• Title/Summary/Keyword: Accurate mass measurements

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Unusual Applications of Kendrick Plots: Recalibration and Tolerance

  • Thierry N. J. Fouquet;Orlando Cabarcos
    • Mass Spectrometry Letters
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    • v.14 no.4
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    • pp.173-177
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    • 2023
  • Kendrick plots offer an alternative visualization of mass spectral data which reveals ion series and patterning by turning a mass spectrum into a map, plotting the fractional mass (wrongly called mass defect) as a function of mass-to-charge ratios and ion abundances. Although routinely used for polymer mass spectrometry, two unreported applications of these Kendrick plots are proposed using the program "kendo2": the graphical recalibration of a mass spectrum via the simulation of a theoretical fractional mass and a multi-segment fit; and the rapid evaluation of scan-to-scan variation of accurate mass measurements used as tolerances for the blank subtraction of UPLC-MS data files. Both applications are compatible with any type of high-resolution MS data including LC/GC-MS(/MS).

A Correction Method for the Peak Tailing Backgrounds for Accurate Isotope Ratio Measurements of Uranium in Ultra Trace Levels using Thermal Ionization Mass Spectrometry

  • Park, Jong-Ho;Choi, In-Hee;Park, Su-Jin;Lee, Myung-Ho;Song, Kyu-Seok
    • Bulletin of the Korean Chemical Society
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    • v.32 no.12
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    • pp.4327-4331
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    • 2011
  • A new method in thermal ionization mass spectrometry (TIMS) was developed to correct peak tailing backgrounds in the isotope ratio measurements of uranium in ultra trace levels for higher accuracy. Two different uranium standard reference materials (U005 and U030) were used to construct databases of signal intensities at mass 234 u and mass 236 u, which correspond to the two uranium minor isotopes, and signal intensity of $^{238}U$. Correlations between peak tailing backgrounds and $^{238}U$ were obtained by least-squares regression on calculated backgrounds at mass 234 u and mass 236 u with respect to the signal intensity of $^{238}U$ followed by separation of the peak tails of the two major isotopes of uranium ($^{235}U$ and $^{238}U$), which enables us to obtain a master equation for peak tailing background correction on all kinds of samples. Verification of the correction method was carried out using U010 and IRMM-040a.

High Accuracy Mass Measurement Approach in the Identification of Phospholipids in Lipid Extracts: 7 T Fourier-transform Mass Spectrometry and MS/MS Validation

  • Yu, Seong-Hyun;Lee, Youn-Jin;Park, Soo-Jin;Lee, Ye-Won;Cho, Kun;Kim, Young-Hwan;Oh, Han-Bin
    • Bulletin of the Korean Chemical Society
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    • v.32 no.4
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    • pp.1170-1178
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    • 2011
  • In the present study, the approach of high accuracy mass measurements for phospholipid identifications was evaluated using a 7 T ESI-FTMS/linear ion trap MS/MS. Experiments were carried out for porcine brain, bovine liver, and soybean total lipid extracts in both positive and negative ion modes. In total, 59, 55, and 18 phospholipid species were characterized in the positive ion mode for porcine brain, bovine liver, and soybean lipid extracts, respectively. Assigned lipid classes were PC, PE, PEt, PS, and SM. In the negative ion mode, PG, PS, PA, PE, and PI classes were observed. In the negative ion mode, for porcine brain, bovine liver, and soybean lipid extracts, 28, 34, and 29 species were characterized, respectively. Comparison of our results with those obtained by other groups using derivatization-LC-APCI MS and nano-RP-LC-MS/MS showed that our approach can characterize PC species as effectively as those methods could. In conclusion, we demonstrated that high accuracy mass measurements of total lipid extracts using a high resolution FTMS, particularly, 7T FTMS, plus ion-trap MS/MS are very useful in profiling lipid compositions in biological samples.

