• 제목/요약/키워드: Quantification Method

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Accurate Quantification of Saccharin Using Isotope Dilution Liquid Chromatography Mass Spectrometry (ID-LC/MS)

  • Lee, Yun-Jung;Kim, Byung-Joo;Kim, Jeong-Kwon;Ahn, Seong-Hee
    • Mass Spectrometry Letters
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    • 제2권2호
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    • pp.37-40
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    • 2011
  • Saccharin is a commonly used artificial sweetener in foodstuffs. However, for its carcinogenic dispute, it has been regulated by government bodies. In this study, isotope dilution mass spectrometry (ID-MS) was introduced for the accurate quantification of saccharin. To employ ID-LC/MS, we obtained its isotope analogue, $^{13}C_1$-sodium saccharin, by customized synthesis. Samples were spiked with $^{13}C_1$-sodium saccharin and analyzed with LC/MS in negative mode. Chromatographic conditions were optimized for the adequate chromatographic retention and separation of saccharin with a $C_{18}$ column. MS was operated with electrospray ionization by the selected ion monitoring (SIM) mode of $[M-H]^-$ for saccharin (m/z 182) and $[M-Na]^-$ for its isotope analogue (m/z 183). To validate the ID-LC/MS method for accurate measurement, we prepared a batch of a candidate material by sortifying quasi-tea-drinks with saccharin and analyzed samples gravimetrically fortified in various levels of concentration. The repeatability and reproducibility of this method was tested by analyzing the reference material. Result show that ID-LC/MS is a reliable method for the quantitative analysis of saccharin.

Liquid Chromatography-Tandem Mass Spectrometry Analysis of Riboflavin in Beagle Dog Plasma for Pharmacokinetic Studies

  • Jeong, Hyeon Myeong;Shin, Beom Soo;Shin, Soyoung
    • Mass Spectrometry Letters
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    • 제11권1호
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    • pp.10-14
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    • 2020
  • Riboflavin is a water-soluble vitamin, which serves as a precursor to flavin mononucleotide and flavin adenine dinucleotide. This study aimed to develop a simple and rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis for the quantification of riboflavin in the Beagle dog plasma. This method utilized simple protein precipitation with acetonitrile and 13C4, 15N2-riboflavin was used as an internal standard (IS). For chromatographic separation, a hydrophilic interaction liquid chromatography (HILIC) column was used with gradient elution. The mobile phase consisted of 0.1% (v/v) aqueous formic acid with 10 mM ammonium formate and acetonitrile with 0.1% (v/v) formic acid. Since riboflavin is an endogenous compound, 4% bovine serum albumin in phosphate buffered saline was used as a surrogate matrix to prepare the calibration curve. The quantification limit for riboflavin in the Beagle dog plasma was 5 ng/mL. The method was fully validated for its specificity, sensitivity, accuracy and precision, recovery, and stability according to the US FDA guidance. The developed LC-MS/MS method may be useful for the in vivo pharmacokinetic studies of riboflavin.

Optimization of Microwave-Assisted Method for Accelerated Glycated Hemoglobin Quantification from Amino Acids to Proteins

  • Tran, Thi Thanh Huong;Jeong, Ji-Seon
    • Mass Spectrometry Letters
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    • 제8권3호
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    • pp.53-58
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    • 2017
  • Glycated hemoglobin ($HbA_{1c}$) has been commonly used to screen and diagnose for patients with diabetes mellitus. Here the accelerated procedure of microwave-assisted sample treatment from acid hydrolysis to enzyme digestion followed by isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS) was optimized and applied to measure $HbA_{1c}$ in an effort to speed up analysis time. First, two signature peptides of $HbA_{1c}$ and hemoglobin $A_0$ were certified with amino acid analysis by setting optimized acid hydrolysis conditions to $150^{\circ}C$, 1.5 h and $10{\mu}M$ sample concentration in 8 M hydrochloric acid. Consequently, the accurate certified peptides above were used as calibration standards to implement the proteolytic procedure with endoproteinase Glu-C at $37^{\circ}C$, 700 W for 6 h. Compared to the traditional method, the microwave heating not only shortened dramatically sample preparation time, but also afforded comparable recovery yields. The optimized protocol and analytical conditions in this study are suitable for a primary reference method of $HbA_{1c}$ quantification with full SI-traceability and other similar proteins in complex biological samples.

