• Title/Summary/Keyword: Instrument Accuracy

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Development and Validation of the Determination of Sorafenib in Human Plasma using Tandem Mass Spectrometry Coupled with Liquid Chromatography (고속액체크로마토그래피 텐덤질량분석기법을 이용한 사람 혈장 내 소라페닙 농도분석법의 개발 및 검정)

  • Park, Daejin;Lee, Sunggon;Kim, Woomi
    • Journal of Life Science
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    • v.22 no.11
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    • pp.1456-1462
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    • 2012
  • Sorafenib is a multikinase inhibitor and an oral anticancer drug approved for the treatment of patients with advanced renal cell carcinoma and those with unresectable hepatocellular carcinoma. The purpose of this study was to develop an efficient method of the determination of sorafenib in human plasma using tandem mass spectrometry coupled with liquid chromatography (LC/MS/MS) and validate the method by the guidelines of the Korean Food and Drug Administration (KFDA). Plasma samples ($100{\mu}l$) were added with chlorantraniliprole as an internal standard and then mixed with the 0.1% formic acid-containing extraction solution composed of isopropyl alcohol and ethyl acetate (1:4, v/v). After centrifugation, the supernatant was concentrated at $45^{\circ}C$ under negative pressure and centrifugal force. The residue was reconstituted with a mobile phase and injected into the HPLC instrument using a reverse phase Waters XTerra$^{TM}$ C18 column (particle size $3.5{\mu}m$). Liquid chromatography was carried out within the run time of 5 min using a mobile phase composed of buffer (0.1% formic acid and 10 mM ammonium formate), methanol, and acetonitrile (1:6:3, v/v/v). The analytes were monitored by tandem mass spectrometry in the multiple reaction monitoring method programmed to detect sorafenib at 'm/z 465.2 ${\rightarrow}$ 252.5' and chlorantraniliprole at 'm/z 484.4 ${\rightarrow}$ 286.2' with positive electrospray ionization mode ($ES^+$). The result showed the proper linearity ($r^2$ > 0.99) over the range of 2,000-5,000 ng/ml with good accuracy (90.7-103.9%) and precision (less than 10%). The newly developed method using LC/MS/MS was validated by the guideline of KFDA and identified as more sensitive compared to the previous methods.

EVALUATING THE RELIABILITY AND REPEATABILITY OF THE DIGITAL COLOR ANALYSIS SYSTEM FOR DENTISTRY (치과용 디지털 색상 분석용 기기의 정확성과 재현 능력에 대한 평가)

  • Jeong, Joong-Jae;Park, Su-Jung;Cho, Hyun-Gu;Hwang, Yun-Chan;Oh, Won-Mann;Hwang, In-Nam
    • Restorative Dentistry and Endodontics
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    • v.33 no.4
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    • pp.352-368
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    • 2008
  • This study was done to evaluate the reliability of the digital color analysis system (ShadeScan, CYNOVAD, Montreal. Canada) for dentistry. Sixteen tooth models were made by injecting the A2 shade chemical cured resin for temporary crown into the impression acquired from 16 adults. Surfaces of the model teeth were polished with resin polishing cloth. The window of the ShadeScan handpiece was placed on the labial surface of tooth and tooth images were captured, and each tooth shade was analyzed with the ShadeScan software. Captured images were selected in groups, and compared one another. Two models were selected to evaluate repeatability of ShadeScan, and shade analysis was performed 10 times for each tooth. And, to ascertain the color difference of same shade code analyzed by ShadeScan, CIE $L^*a^*b^*$values of shade guide of Gradia Direct (GC, Tokyo, Japan) were measured on the white and black background using the Spectrolino (GretagMacbeth, USA), and Shade map of each shade guide was captured using the ShadeScan. There were no teeth that were analyzed as A2 shade and unique shade. And shade mapping analyses of the same tooth revealed similar shade and distribution except incisal third. Color difference (${\Delta}E^*$) among the Shade map which analyzed as same shade by ShadeScan were above 3. Within the limits of this study, digital color analysis instrument for dentistry has relatively high repeatability, but has controversial in accuracy.

