatory Inertia Using the Method of Differential Quadrature (미분구적법을 이용 중면신장 및 회전관성의 영향을 고려한 원형아치의 고유진동해석)

  • Kang, Ki-Jun
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.22 no.1
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    • pp.9-17
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    • 2021
  • Curved beams are increasingly used in buildings, vehicles, ships, and aircraft, which has resulted in considerable effort being directed toward developing an accurate method for analyzing the dynamic behavior of such structures. The stability behavior of elastic circular arches has been the subject of a large number of investigations. One of the efficient procedures for the solution of ordinary differential equations or partial differential equations is the differential quadrature method DQM. This method has been applied to a large number of cases to overcome the difficulties of the complex computer algorithms, as well as excessive use of storage due to conditions of non-linear geometries, loadings, or material properties. This study uses DQM to analyze the in-plane vibration of the circular arches considering the effects of midsurface extension and rotatory inertia. Fundamental frequency parameters are calculated for the member with various parameter ratios, boundary conditions, and opening angles. The solutions from DQM are compared with exact solutions or other numerical solutions for cases in which they are available and given to analyze the effects of midsurface extension and rotatory inertia on the frequency parameters of the circular arches.

Soil Depth Estimation and Prediction Model Correction for Mountain Slopes Using a Seismic Survey (탄성파 탐사를 활용한 산지사면 토심 추정 및 예측모델 보정)

  • Taeho Bong;Sangjun Im;Jung Il Seo;Dongyeob Kim;Joon Heo
    • Journal of Korean Society of Forest Science
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    • v.112 no.3
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    • pp.340-351
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    • 2023
  • Landslides are major natural geological hazards that cause enormous property damage and human casualties annually. The vulnerability of mountainous areas to landslides is further exacerbated by the impacts of climate change. Soil depth is a crucial parameter in landslide and debris flow analysis, and plays an important role in the evaluation of watershed hydrological processes that affect slope stability. An accurate method of estimating soil depth is to directly investigate the soil strata in the field. However, this requires significant amounts of time and money; thus, numerous models for predicting soil depth have been proposed. However, they still have limitations in terms of practicality and accuracy. In this study, 71 seismic survey results were collected from domestic mountainous areas to estimate soil depth on hill slopes. Soil depth was estimated on the basis of a shear wave velocity of 700 m/s, and a database was established for slope angle, elevation, and soil depth. Consequently, the statistical characteristics of soil depth were analyzed, and the correlations between slope angle and soil depth, and between elevation and soil depth were investigated. Moreover, various soil depth prediction models based on slope angle were investigated, and corrected linear and exponential soil depth prediction models were proposed.