Coronary Artery Stenosis Quantification for Computed Tomography Angiography Based on Modified Student's t-Mixture Model

  • Sun, Qiaoyu;Yang, Guanyu;Shu, Huazhong;Shi, Daming
    • ETRI Journal
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    • 제39권5호
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    • pp.662-671
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    • 2017
  • Coronary artery disease (CAD) is a major cause of death in the world. As a non-invasive imaging modality, computed tomography angiography (CTA) is now usually used in clinical practice for CAD diagnosis. Precise quantification of coronary stenosis is of great interest for diagnosis and treatment planning. In this paper, a novel cluster method based on a Modified Student's t-Mixture Model is applied to separate the region of vessel lumen from other tissues. Then, the area of the vessel lumen in each slice is computed and the estimated value of it is fitted with a curve. Finally, the location and the level of the most stenoses are captured by comparing the calculated and fitted areas of the vessel. The proposed method has been applied to 17 clinical CTA datasets and the results have been compared with reference standard degrees of stenosis defined by an expert. The results of the experiment indicate that the proposed method can accurately quantify the stenosis of the coronary artery in CTA.

Multi-spectral adaptive vibration suppression of two-path active mounting systems with multi-NLMS algorithms

  • Yang Qiu;Dongwoo Hong;Byeongil Kim
    • Smart Structures and Systems
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    • 제32권6호
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    • pp.393-402
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    • 2023
  • Recently, hybrid and electric vehicles have been actively developed to replace internal combustion engine (ICE) vehicles. However, their vibrations and noise with complex spectra cause discomfort to drivers. To reduce the vibrations transmitted through primary excitation sources such as powertrains, structural changes have been introduced. However, the interference among different parts is a limitation. Thus, active mounting systems based on smart materials have been actively investigated to overcome these limitations. This study focuses on diminishing the source movement when a structure with two active mounting systems is excited to a single sinusoidal and a multi-frequency signal, which were investigated for source movement reduction. The overall structure was modeled based on the lumped parameter method. Active vibration control was implemented based on the modeled structure, and a multi-normalization least mean square (NLMS) algorithm was used to obtain the control input for the active mounting system. Furthermore, the performance of the NLMS algorithm was compared with that of the quantification method to demonstrate the performance of active vibration control. The results demonstrate that the vibration attenuation performance of the source component was improved.

Multihazard capacity optimization of an NPP using a multi-objective genetic algorithm and sampling-based PSA

  • Eujeong Choi;Shinyoung Kwag;Daegi Hahm
    • Nuclear Engineering and Technology
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    • 제56권2호
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    • pp.644-654
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    • 2024
  • After the Tohoku earthquake and tsunami (Japan, 2011), regulatory efforts to mitigate external hazards have increased both the safety requirements and the total capital cost of nuclear power plants (NPPs). In these circumstances, identifying not only disaster robustness but also cost-effective capacity setting of NPPs has become one of the most important tasks for the nuclear power industry. A few studies have been performed to relocate the seismic capacity of NPPs, yet the effects of multiple hazards have not been accounted for in NPP capacity optimization. The major challenges in extending this problem to the multihazard dimension are (1) the high computational costs for both multihazard risk quantification and system-level optimization and (2) the lack of capital cost databases of NPPs. To resolve these issues, this paper proposes an effective method that identifies the optimal multihazard capacity of NPPs using a multi-objective genetic algorithm and the two-stage direct quantification of fault trees using Monte Carlo simulation method, called the two-stage DQFM. Also, a capacity-based indirect capital cost measure is proposed. Such a proposed method enables NPP to achieve safety and cost-effectiveness against multi-hazard simultaneously within the computationally efficient platform. The proposed multihazard capacity optimization framework is demonstrated and tested with an earthquake-tsunami example.

Uncertainty analysis of UAM TMI-1 benchmark by STREAM/RAST-K

  • Jaerim Jang;Yunki Jo;Deokjung Lee
    • Nuclear Engineering and Technology
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    • 제56권5호
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    • pp.1562-1573
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    • 2024
  • This study rigorously examined uncertainty in the TMI-1 benchmark within the Uncertainty Analysis in Modeling (UAM) benchmark suite using the STREAM/RAST-K two-step method. It presents two pivotal advancements in computational techniques: (1) Development of an uncertainty quantification (UQ) module and a specialized library for the pin-based pointwise energy slowing-down method (PSM), and (2) Application of Principal Component Analysis (PCA) for UQ. To evaluate the new computational framework, we conducted verification tests using SCALE 6.2.2. Results demonstrated that STREAM's performance closely matched SCALE 6.2.2, with a negligible uncertainty discrepancy of ±0.0078% in TMI-1 pin cell calculations. To assess the reliability of the PSM covariance library, we performed verification tests, comparing calculations with Calvik's two-term rational approximation (EQ 2-term) covariance library. These calculations included both pin-based and fuel assembly (FA-wise) computations, encompassing hot zero-power and hot full-power operational conditions. The uncertainties calculated using both the EQ 2-term and PSM resonance treatments were consistent, showing a deviation within ±0.054%. Additionally, the data compression process yielded compression ratios of 88.210% and 92.926% for on-the-fly and data-saving approaches, respectively, in TMI fuel assembly calculations. In summary, this study provides a comprehensive explanation of the PCA process used for UQ calculations and offers valuable insights into the robustness and reliability of newly developed computational methods, supported by rigorous verification tests.

