• Title/Summary/Keyword: Analytical validation

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A semi-analytical mesh-free method for 3D free vibration analysis of bi-directional FGP circular structures subjected to temperature variation

  • Shamshirsaz, Mahnaz;Sharafi, Shahin;Rahmatian, Javad;Rahmatian, Sajad;Sepehry, Naserodin
    • Structural Engineering and Mechanics
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    • v.73 no.4
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    • pp.407-426
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    • 2020
  • In this present paper, a semi-analytical mesh-free method is employed for the three-dimensional free vibration analysis of a bi-directional functionally graded piezoelectric circular structure. The dependent variables have been expanded by Fourier series with respect to the circumferential direction and have been discretized through radial and axial directions based on the mesh-free shape function. The current approach has a distinct advantage. The nonlinear Green-Lagrange strain is employed as the relationship between strain and displacement fields to observe thermal impacts in stiffness matrices. Nevertheless, high order terms have been neglected at the final steps of equations driving. The material properties are assumed to vary continuously in both radial and axial directions simultaneously in accordance with a power law distribution. The convergence and validation studies are conducted by comparing our proposed solution with available published results to investigate the accuracy and efficiency of our approach. After the validation study, a parametric study is undertaken to investigate the temperature effects, different types of polarization, mechanical and electric boundary conditions and geometry parameters of structures on the natural frequencies of functionally graded piezoelectric circular structures.

Development and validation of a qualitative GC-MS method for methamphetamine and amphetamine in human urine using aqueous-phase ethyl chloroformate derivatization

  • Kim, Jiwoo;Sim, Yeong Eun;Kim, Jin Young
    • Analytical Science and Technology
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    • v.33 no.1
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    • pp.23-32
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    • 2020
  • Methamphetamine (MA) is the most common and available drug of abuse in Korea and its primary metabolite is amphetamine (AP). Detection of AP derivatives, such as MA, AP, phentermine (PT), MDA, MDMA, and MDEA by the use of immunoassay screening is not reliable and accurate due to cross-reactivity and insufficient specificity/sensitivity. Therefore, the analytical process accepted by most urine drug-testing programs employs the two-step method with an initial screening test followed by a more specific confirmatory test if the specimen screens positive. In this study, a gas chromatography-mass spectrometric (GC-MS) method was developed and validated for confirmation of MA and AP in human urine. Urine sample (500 µL) was added with N-isopropylbenzylamine as internal standard and ethyl chloroformate as a derivatization reagent, and then extracted with 200 µL of ethyl acetate. Extracted samples were analysed with GC-MS in the SIM/ Scan mode, which were screened by Cobas c311 analyzer (Roche/Hitachi) to evaluate the efficiency as well as the compatibility of the GC-MS method. Qualitative method validation requirements for selectivity, limit of detection (LOD), precision, accuracy, and specificity/sensitivity were examined. These parameters were estimated on the basis of the most intense and characteristic ions in mass spectra of target compounds. Precision and accuracy were less than 5.2 % (RSD) and ±14.0 % (bias), respectively. The LODs were 3 ng/mL for MA and 1.5 ng/mL for AP. At the screening immunoassay had a sensitivity of 100% and a specificity of 95.1 % versus GC-MS for confirmatory testing. The applicability of the method was tested by the analysis of spiked urine and abusers' urine samples.

Quantitative Analysis of Kynurenic Acid in Chestnut Honey from Different Regions and Method Validation (산지별 밤꿀에 함유된 Kynurenic Acid의 정량 분석과 분석법 검증)

  • Kim, Juree;Kim, Doyun;Lee, Sanghyun
    • Korean Journal of Pharmacognosy
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    • v.53 no.2
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    • pp.111-118
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    • 2022
  • Chestnut honey is a sweet dark-colored honey with a distinct bitter aftertaste. It contains numerous phenolic compounds and alkaloids and is noted for its antioxidant and anti-inflammatory activities. However, it has been established that there are differences in the composition and activity of chestnut honey constituents depending on the region of origin, the sources of which warrant further research. In this study, we analyzed the kynurenic acid (KA) contents in chestnut honey produced in nine different regions in Korea, using high-performance liquid chromatography in conjunction with ultraviolet detection, and validated the analytical method developed. Use of a reverse-phase column and detection at a wavelength of 240 nm were found to be optimal for the detection of KA. Similar evaluation of an optimal method for extracting KA from chestnut honey revealed that extraction using 10% EtOH at 20 times the sample volume over a 6 h period was the most suitable for obtaining a high content of KA. Among the nine regional chestnut honeys assessed, KA content was found to be highest in the "Gongju" sample (1.14 mg/g), followed by that in the "Cheongdo" and "Damyang" samples. Validation of the KA analytical method revealed a good analyte linearity, with a correlation coefficient (r2) of 0.9995, an accuracy of between 92.37% and 107.35%, and good precision (RSD ≤ 1.05%). Our findings in this study, based on a validated quantitative analytical method for KA, could make an important contribution to establishing a data profiling procedure for characterizing chestnut honeys produced in different regions, and may also provide basic data for the identification of functional honey.

