• Title/Summary/Keyword: Ionization development

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Determination of Glimepiride in Human Plasma by Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry

  • Kim, Ho-Hyun;Chang, Kyu-Young;Lee, Hee-Joo;Han, Sang-Beom
    • Bulletin of the Korean Chemical Society
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    • v.25 no.1
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    • pp.109-114
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    • 2004
  • A sensitive method for quantitation of glimepiride in human plasma has been established using liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS). Glipizide was used as an internal standard. Glimepiride and internal standard in plasma sample was extracted using diethyl etherethyl acetate (1 : 1). A centrifuged upper layer was then evaporated and reconstituted with the mobile phase of acetonitrile-5 mM ammonium acetate (60:40, pH 3.0). The reconstituted samples were injected into a $C_{18}$ reversed-phase column. Using MS/MS in the multiple reaction monitoring (MRM) mode, glimepiride and glipizide were detected without severe interference from human plasma matrix. Glimepiride produced a protonated precursor ion ([M+H]$^+$) at m/z 491 and a corresponding product ion at m/z 352. And the internal standard produced a protonated precursor ion ([M+H]]$^+$) at m/z 446 and a corresponding product ion at m/z 321. Detection of glimepiride in human plasma by the LC-ESI/MS/MS method was accurate and precise with a quantitation limit of 0.1 ng/mL. The validation, reproducibility, stability, and recovery of the method were evaluated. The method has been successfully applied to pharmacokinetic studies of glimepiride in human plasma.

MALDI Mass Spectrometric Analysis of Nonderivatized Steroids Using Cyclodextrin-supported 2,5-Dihydroxybenzoic Acid as Matrix

  • Son, Jeongjin;Cha, Sangwon
    • Bulletin of the Korean Chemical Society
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    • v.35 no.5
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    • pp.1409-1412
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    • 2014
  • Sex hormones are important metabolites in vertebrates' development and reproduction. For rapid screening sex hormones, matrix-assisted laser desorption/ionization (MALDI) mass spectrometry (MS) is one of the promising analytical platforms, but MALDI MS faces many challenges in detecting steroids such as low ionization efficiency and matrix background interference. One potential strategy to overcome matrix interference in the low m/z region is using a cyclodextrin (CD)-supported matrix for steroid analysis since CD-supported matrixes are known to effectively suppress matrix-related ion signals. In this study, we aimed to find the optimal CD-supported matrix for the analysis of the nonderivatized sex steroids. Our results showed that the ${\alpha}CD$-supported 2,5-dihydroxybenzoic acid (DHB) matrix efficiently ionized all three major classes of sex hormones, estrogens, androgens, and progestagens, with low or no matrix background and also with high sensitivity. In addition, the ${\alpha}CD$-supported DHB matrix mainly generated molecular ions or protonated ions of sex hormones, and this enabled us to obtain information-rich tandem mass spectra which potentially lead to unambiguous identification of steroid species from complex metabolite mixtures.

Effects of Column Length and Particle Diameter on Phospholipid Analysis by Nanoflow Liquid Chromatography-Electrospray Ionization-Mass Spectrometry

  • Lee, Ju-Yong;Lim, Sang-Soo;Moon, Myeong-Hee
    • Mass Spectrometry Letters
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    • v.2 no.3
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    • pp.65-68
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    • 2011
  • The effects of column length and particle size on the efficiency of separation and characterization of phospholipids (PLs) are investigated using nanoflow liquid chromatography-electrospray ionization-tandem mass spectrometry (nLC-ESI-MS-MS). Since PLs are associated with cell proliferation, apoptosis, and signal transduction, it is of increasing interests in lipidomics to establish reliable analytical methods for the qualitative and quantitative profiling of PLs related to biomarker development in adult diseases. Due to the complexity of PLs, the preliminary separation of PLs is necessary prior to MS analysis. In this study, length of capillary column and the particle size of reversed phase ($C_{18}$) packing materials are varied to find a reliable condition for the high speed and high resolution separation using 8 PL standard mixtures. From experiments, it was found that a capillary column of nLC-ESI-MS-MS analysis for PL mixtures can be minimized to a 5 cm long pulled tip column packed with 3 ${\mu}m$ $C_{18}$ particles without losing resolution.

