Averaging of results derived from different, simultaneously acquired mass transitions in ID-LC-MS/MS - Potential impact on measurement imprecision
CLINICAL MASS SPECTROMETRY
Authors: Schuster, Carina; Habler, Katharina; Vogeser, Michael
Abstract
Background: LC-MS/MS allows for many measurands monitoring different mass transitions simultaneously. So far, such alternative mass transitions are usually assessed as "quantifier and qualifier ions" in order to rule out interferences in individual samples. However, quantification can also be based on assessment of alternative mass transitions for both the measurand and its internal standard, with two distinct results for one injection of an individual sample. These paired results can be averaged. The aim of this study was to determine the potential impact of this averaging approach on measurement imprecision. Methods: We studied the impact of averaging results from different transitions for four exemplary measurands (linezolid (LIN), piperacillin (PIP), voriconazole (VOR), ethylglucuronide (ETG)). Intra-batch studies were performed with 21 injections of single clinical samples in sequence for each analyte (LIN, PIP, VOR), and a between-batch study with evaluation of data from routine QC samples from 20 series over 20 weeks (ETG). CVs and their confidence intervals were assessed comparatively for quantification based on single transitions, and for averaged results from these two transitions, respectively. Results: In all data sets, we observed lower CVs for the averaged results compared to the results obtained from single mass transitions. CVs from averaged results were up to 39.4% lower compared to the CVs observed for results obtained from single transitions for the respective measurands. Conclusion: Averaging of quantification results obtained from separate mass transitions acquired simultaneously in ID-LC-MS/MS seems to have the potential to minimize the measurement imprecision for different measurands in short- and long-term settings. (C) 2020 The Association for Mass Spectrometry: Applications to the Clinical Lab (MSACL). Published by Elsevier B.V. All rights reserved.
On the formation of temperature-induced defects at the surface of TEM specimens prepared from TiAl using high-energy Gallium and low-energy Argon ions
PHILOSOPHICAL MAGAZINE
Authors: Froebel, Ulrich; Laipple, Daniel
Abstract
Specimens for transmission electron microscopic (TEM) investigations were prepared from gamma titanium aluminide alloys with Gallium and Argon ions using a focused ion beam (FIB) and a precision ion polishing system (PIPS). Preparation to electron transparency by Gallium ions alone leads to the formation of crystalline platelets of the alpha titanium phase at the specimen surfaces, revealed through conventional and high resolution (HR) TEM analysis. The platelets are assumed to precipitate from priorly formed amorphous layers. The required crystallisation temperature of about 480 degrees C is generated through the ion bombardment implying that the gamma titanium aluminides can be heated substantively during sputtering. The primary reason for this is the restricted transfer of heat away from the beam impact point when the specimen thickness comes close to the beam diameter. The formation of the platelets can be avoided by terminating the Gallium ion treatment prior to that, while providing for a sufficient thermal bonding of the specimen to the grid as well and polishing off the remaining material by Argon ions, which are much less focused and less energetic, so that the local heat peaks are reduced.