• Title/Summary/Keyword: Calibration matrix

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Simultaneous Quantitative Determination of Nine Hallucinogenic NBOMe Derivatives in Human Plasma Using Liquid Chromatography Tandem Mass Spectrometry

  • Seo, Hyewon;Yoo, Hye Hyun;Kim, Young-Hoon;Hong, Jin;Sheen, Yhun Yhong
    • Mass Spectrometry Letters
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    • v.10 no.1
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    • pp.18-26
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    • 2019
  • We developed a bioanalytical method for simultaneous determination of nine NBOMe derivatives (25H-NBOMe, 25B-NBOMe, 25E-NBOMe, 25N-NBOMe, 25C-NBOH, 25I-NBOH, 25B-NBF, 25C-NBF, and 25I-NBF) in human plasma using liquid chromatography tandem mass spectrometry (LC-MS/MS). Human plasma samples were pre-treated using solid-phase extraction. Separation was achieved on a C18 column under gradient elution using a mobile phase containing 0.1% formic acid in acetonitrile and 0.1% formic acid in water at a flow rate of 0.3 mL/min. Mass detection was performed in the positive ion mode using multiple reaction monitoring. The calibration range was 1-100 ng/mL for all quantitative analytes, with a correlation coefficient greater than 0.99. The intra- and inter-day precision and accuracy varied from 0.85 to 6.92% and from 90.19 to 108.69%, respectively. The recovery ranged from 86.36 to 118.52%, and the matrix effects ranged from 27.09 to 99.72%. The stability was acceptable in various conditions. The LC-MS/MS method was validated for linearity, accuracy, precision, matrix effects, recovery and stability in accordance with the FDA guidance. The proposed method is suitable for reliable and robust routine screening and analysis of nine NBOMe derivatives in forensic field.

Development of a Simultaneous Analytical Method for Diquat, Paraquat and Chlormequat in Animal Products Using UPLC-MS/MS

  • Cho, Il Kyu;Rahman, Md. Musfiqur;Seol, Jae Ung;Noh, Hyun Ho;Jo, Hyeong-Wook;Moon, Joon-Kwan
    • Korean Journal of Environmental Agriculture
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    • v.39 no.4
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    • pp.368-374
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    • 2020
  • BACKGROUND: The residual analysis of polar pesticides has remained a challenge. It is even more difficult to simultaneously analyze multiple polar pesticides. Diquat, paraquat, and chlormequat are typical examples of highly polar pesticides. The existing methods for the analysis of diquat, paraquat and chlormequat are complex and time consuming. Therefore, a simple, quick and effective method was developed in the represent study for simultaneous analysis of diquat, paraquat and chlormequat in animal products, meat and fat using UPLC-MS/MS. METHODS AND RESULTS: Sample extraction was carried out using acidified acetonitrile and water and re- extracted with acidified acetonitrile and combine the extracts followed by centrifugation. The extract was then cleaned up with a HLB cartridge after reconstitution with acidic acetonitrile and water. The method was validated in quintuplicate at three different concentrations. The limits of detection (LOD) and quantification (LOQ) were 0.0015 and 0.005 mg/L, respectively. Matrix suppression effect was observed for all of the analytes. A seven point matrix matched calibration curve was constructed for each of the compound resulted excellent linearity with determination coefficients (R2) ≥ 0.991. Accuracy and precision of the method was calculated from the recovery and repeatability and ranged from 62.4 to 119.7% with relative standard deviation less than 18.8%. CONCLUSION: The recovery and repeatability of the developed method were in the acceptable range according to the Codex Alimentarius guideline. The developed method can be applied for the routine monitoring of diquat, paraquat, and chlormequat in animal products, meat and fat.

Video Camera Characterization with White Balance (기준 백색 선택에 따른 비디오 카메라의 전달 특성)

  • 김은수;박종선;장수욱;한찬호;송규익
    • Journal of the Institute of Electronics Engineers of Korea SP
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    • v.41 no.2
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    • pp.23-34
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    • 2004
  • Video camera can be a useful tool to capture images for use in colorimeter. However the RGB signals generated by different video camera are not equal for the same scene. The video camera for use in colorimeter is characterized based on the CIE standard colorimetric observer. One method of deriving a colorimetric characterization matrix between camera RGB output signals and CIE XYZ tristimulus values is least squares polynomial modeling. However it needs tedious experiments to obtain camera transfer matrix under various white balance point for the same camera. In this paper, a new method to obtain camera transfer matrix under different white balance by using 3${\times}$3 camera transfer matrix under a certain white balance point is proposed. According to the proposed method camera transfer matrix under any other white balance could be obtained by using colorimetric coordinates of phosphor derived from 3${\times}$3 linear transfer matrix under the certain white balance point. In experimental results, it is demonstrated that proposed method allow 3${\times}$3 linear transfer matrix under any other white balance having a reasonable degree of accuracy compared with the transfer matrix obtained by experiments.