Screening Analysis of 10 Adrenal Steroids by Matrix-Assisted Laser Desorption Ionization-Tandem Mass Spectrometry

  • Kim, Sun-Ju;Jung, Hyun-Jin;Chung, Bong-Chul;Choi, Man-Ho
    • Mass Spectrometry Letters
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    • v.2 no.3
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    • pp.69-72
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    • 2011
  • Defective synthesis of the steroid hormones by the adrenal cortex has profound effects on human development and homeostasis. Due to the time-consuming chromatography procedure combined with mass spectrometry, the matrix-assisted laser desorption ionization method coupled to the linear ion-trap tandem mass spectrometry (MALDI-LTQ-MS/MS) was developed for quantitative analysis of 10 adrenal steroids in human serum. Although MALDI-MS can be introduced for its applicability as a high-throughput screening method, it has a limitation on reproducibility within and between samples, which renders poor reproducibility for quantification. For quantitative MALDI-MS/MS analysis, the stable-isotope labeled internal standards were used and the conditions of crystallization were tested. The precision and accuracy were 3.1~35.5% and 83.8~138.5%, respectively, when a mixture of 10 mg/mL ${\alpha}$-cyano-4-hydroxycinnamic acid in 0.2% TFA of 70% acetonitrile was used as the MALDI matrix. The limit of quantification ranged from 5 to 340 ng/mL, and the linearity as a correlation coefficient was higher than 0.988 for all analytes in the calibration range. Clinical applications include quantitative analyses of patients with congenital adrenal hyperplasia. The devised MALDI-MS/MS technique could be successfully applied to diagnosis of clinical samples.

Xenon in molten salt reactors: The effects of solubility, circulating particulate, ionization, and the sensitivity of the circulating void fraction

  • Price, Terry J.;Chvala, Ondrej;Taylor, Zack
    • Nuclear Engineering and Technology
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    • v.52 no.6
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    • pp.1131-1136
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    • 2020
  • Xenon behaves differently in molten salt reactors (MSRs) compared to solid fuel reactors. This behavior needs exploring due to the large reactivity effect of the 135Xe isotope, given the current interest in MSR power plant development for commercial deployment. This paper focuses on select topics in xenon transport, reviews relevant past works, and proposes specific research questions to advance the state of the art in each of the focus areas. Specifically, the paper discusses the issue of xenon solubility in MSRs, the behavior of particulates circulating in MSR fuel salt and its influence on the xenon transport, the possibility of ionization of xenon atoms which changes its effective size and thus affects its mass transport, and finally the issue of circulating void fraction and how it is measured. This work presents specific recommendations for MSR designers to research the limits of Henry's law validity, circulating particulate scrubbers, validity of mass transport coefficients in high radiation fields, and the effects of pump speed on circulating void fraction.

The development of photo-diode dosimeter(PD-2000) for the diagnostic X-ray Energy (X선 진단영역 에너지 측정을 위한 Photo-Diode 선량계(PD-2000)의 개발)

  • Kim, Sung-Chul;Lee, Woo-Chul;Kim, Jung-Min
    • Journal of radiological science and technology
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    • v.23 no.2
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    • pp.27-32
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    • 2000
  • It was produced radiation dosimeter used photo-diodes for which ionization by x-ray was applied and evaluated the value of utility in clinics as compared with ion-chamber. The result obtained were as follows : 1. Comparison of ion-chamber with photo-diode dosimeter's x-ray output by the change of x-ray tube voltage, and the ratio of ion-chamber to diode was $0.96{\sim}1.02$ which was not affected by x-ray beam quality. 2. The ratio of ion-chamber to diode was 0.96 by change of tube current and 0.97 by change of exposure time that is not affected by x-ray quantity. 3. The ratio of ion-chamber to diode was $0.97{\sim}1.04$ by thickness and $0.93{\sim}1.10$ by radiation field that is little affected by second ray quantity. 4. Reproducibility of photo-diode dosimeter was 0.011(CV) and it is a good result. 5. Photo-diode dosimeter was affected by the surface angle of detector over 30 degrees. Produced dosimeter was small, light, and meets good result compared with ionization chamber. It was expected come into wide use in clinic.