Simultaneous Analysis of Conazole Fungicides in Garlic by Q-TOF Mass Spectrometer Coupled with a Modified QuEChERS Method

  • Bong, Min-Sun;Yang, Si-Young;Lee, Seung-Ho;Seo, Jung-Mi;Kim, In-Seon
    • Korean Journal of Environmental Agriculture
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    • v.30 no.3
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    • pp.323-329
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    • 2011
  • BACKGROUND: The conazoles, difenoconazole, diniconazole, hexaconazole, penconazole and tetraconazole are a large class of synthetic fungicides used extensively for foliage and seed treatments in agricultural crops. The extensive use of conazoles has brought concerns on the potentiality of environmental contamination and toxicity. Thus studies on the development of methods for monitoring the conazoles are required. METHODS AND RESULTS: A modified quick, easy, effective, rugged and safe (QuEChERS) method was involved in sample preparation. Quadrapole time of flight mass spectrometer (Q-TOF MS) in electron spray ionization (ESI) mode was employed to determine conazoles in garlic samples. The limit of detection (LOD) and limit of quantification (LOQ) of conazoles by Q-TOF-MS ranged from 0.001 to 0.002 mg/L and 0.002 to 0.005 mg/L, respectively. Q-TOF-MS analysis exhibited less than 2.6 ppm error of accurate mass measurements for the detection of conazoles spiked at 0.05 mg/L in garlic matrix. Recovery values of conazoles fortified in garlic samples at 0.02, 0.05 and 0.1 mg/L were between 79.2 and 106.2% with a maximum 11.8% of standard deviation. No detectable conazoles were found in the domestic market samples by using the Q-TOF-MS method. CONCLUSION(s): High degree of confirmation for conazoles by accurate mass measurements demonstrated that Q-TOF-MS analysis combined with a QuEChERS method may be applicable to simultaneous determination of conazoles in garlic samples.

Adaptive Estimation of Hairy Root Mass Using Conductometry

  • Kim, Ji-Hyeon;Yoo, Young-Je
    • Journal of Microbiology and Biotechnology
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    • v.13 no.5
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    • pp.641-646
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    • 2003
  • An accurate and efficient method for measuring the mass of hairy roots using conductometry is established. A conductivity equation expressed in terms of the concentration of the ion species in the medium is suggested. By using this equation, the effect of the individual ions on the total conductivity can be quantitatively analyzed. An equation for the in situ estimation of the cell growth coefficient for determining the mass of hairy roots is established based on measurements of the nitrogen concentration and conductivity during cultivation. The proposed equation does not require preliminary experiments to determine the cell growth coefficient. Instead, the physiological characteristics of the plant species are reflected by introducing the cellular nitrogen content. Since the cell growth coefficient is determined by measuring the major ionic nutrient concentrations, it is more effective to express the dynamics of an actual culture system. This improved method for determining the mass of hairy roots was successfully utilized in a fed-batch culture system.

Estimation of viscous and Coulomb damping from free-vibration data by a least-squares curve-fitting analysis

  • Slemp, Wesley C.H.;Hallauer, William L. Jr.;Kapania, Rakesh K.
    • Smart Structures and Systems
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    • v.4 no.3
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    • pp.279-290
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    • 2008
  • The modeling and parameter estimation of a damped one-degree-of-freedom mass-spring system is examined. This paper presents a method for estimating the system parameters (damping coefficients and natural frequency) from measured free-vibration motion of a system that is modeled to include both subcritical viscous damping and kinetic Coulomb friction. The method applies a commercially available least-squares curve-fitting software function to fit the known solution of the equations of motion to the measured response. The method was tested through numerical simulation, and it was applied to experimental data collected from a laboratory mass-spring apparatus. The mass of this apparatus translates on linear bearings, which are the primary source of light inherent damping. Results indicate that the curve-fitting method is effective and accurate for both perfect and noisy measurements from a lightly damped mass-spring system.

Computational and experimental forensics characterization of weapons-grade plutonium produced in a thermal neutron environment