Full validation of high-throughput bioanalytical method for the new drug in plasma by LC-MS/MS and its applicability to toxicokinetic analysis

  • Han, Sang-Beom
    • Proceedings of the Korean Society of Toxicology Conference
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    • 2006.11a
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    • pp.65-74
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    • 2006
  • Modem drug discovery requires rapid pharmacokinetic evaluation of chemically diverse compounds for early candidate selection. This demands the development of analytical methods that offer high-throughput of samples. Naturally, liquid chromatography / tandem mass spectrometry (LC-MS/MS) is choice of the analytical method because of its superior sensitivity and selectivity. As a result of the short analysis time(typically 3-5min) by LC-MS/MS, sample preparation has become the rate- determining step in the whole analytical cycle. Consequently tremendous efforts are being made to speed up and automate this step. In a typical automated 96-well SPE(solid-phase extraction) procedure, plasma samples are transferred to the 96-well SPE plate, internal standard and aqueous buffer solutions are added and then vacuum is applied using the robotic liquid handling system. It takes only 20-90 min to process 96 samples by automated SPE and the analyst is physically occupied for only approximately 10 min. Recently, the ultra-high flow rate liquid chromatography (turbulent-flow chromatography)has sparked a huge interest for rapid and direct quantitation of drugs in plasma. There is no sample preparation except for sample aliquotting, internal standard addition and centrifugation. This type of analysis is achieved by using a small diameter column with a large particle size(30-5O ${\mu}$m) and a high flow rate, typically between 3-5 ml/min. Silica-based monolithic HPLC columns contain a novel chromatographic support in which the traditional particulate packing has been replaced with a single, continuous network (monolith) of pcrous silica. The main advantage of such a network is decreased backpressure due to macropores (2 ${\mu}$m) throughout the network. This allows high flow rates, and hence fast analyses that are unattainable with traditional particulate columns. The reduction of particle diameter in HPLC results in increased column efficiency. use of small particles (<2 urn), however, requires p.essu.es beyond the traditional 6,000 psi of conventional pumping devices. Instrumental development in recent years has resulted in pumping devices capable of handling the requirements of columns packed with small particles. The staggered parallel HPLC system consists of four fully independent binary HPLC pumps, a modified auto sampler, and a series of switching and selector valves all controlled by a single computer program. The system improves sample throughput without sacrificing chromatographic separation or data quality. Sample throughput can be increased nearly four-fold without requiring significant changes in current analytical procedures. The process of Bioanalytical Method Validation is required by the FDA to assess and verify the performance of a chronlatographic method prior to its application in sample analysis. The validation should address the selectivity, linearity, accuracy, precision and stability of the method. This presentation will provide all overview of the work required to accomplish a full validation and show how a chromatographic method is suitable for toxirokinetic sample analysis. A liquid chromatography/tandem mass spectrometry (LC-MS/MS) method developed to quantitate drug levels in dog plasma will be used as an example of tile process.

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An Analytical Model for FRP Debonding in Strengthened RC Beams under Monotonic and Cyclic Loads

  • Moein, Reza Saeidi;Tasnimi, Abbas Ali
    • International Journal of Concrete Structures and Materials
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    • v.10 no.4
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    • pp.499-511
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    • 2016
  • Reinforced concrete (RC) beams strengthened by externally bonded reinforcement often fail by debonding. This paper presents an experimental and analytical study aimed at better understanding and modeling the fiber reinforced polymer (FRP) debonding failures in strengthened RC beams under monotonic and cyclic loads. In order to investigate the flexural behavior and failure modes of FRP-strengthened beams under monotonic and cyclic loadings, an experimental program was carried out. An analytical study based on the energy balance of the system was also performed. It considers the dominant mechanisms of energy dissipation during debonding and predicts the failure load of the strengthened beams. Validation of the model was carried out using test data obtained from the own experimental investigation.