Determination of Coccidiostats (Amprolium and Decoquinate) in Cattle and Chicken's Muscle using High Performance Liquid Chromatography

  • Kim, Byung-Ju;Ham, Hyun-Sun;Lee, Jin-Joo;Cheong, Nam-Yong;Myung, Seung-Woon
    • Bulletin of the Korean Chemical Society
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    • v.33 no.2
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    • pp.559-563
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    • 2012
  • An analytical method for the simultaneous determination of veterinary medicines (amprolium and decoquinate) in cattle and chicken's muscle by HPLC/UV-vis was established. Samples were extracted by a HLB (Hydrophilic-Liphophilic Balance) cartridge with acetonitrile and methanol. Prior to HPLC injection, a mixture solvent (Water:MeOH, 1:1) was utilized as a reconstitution solvent. Chromatographic separation was achieved with a C18 column ($250{\times}4.6mm$, $5{\mu}m$) using gradient elution with 20 mM HFBA and MeOH:ACN (1:1.8). The calibration curves from the spiked blank matrix showed good linearity (above $r^2$=0.997) in the concentration range of $0.13-12.0mg\;kg^{-1}$. The relative recovery (accuracy) and limit of quantitation (LOQ) were in the range of 78.5-107.1% and $0.13-0.42mg\;kg^{-1}$, respectively. The developed method can be used to determine under the MRL (Maximum Residue Limits) levels of veterinary medicines in animal tissues.

Simple measurement the chelator number of antibody conjugates by MALDI-TOF MS

  • Shin, Eunbi;Lee, Ji Woong;Lee, Kyo Chul;Shim, Jae Hoon;Cha, Sangwon;Kim, Jung Young
    • Journal of Radiopharmaceuticals and Molecular Probes
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    • v.3 no.2
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    • pp.54-58
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    • 2017
  • Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry(MALDI-TOF MS) is one of the powerful methods that enable analysis of small molecules as well as large molecules up to about 500,000 Da without severe fragmentation. MALDI-TOF MS, thus, has been a very useful an analytical tool for the confirmation of synthetic molecules, probing PTMs, and identifying structures of a given protein. In recent nuclear medicine, MALDI-TOF MS liner ion mode helps researcher calculate the average number of chelator(or linkage) per an antibody conjugate, such as DOTA-(or DFO-) trastuzumab for labeling a medical radioisotope. This simple technique can be utilized to improve the labeling method and control the quality at the development of antibody-based radiopharmaceuticals, which is very effected to diagnosis and therapy for in vivo tumor cells, with radioisotopes like $^{89}Zr$, $^{64}Cu$, and 177Lu. To minimize the error, MALDI-TOF MS measurement is repeatedly performed for each sample in this study, and external calibration is carried out after data collection.

A Study on the Mixing Characteristics in Complex Turbulent Flow by a Laser Induced Fluorescence Method (레이저 형광여기법(LIF)를 이용한 복잡 난류유동장의 혼합특성에 관한 연구)

  • Kim, Kyung-Chun;Jeong, Eun-Ho
    • Proceedings of the KSME Conference
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    • 2001.06e
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    • pp.542-547
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    • 2001
  • A non-intrusive Planar Laser-Induced Fluorescence(PLIF) technique was applied to study the turbulent mixing process in a Rushton turbine reactor. Instantaneous and ensemble averaged concentration fields are obtained by measuring the fluorescence intensity of Rhodamine B tracer excited by a thin Nd:Yag laser sheet illuminating the whole center plane of the stirred tank. The gray level images captured by a 14-bit cooled CCD camera can be transformed to the local concentration values using a calibration matrix. The dye injection point was selected at the tank wall with three quarter height (3/4H) from the tank bottom to observe the mixing characteristics in upper bulk flow region. There exist distinct two time scales: the rapid decay of mean concentration in each region after the dye infusion reflects the large scale mixing while the followed slow decay reveals the small scale mixing. The temporal change of concentration probability functions conjectures the two sequential processes in the batch type mixing. An inactive column of water existed above the impeller disk, in which the fluid rotates with the shaft but is isolated from the mean bulk flow.