  • Osborn, Jeremy M.;Glennon, Kevin J.;Kitcher, Evans D.;Burns, Jonathan D.;Folden, Charles M.III;Chirayath, Sunil S.
    • Nuclear Engineering and Technology
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    • v.50 no.6
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    • pp.820-828
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    • 2018
  • The growing nuclear threat has amplified the need for developing diverse and accurate nuclear forensics analysis techniques to strengthen nuclear security measures. The work presented here is part of a research effort focused on developing a methodology for reactor-type discrimination of weapons-grade plutonium. To verify the developed methodology, natural $UO_2$ fuel samples were irradiated in a thermal neutron spectrum at the University of Missouri Research Reactor (MURR) and produced approximately $20{\mu}g$ of weapons-grade plutonium test material. Radiation transport simulations of common thermal reactor types that can produce weapons-grade plutonium were performed, and the results are presented here. These simulations were needed to verify whether the plutonium produced in the natural $UO_2$ fuel samples during the experimental irradiation at MURR was a suitable representative to plutonium produced in common thermal reactor types. Also presented are comparisons of fission product and plutonium concentrations obtained from computational simulations of the experimental irradiation at MURR to the nondestructive and destructive measurements of the irradiated natural $UO_2$ fuel samples. Gamma spectroscopy measurements of radioactive fission products were mostly within 10%, mass spectroscopy measurements of the total plutonium mass were within 4%, and mass spectroscopy measurements of stable fission products were mostly within 5%.

Supermassive Black Hole Masses of ~500k QSOs from the Sloan Digital Sky Survey

  • Taak, Yoon Chan;Im, Myungshin
    • The Bulletin of The Korean Astronomical Society
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    • v.44 no.2
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    • pp.77.2-77.2
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    • 2019
  • Measurements of supermassive black hole (SMBH) masses are crucial in studying the co-evolution of SMBHs and their host galaxies. Although reverberation mapping is the most accurate method known to date, this requires spectroscopic monitoring over long periods. Thus, the current sample barely reaches three digits. The virial method, on the other hand, uses emission-line and continuum properties from a single spectrum to estimate the SMBH mass; hence the name single-epoch method. The Sloan Digital Sky Survey (SDSS) has observed spectra of almost all quasi-stellar objects (QSOs) discovered so far. Building on previous studies, using the single-epoch method, we estimate the SMBH masses of more than 500,000 QSOs from the SDSS DR14 Quasar Catalog. This increases the mass-estimated SMBH sample almost by a factor of two, and especially more for the low-mass regime, which was the main target of SDSS-IV (eBOSS).

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On the control of vibratory MEMS gyroscopes

  • Choura, S.;Aouni, N.;El-Borgi, S.
    • Smart Structures and Systems
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    • v.6 no.7
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    • pp.793-810
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    • 2010
  • This paper addresses the control issue of vibratory MEMS-based gyroscopes. This study considers a gyroscope that can be modeled by an inner mass attached to an outer mass by four springs and four dampers. The outer mass itself is attached to the rotating frame by an equal number of springs and dampers. In order to measure the angular rate of the rotating frame, a driving force is applied to the inner mass and the Coriolis force is sensed along the y-direction associated with the outer mass. Due to micro-fabrication imperfections, including anisoelasticity and damping effects, both gyroscopes do not allow accurate measurements, and therefore, it becomes necessary to devise feedback controllers to reduce the effects of such imperfections. Given an ideal gyroscope that meets certain performance specifications, a feedback control strategy is synthesized to reduce the error dynamics between the actual and ideal gyroscopes. For a dual-mass gyroscope, it is demonstrated that the error dynamics are remarkably decreased with the application of four actuators applied to both masses in the x and y directions. It is also shown that it is possible to reduce the error dynamics with only two actuators applied to the outer mass only. Simulation results are presented to prove the efficiency of the proposed control design.

MS Platform for Erythropoietin Glycome Characterization

  • Seo, Youngsuk;Kim, Unyong;Oh, Myung Jin;Yun, Na Young;An, Hyun Joo
    • Mass Spectrometry Letters
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    • v.6 no.3
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    • pp.53-58
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    • 2015
  • Recombinant erythropoietins (EPOs) are an important class of biotherapeutics that stimulate red blood cell production. The quality, safety, and potency of EPO variants are determined largely by their glycosylation, which makes up nearly half their mass. Thus, detailed glycomic analyses are important to assess biotherapeutic quality and establish the equivalency of biosimilar EPOs now coming to market. High-resolution mass spectrometry (MS) has recently emerged as the premier tool for glycan analysis in EPOs. Using the accurate mass measurements provided by high-resolution MS, the compositions of even large, complex glycans can easily be determined. When combined with a nano-LC separation, differentiation of structural isomers also becomes a possibility. These components, together, provide a comprehensive picture of biotherapeutic glycosylation. In this review, we provide an overview of MS-based analytical platform for glycomic characterization of EPO biotherapeutics and biosimilars.