Deflection of battened beams with shear and discrete effects

  • Li, Ji-liang;Chen, Jian-kang
    • Structural Engineering and Mechanics
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    • v.59 no.5
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    • pp.921-932
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    • 2016
  • This paper presents a theoretical analysis for determining the transverse deflection of simply supported battened beams subjected to a uniformly distributed transverse quasi-static load. The analysis considers not only the shear effect but also the discrete effect of battens on the transverse deflection of the battened beam. The analytical solution is obtained using the principle of minimum potential energy. Numerical validation of the present analytical solution is accomplished using finite element methods. The present analytical solution shows that the shear effect on the transverse deflection of battened beams increases with the cross-section area of the main member but decreases with the cross-section area of the batten. The longer the battened beam is, or the larger the moment of inertia of the main member is, the smaller the shear effect will be.

HPLC analytical method validation of Aralia elata extract as a functional ingredients (두릅 추출물의 기능성 원료 표준화를 위한 HPLC 분석법 검증)

  • Ahn, Eun-Mi;Choi, Song-Am;Choi, Ji-Young
    • Food Science and Preservation
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    • v.24 no.6
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    • pp.795-801
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    • 2017
  • Aralia elata Seemann (AE) has long been used as a folk medicine for the treatment of various diseases including diabetes mellitus, anti-arthritic, and anti-gastric ulcer agent in Korea, Japan, and China. This study was performed to establish a simple and reliable HPLC/UV analytical method for determination of most active anti-hypertensive compound, a 3-O-${\alpha}$-L-rhamnopyranosyl($1{\rightarrow}$2)-${\alpha}$-L-arabinopyranosyl hederagenin 28-O-${\beta}$-D-xylopyranosyl($1{\rightarrow}6$)-${\beta}$-D-glucopyranosylester (HE) for the standardization of the shoot extract of AE as a health functional food ingredient. The quantitative analytical method of HE was optimized by HPLC analysis using reverse-phase C18 column at $40^{\circ}C$ with $H_2O$ and acetonitrile (70:30, v/v) as an isocratic mobile phase at a flow rate of 1.0 mL/min and detection wavelength of UV 205 nm. This HPLC/UV analytical method showed good specificity and high linearity in the tested range of 0.03125-2.0mg/ml with excellent coefficient of determination ($R^2$) of 0.9999. The limit of detection and limit of quantification were $12.0{\mu}g/mL$ and $36.5{\mu}g/mL$, respectively. Relative standard deviation (RSD) values of data from intra- and inter-day precision were less than 0.2% and 0.1%, respectively. These results indicate that the established HPLC/UV analytical method is very simple, specific, precise, accurate, and reproducible and thus can be useful for the quantitative analysis of HE as a functional anti-hypertensive compound in AE extract.

New Method for Measurement and Validation of In-situ Sound Transmission Loss (In-situ 소음투과손실 측정 및 검증을 위한 기법 개발)

  • Lee, Hwa-Soo;Park, Hong-Cheol;Yoon, Seong-Ho
    • Proceedings of the Korean Society for Noise and Vibration Engineering Conference
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    • 2008.04a
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    • pp.795-800
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    • 2008
  • The sound transmission loss is a key index to evaluate the acoustic performance of a car-body structure at the high frequency range. From this paper, a new validation method for in-situ sound transmission loss is proposed. First, in-situ sound transmission loss is measured by using PU intensity probe on the condition of complete vehicle. Second, validation test, which is consisted of internal, external and total frequency response function test, is performed by using volume acceleration source and microphones. Then, these test results are compared to validate the accuracy of in-situ sound transmission loss. Finally, the test result of in-site method is compared with results of two reverberant room test method and SEA analytical method. The reliability of in-situ method is confirmed by these procedures.

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Parity Space and Pattern Recognition Approach for Hardware Redundant System Signal Validation using Artificial Neural Networks (인공신경망을 이용하여 하드웨어 다중 센서 신호 검증을 위한 패리티 공간 및 패턴인식 방법)

  • 윤태섭
    • Journal of Institute of Control, Robotics and Systems
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    • v.4 no.6
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    • pp.765-771
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    • 1998
  • An artificial neural network(NN) technique is developed for hardware redundant sensor validation. Since the measurement space is a continuous space with many operating regions, it is difficult to train a NN to correctly detect failure in an accurate measurement system. A conventional backpropagation NN is modified to include an additional preprocessing layer that extracts classification features from scalar measurements. This feature extraction means transform the measurement space to parity space. The NN is independent of the state variable being measured, the instrument range, and the signal tolerance. This NN resembles the parity space approach to signal validation, except that analytical parity equations are unneeded and the NN pattern recognition capability is utilized for decision making.

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