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Simultaneous Measurement of Strain and Temperature During and After Cure of Unsymmetric Composite Laminate Using Fiber Optic Sensors (비대칭 복합적층판의 성형시 및 성형후 광섬유 센서를 이용한 변형률 및 온도의 동시 측정)

  • 강동훈;강현규;김대현;방형준;홍창선;김천곤
    • Proceedings of the Korean Society For Composite Materials Conference
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    • 2001.05a
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    • pp.244-249
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    • 2001
  • In this paper, we present the simultaneous measurement of the fabricaition strain and temperature during and after cure of unsymmetric composite laminate uising fiber optic sensors. Fiber Bragg grating/extrinsic Fabry-Perot interferometric (FBG/EFPl) hybrid sensors are used to measure those measurands. The characteristic matrix of sensor is analytically derived and measurements can be done without sensor calibration. A wavelength-swept fiber laser is utilized as a light source. FBG/EFPI sensors are embedded in a graphite/epoxy unsymmetric cross-ply composite laminate at different direction and different location. We perform the real time measurement of fabrication strains and temperatures at two points of the composite laminate during cure process in an autoclave. Also, the thermal strains and temperatures of the fabricated laminate are measured in thermal chamber. Through these experiments, we can provide a basis for the efficient smart processing of composite and know the thermal behavior of unsymmetric cross-ply composite laminate.

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Determination of Corticosteroids in Moisturizers by LC-MS/MS

  • Park, Sumin;Choi, Gye Young;Lee, Seon-Ah;Kim, Hyun Jeong;Yum, Hye Yung;Paeng, Ki-Jung
    • Mass Spectrometry Letters
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    • v.7 no.1
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    • pp.26-29
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    • 2016
  • Simultaneous determination of three corticosteroids (clobetasol propionate, betamethasone dipropionate, fluticasone propionate) in moisturizers was performed by using liquid chromatography (LC) coupled with tandem mass spectrometry (MS/MS). Sample preparation was conducted by the liquid-liquid extraction (LLE). Moisturizers include emulsifying agent and it forms micelles. In order to improve the extraction efficiency of corticosteroids trapped in micelle, newly developed-optimized extraction conditions which can remove the matrix effect from moisturizers was applied with various pH conditions in LLE extraction stage of sample preparation. Thus, the addition of 10 μL of 1 M HCl into moisturizers sample before extraction could improve the extraction efficiency. For the quantitative analysis, SRM table that contained specific transition of all of target corticosteroids was created. The developed method was validated for linearity, accuracy, precision, limit of detection (LOD), limit of quantization (LOQ) and recovery. Over the 0.99 r2 value was obtained in calibration standard range. Effective accuracy and precision were also obtained. LODs were below 31 ng/mL and LOQs were estimated below 94 ng/mL for all corticosteroids tested.

A Study on the Mixing Characteristics in a Rushton Turbine Reactor by a Laser Induced Fluorescence Method (레이저 형광여기법(LIF)를 이용한 러쉬톤 터빈 교반기의 혼합특성에 관한 연구)

  • Jeong, Eun-Ho;Kim, Gyeong-Cheon
    • Transactions of the Korean Society of Mechanical Engineers B
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    • v.26 no.8
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    • pp.1145-1152
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    • 2002
  • A non-intrusive Planar Laser-Induced Fluorescence(PLIF) technique was applied to study the turbulent mixing process in a Rushton turbine reactor. Instantaneous and ensemble averaged concentration fields was obtained by measuring the fluorescence intensity of Rhodamine B tracer excited by a thin Nd:Yag laser sheet illuminating the whole center plane of the stirred tank. The gray level images captured by a 14-bit cooled CCD camera could be transformed to the local concentration values using a calibration matrix. The dye injection point was selected at the tank wall with three quarter. height (3/4H) from the tank bottom to observe the mixing characteristics in upper bulk flow region. There exist distinct two time scales: the rapid decay of mean concentration after the dye infusion reflects the large scale turbulent mixing while the fellowed slow decay reveals the small scale molecular mixing. The temporal change of concentration variance field conjectures the two sequential processes for the batch type mixing. An inactive column of water is existed above the impeller disk, in which the fluid rotates with the shaft but is isolated from the mean bulk flow.

A Study on the Analytical Characterizations of the Low Flow-Low Power ICP-AES (Low flow-low power 유도결합 플라즈마 원자방출 분광법에서의 분석적 특성에 관한 연구)

  • Yang, Hae Soon;Kim, Young Man;Kim, Sun Tae;Choi, Beom Suk
    • Analytical Science and Technology
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    • v.7 no.3
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    • pp.253-260
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    • 1994
  • Analytical characteristics of low power-low flow inductively coupled plasma-atomic emission spectometry(ICP-AES) has been studied. Although the net intensity of the low power ICP is lower than the moderate power ICP, the signal to background ratio becomes higher since the background intensity decreases with decreasing the RF power. The detection limit of the low power ICP is comparable with that of the moderate power ICP. The dynamic range of the calibration curve of the low power ICP is $10^4{\sim}10^5$. The ionization interferences by alkali metals increase with increasing the carrier gas flow rate, but the effects are not varied significantly with the RF power.

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