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MALDI-MS: A Powerful but Underutilized Mass Spectrometric Technique for Exosome Research

  • Jalaludin, Iqbal;Lubman, David M.;Kim, Jeongkwon
    • Mass Spectrometry Letters
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    • v.12 no.3
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    • pp.93-105
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    • 2021
  • Exosomes have gained the attention of the scientific community because of their role in facilitating intercellular communication, which is critical in disease monitoring and drug delivery research. Exosome research has grown significantly in recent decades, with a focus on the development of various technologies for isolating and characterizing exosomes. Among these efforts is the use of matrix-assisted laser desorption ionization (MALDI) mass spectrometry (MS), which offers high-throughput direct analysis while also being cost and time effective. MALDI is used less frequently in exosome research than electrospray ionization due to the diverse population of extracellular vesicles and the impurity of isolated products, both of which necessitate chromatographic separation prior to MS analysis. However, MALDI-MS is a more appropriate instrument for the analytical approach to patient therapy, given it allows for fast and label-free analysis. There is a huge drive to explore MALDI-MS in exosome research because the technology holds great potential, most notably in biomarker discovery. With methods such as fingerprint analysis, OMICs profiling, and statistical analysis, the search for biomarkers could be much more efficient. In this review, we highlight the potential of MALDI-MS as a tool for investigating exosomes and some of the possible strategies that can be implemented based on prior research.

Development of a device to improve the precision of water surface identification for MeV electron beam dosimetry

  • F. Okky Agassy;Jong In Park;In Jung Kim
    • Nuclear Engineering and Technology
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    • v.56 no.4
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    • pp.1431-1440
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    • 2024
  • The study aimed to develop a laser-based distance meter (LDM) to improve water surface identification for clinical MeV electron beam dosimetry, as inaccurate water surface determination can lead to imprecise positioning of ionization chambers (ICs). The LDM consisted of a laser ranging sensor, a signal processing microcontroller, and a tablet PC for data acquisition. I50 (the water depth at which ionization current drops to 50 % of its maximum) measurements of electron beams were performed using six different types of ICs and compared to other water surface identification methods. The LDM demonstrated reproducible I50 measurements with a level of 0.01 cm for all six ICs. The uncertainty of water depth was evaluated at 0.008 cm with the LDM. The LDM also exposed discrepancies between I50 measurements using different ICs, which was partially reduced by applying an optimum shift of IC's point of measurement (POM) or effective point of measurement (EPOM). However, residual discrepancies due to the energy dependency of the cylindrical chamber's EPOM caused remained. The LDM offers straightforward and efficient means for precision water surface identification, minimizing reliance on individual operator skills.

Profiling of the leaves and stems of Curcuma longa using LC-ESI-MS and HPLC analysis

  • Gia Han Tran;Hak-Dong Lee;Sun-Hyung Kim;Seok Lee;Sanghyun Lee
    • Journal of Applied Biological Chemistry
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    • v.66
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    • pp.338-344
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    • 2023
  • Curcuma longa is a plant belonging to the genus Curcuma and is distributed across various Asian regions. This plant is widely known for its rhizomes, which possess a variety of pharmacological properties. However, although the leaves and stems of this plant also contain several health-promoting secondary metabolites, very few studies have characterized these compounds. Therefore, our study sought to quantify the secondary metabolites from the leaves and stems of Curcuma longa L. (LSCL) using liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) and high-performance liquid chromatography (HPLC). Our LC-ESI-MS analyses detected twenty-one phenolic compounds in the LSCL, among which fifteen compounds were detected via HPLC analysis. Four compounds, namely vanillic acid (0.129 mg/g), p-coumaric acid (0.431 mg/g), 4-methylcatechol (0.199 mg/g), and afzelin (0.074 mg/g) were then quantified. These findings suggest that LSCL is rich in secondary metabolites and holds potential as a valuable resource for the development of functional and nutritional supplements in the future.