Measurement and Quality Control of MIROS Wave Radar Data at Dokdo (독도 MIROS Wave Radar를 이용한 파랑관측 및 품질관리)

  • Jun, Hyunjung;Min, Yongchim;Jeong, Jin-Yong;Do, Kideok
    • Journal of Korean Society of Coastal and Ocean Engineers
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    • v.32 no.2
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    • pp.135-145
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    • 2020
  • Wave observation is widely used to direct observation method for observing the water surface elevation using wave buoy or pressure gauge and remote-sensing wave observation method. The wave buoy and pressure gauge can produce high-quality wave data but have disadvantages of the high risk of damage and loss of the instrument, and high maintenance cost in the offshore area. On the other hand, remote observation method such as radar is easy to maintain by installing the equipment on the land, but the accuracy is somewhat lower than the direct observation method. This study investigates the data quality of MIROS Wave and Current Radar (MWR) installed at Dokdo and improve the data quality of remote wave observation data using the wave buoy (CWB) observation data operated by the Korea Meteorological Administration. We applied and developed the three types of wave data quality control; 1) the combined use (Optimal Filter) of the filter designed by MIROS (Reduce Noise Frequency, Phillips Check, Energy Level Check), 2) Spike Test Algorithm (Spike Test) developed by OOI (Ocean Observatories Initiative) and 3) a new filter (H-Ts QC) using the significant wave height-period relationship. As a result, the wave observation data of MWR using three quality control have some reliability about the significant wave height. On the other hand, there are still some errors in the significant wave period, so improvements are required. Also, since the wave observation data of MWR is different somewhat from the CWB data in high waves of over 3 m, further research such as collection and analysis of long-term remote wave observation data and filter development is necessary.

Establishment of Analytical Method for Methylmercury in Fish by Using HPLC-ICP/MS (고성능액체크로마토그래피-유도결합플라즈마 질량분석기를 이용한 어류 중 메틸수은 분석법 확립)

  • Yoo, Kyung-Yoal;Bahn, Kyeong-Nyeo;Kim, Eun-Jung;Kim, Yang-Sun;Myung, Jyong-Eun;Yoon, Hae-Seong;Kim, Mee-Hye
    • Korean Journal of Environmental Agriculture
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    • v.30 no.3
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    • pp.288-294
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    • 2011
  • BACKGROUND: Methylmercury is analyzed by HPLC-ICP/MS because of the simplicity for sample preparation and interference. However, most of the pre-treatment methods for methylmercury need a further pH adjustment of the extracted solution and removal of organic matter for HPLC. The purpose of this study was to establish a rapid and accurate analytical method for determination of methylmercury in fish by using HPLC-ICP/MS. METHOD AND RESULTS: We conducted an experiment for pre-treatment and instrument conditions and analytical method verification. Pre-treatment condition was established with aqueous 1% L-cysteine HCl and heated at $60^{\circ}C$ in microwave for 20 min. Methylmercury in $50{\mu}L$ of filtered extract was separated by a C18 column and aqueous 0.1% L-cysteine HCl + 0.1% L-cysteine mobile phase at $25^{\circ}C$. The presence of cysteine in mobile phase and sample solution was essential to eliminate adsorption, peak tailing and memory effect problems. Correlation coefficient($r^2$) for the linearity was 0.9998. The limits of detection and quantitation for this method were 0.15 and $0.45{\mu}g/kg$ respectively. CONCLUSION: Result for analytical method verification, accuracy and repeatability of the analytes were in good agreement with the certified reference materials values of methylmercury at a 95% confidence level. The advantage of the established method is that the extracted solution can be directly injected into the HPLC column without additional processes and the memory effect of mercury in the ICP-MS can be eliminated.