실용적이고 최적화된 광물정량분석법 연구 (A Study of Practical and Optimized Mineral Quantification)

  • 손병국;안기오
    • 광물과 암석
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    • 제34권4호
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    • pp.227-239
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    • 2021
  • 자연산 시료의 광물함량을 X-선 분말회절분석에 의하여 실용적이고 효과적으로 정량분석하는 방법에 대하여 연구하였다. 이를 위하여 무작위 배향된 분말시료 마운트(randomly oriented powder sample mount)를 최적으로 제작하는 실험을 하였으며, 단일 피크강도를 표준물질과 비교하여 정량분석하는 레퍼런스 강도비(RIR) 방법과 X-선 회절도의 전패턴을 계산하는 리트벨드 방법의 효율성을 비교하는 실험을 수행 하였다. 또한, 비정질 광물이 포함된 시료를 리트벨드 방법에 의하여 정량분석하고 효율성을 검토하였다. 연구결과, 측면 마운팅(side mounting) 방법에 의하여 최적의 무작위 배향(random orientation)에 도달할 수 있었다. 또한, 특정 피크를 사용하는 RIR방법보다는 X-선 회절도의 전패턴을 사용하는 리트벨드 방법이 정량분석에 더 적합하였다. 그러나 어느 방법이든 분석기술 뿐만 아니라 분석자의 숙련된 경험을 필요로 한다. 리트벨드 방법에 의해 비정질 광물도 정량분석할 수 있었으며 분석결과는 지질해석을 가능하게 하였다.

LC-MS/MS를 이용한 어류 및 갑각류의 잔류 Erythromycin 항생제 분석 (Determination of Residual Erythromycin Antibiotic in Fishery Products by Liquid Chromatography-electrospray Ionization Mass Spectrometry)

  • 조미라;목종수;이두석;김민정;김풍호
    • 한국수산과학회지
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    • 제42권1호
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    • pp.15-19
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    • 2009
  • A simple and sensitive method for erythromycin quantification by liquid chromatography electrospray mass spectrometry (LC-MS/MS) in fishery products was developed. Samples were extracted by liquid-liquid extraction using 70% acetonitrile. Lipids were removed by acetonitrile saturated hexane. LC separation was performed on a Shiseido UG C-18 column ($150\;mm{\times}2.0\;mm$ internal diameter.) with a gradient system of 0.2% acetic acid-acetonitrile containing 0.2% acetic acid as a mobile phase at flow rate of 0.2 mL/min. The mass spectrometer was operated in selected reaction monitoring with positive electro-spray interface. Transitions were monitored a m/z $734{\to}577$ and $734{\to}158$, with m/z $734{\to}577$ chosen for quantification. Recovery of erythromycin from fish and shrimp fortified at the 10 ng/mL, 50 ng/mL and 100 ng/mL were 91.6-109.4%, 84.4-111.2% and 98.8-109.6% with high precision, respectively. Limits of quantification and limits of detection of erythromycin in both fish and shrimp were 10.0 ng/mL and 1.0 ng/mL, respectively. This analysis method for erythromycin has been proposed for registration in the Korean Official Methods of Food Analysis and has been utilized for fishery products analysis by the Korea Food and Drug Adminstration and the National Fisheries Products Quality Inspection Service.

암석 절리면 거칠기의 정량화에 대한 연구(II) - 거칠기의 구분과 강도식의 제안 - (A New Quantification Method of Rock Joint Roughness (II) - Roughness classification and strength equation -)

  • 홍은수;조계춘;권태혁;이인모
    • 한국터널지하공간학회 논문집
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    • 제8권2호
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    • pp.183-196
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    • 2006
  • 카메라 방식의 3D 스캐너로부터 구한 암석 절리면의 거칠기를 만곡과 요철의 거칠기 성분으로 구분하였다. 거칠기의 구분 기준은 이전의 연구에서 도출된 것을 적용하였으며, 구분 방법으로는 디지털 필티링 기법을 사용하였다. 원래의 프로파일과 구분한 프로파일을 사용하여 금속 주형을 제작하였으며, 정밀한 가공을 위하여 WEDM(Wire-cut Electric Discharge Machining)을 사용하였다. 고강도 석고를 사용하여 시편을 복제하였고, 절리면 전단시험을 실시하였다. 낮은 연직응력 범위와 높은 연직응력 범위에서 전단시험을 실시하고, 거칠기의 규모와 연직응력에 따른 발현 특성을 분석하였다. 절리면 전단강도 예측을 위한 새로운 상관식을 제안하였으며, 이 상관식은 거칠기의 발현 특성과 거칠기 계수의 특성을 모두 효과적으로 고려할 수 있었다. 그러므로 거칠기의 구분에 의한 정량화가 절리면 전단강도 예측을 위한 효과적인 방법이 될 수 있음을 확인할 수 있었다.

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