This article relates on reversed-phase column technology as the main cause of carryover in the LC-MS/MS analysis of proteomics samples. The separation performance and column carryover was investigated using four capillary columns with different morphologies by monitoring the remaining traces of tryptic peptides of bovine serum albumin in subsequent blank LC-MS runs. The following trend in column carryover was observed: capillary column packed with 3μm porous C18 particles≫2.7μm fused-core C18 packed column>silica C18 monolith≫poly(styrene-co-divinylbenzene) monolith. This is mainly related to the intrinsic properties of the different chromatographic materials, related to surface area and the presence and size of mesopores (stagnant zones where mass transfer is controlled by diffusion). Both isocratic and gradient wash steps with 2-propanol/acetonitrile mixtures were not effective to reduce column carryover. An isocratic wash step using a high acetonitrile percentage or blank gradient reduced carryover with approximately 50%. Nevertheless, it is important to note that effects of column carryover were still observed in a fifth subsequent gradient blank. Although the polymer monolith clearly outperformed the silica materials in terms of carryover, this material exhibited also the lowest loadability, which may be a disadvantage when profiling proteomics mixtures with a broad dynamic range.
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http://dx.doi.org/10.1016/j.jchromb.2012.11.016 | DOI Listing |
J Chromatogr B Analyt Technol Biomed Life Sci
December 2024
Department of Pharmacy, China-Japan Friendship Hospital, Beijing 100029, China. Electronic address:
β-Lactam/β-lactamase inhibitors (BL/BLIs) are widely used in critically ill patients. Recent research has shown the importance of therapeutic drug monitoring (TDM) of BLs, but few studies have highlighted the importance of detecting BLIs in critically ill patients. In our laboratory, we have developed and validated a simple and robust method for the determination of ceftazidime, cefoperazone, piperacillin, avibactam, sulbactam and tazobactam in human plasma by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).
View Article and Find Full Text PDFJ Am Soc Mass Spectrom
December 2024
Institute for Bioscience and Biotechnology Research, National Institute of Standards and Technology and the University of Maryland, College Park, Rockville, Maryland 20850, United States.
Sample carryover is a common problem in hydrogen-deuterium exchange mass spectrometry, particularly because immobilized protease columns cannot withstand the high organic solvent concentrations typically used in liquid chromatography-mass spectrometry (LC-MS) for cleaning. Conventional cleaning methods using injections of guanidine HCl still suffer from carryover and may require four blanks after each sample run to fully remove carryover. We have implemented an additional LC pump to deliver customized wash solutions to protease and enzyme columns, and the associated LC capillaries to eliminate carryover.
View Article and Find Full Text PDFAnal Bioanal Chem
December 2024
Department of Physics and Astronomy, University of Calgary, 2500 University Dr. NW, Calgary, AB, T2N 1N4, Canada.
A fully automated dual-column purification procedure for Zn from biological samples, designed for subsequent Zn isotopic analysis, is presented that utilizes the prepFAST MC™ system (Elemental Scientific), DGA resin (TrisKem International), and TK201 resin (TrisKem International). The procedure developed enables the unattended processing of 20 samples per day and is characterized by low and reproduceable blanks (< 1.5 ng), no carry-over or memory effect, high reusability (> 50 times), high Zn yields 100.
View Article and Find Full Text PDFJ Pharm Biomed Anal
December 2024
Department of Pharmacy, Tongji Hospital, Tongji Medical College, Huazhong University of Science and Technology, Wuhan 430030, China. Electronic address:
Bile acids (BAs), not only promote the absorption of fat-soluble nutrients and regulate the metabolism of multiple substances but also have a potential role as diagnostic and prognostic indicators in a variety of diseases such as cholestasis, hepatocellular carcinoma, and diabetes mellitus. Here, a rapid and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the simultaneous quantification of 50 BAs was developed and validated. Sample preparation included internal standard spiking, followed by protein precipitation, centrifugation, solvent evaporation, and reconstitution.
View Article and Find Full Text PDFJ Chromatogr B Analyt Technol Biomed Life Sci
December 2024
United States Army Medical Research Institute of Chemical Defense, 8350 Ricketts Point Road, Aberdeen Proving Ground, MD 21010, USA. Electronic address:
Chemical warfare nerve agents (CWNAs) are potent and irreversible inhibitors of acetylcholinesterase (AChE). Oxime reactivators are an important part of the standard treatment for CWNA exposure as they can reactivate inhibited AChE. Evaluating the oxime candidates of interest in biological samples requires analytical detection methods and oxime reactivators as a class of compounds have historically been notoriously difficult to isolate, detect and analyze in an analytical laboratory, and there are currently no sensitive or robust analytical detection methods in the literature.
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