Spectrophotometric Determination of Soil Chemical Properties Using Soiltek® KA-P Spectrophotometer (Soiltek KA-P 분광광도계률 사용한 토양 화학적 성질의 분광학적 분석)

  • Hyun, Hae-Nam;Oh, Sang-Sil;Koo, Bon-Jun;Kang, Ho-Jun
    • Korean Journal of Soil Science and Fertilizer
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    • v.33 no.2
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    • pp.127-138
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    • 2000
  • To enable rapid and convenient soil test, new soil analytical methods, which require only one instrument, UV/Vis spectrophotometer, were developed and named "Soiltek KA-P spectrophotometric methods". The Soiltek$^{(R)}$ KA-P spectrophotometric method was compared with standard method of RDA in analytical capability for soil chemical properties. Using the 78 soils collected from upland, paddy, orchard, and vinyl house soils, soil organic matter, exchangeable K, Ca, and Mg. CEC, available $SiO_2$, and nitrate were analyzed by the two methods. The color stability(ratio of the absorbance at elapsed time t to the absorbance at time t=0) of organic matter. Ca, Mg, and available $SiO_2$ decreased to about 2% within one hour. However, that of exchangeable K, CEC, and nitrate remained constant. The results obtained with Soiltek$^{(R)}$ KA-P spectrophotometric method showed highly significant correlation with those measured by the standard method of RDA($R^2$ >0.9501), in which the slopes were near unity of $1.0{\pm}0.05$. The standard deviation values of organic matter, exchangeable K, Ca, and Mg, CEC, available $SiO_2$, and nitrate were apparently lower than ${\pm}1.8gkg^{-1}$, ${\pm}0.05cmol^+kg^{-1}$, ${\pm}0.18cmol^+kg^{-1}$, and ${\pm}0.13cmol^+kg^{-1}$, ${\pm}1.0cmol^+kg^{-1}$, ${\pm}5.0mgkg^{-1}$, and ${\pm}10.0mgkg^{-1}$, respectively. All the measurements showed coefficients of variation of less than 7~17% and were within the confidence level of 95%, which means both the methods are precise. Considering the relative simplicity, low cost, precision and accuracy, the proposed Soiltek$^{(R)}$ KA-P spectrophotometric methods could be recommended as an alternative to standard method.

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Verification of Multi-point Displacement Response Measurement Algorithm Using Image Processing Technique (영상처리기법을 이용한 다중 변위응답 측정 알고리즘의 검증)

  • Kim, Sung-Wan;Kim, Nam-Sik
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.30 no.3A
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    • pp.297-307
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    • 2010
  • Recently, maintenance engineering and technology for civil and building structures have begun to draw big attention and actually the number of structures that need to be evaluate on structural safety due to deterioration and performance degradation of structures are rapidly increasing. When stiffness is decreased because of deterioration of structures and member cracks, dynamic characteristics of structures would be changed. And it is important that the damaged areas and extent of the damage are correctly evaluated by analyzing dynamic characteristics from the actual behavior of a structure. In general, typical measurement instruments used for structure monitoring are dynamic instruments. Existing dynamic instruments are not easy to obtain reliable data when the cable connecting measurement sensors and device is long, and have uneconomical for 1 to 1 connection process between each sensor and instrument. Therefore, a method without attaching sensors to measure vibration at a long range is required. The representative applicable non-contact methods to measure the vibration of structures are laser doppler effect, a method using GPS, and image processing technique. The method using laser doppler effect shows relatively high accuracy but uneconomical while the method using GPS requires expensive equipment, and has its signal's own error and limited speed of sampling rate. But the method using image signal is simple and economical, and is proper to get vibration of inaccessible structures and dynamic characteristics. Image signals of camera instead of sensors had been recently used by many researchers. But the existing method, which records a point of a target attached on a structure and then measures vibration using image processing technique, could have relatively the limited objects of measurement. Therefore, this study conducted shaking table test and field load test to verify the validity of the method that can measure multi-point displacement responses of structures using image processing technique.