Journal of Mass Spectrometry : JMS

Isotope dilution ultrahigh-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) is commonly used for trace analysis of polyfluoroalkyl and perfluoroalkyl substances (PFAS) in difficult matrices. Commercial nontargeted analysis of major PFAS where relative concentrations are obtained cost effectively is rapidly emerging and is claimed to provide comparable results to that of absolute quantification using matrix matched calibration and isotope dilution UHPLC-MS/MS. However, this remains to be demonstrated on a large scale...

Gold nanoparticles (AuNPs) synthesized in the 1-3 nm range have a specific number of gold core atoms and outer protecting ligands. They have become one of the "hot topics" in recent decades because of their interesting physical and chemical properties. The characterization of their structures is usually achieved by crystal X-ray diffraction although the structures of some AuNPs remain unknown because they have not been successfully crystallized. An alternative method for studying the structure of AuNPs is electrospray ionization-ion mobility-tandem mass spectrometry (ESI-IM-MSMS)...

This study describes a novel application for sandpaper spray ionization mass spectrometry (SPS-MS), to examine the surface of maple tree (Acer sp.) leaves. By comparing mass spectrometry fingerprints, healthy leaves from those infected with powdery mildew and Rhytisma acerinum were distinguished. Leaves were grated with sandpaper, cut into triangles, and placed before the mass spectrometer, with the addition of a methanol-formic acid solution. Multivariate statistical analysis categorized the samples into three groups...

This work aimed to simplify and improve the process of binding monoclonal antibodies (mAbs) covalently to filter paper for use in dried blood spot sampling, enabling instant capture of protein biomarkers for targeted protein determination. Incorporating the necessary immunocapture sample preparation step in the initial sampling stage saves time and reduces the workload. The biomarker human chorionic gonadotropin (hCG) was used as the model analyte. The antibody-based paper samplers were prepared by functionalizing paper discs (6 mm) through a simple reaction using divinyl sulfone (DVS)...

Peptides with a molecular mass between 2 and 10 kDa that are prohibited in elite sports usually require dedicated sample preparation and mass spectrometric detection that commonly cannot be combined with other (lower molecular mass) substances. In most instances, the physicochemical differences are too significant to allow for a generic analytical procedure. A simplification of established and comparably complex analytical approaches is therefore desirable and has been accomplished in the context of this study...

Criminal practices in which an individual becomes vulnerable and prone to sexual assault after ingesting drinks spiked with doping substances have become a social concern globally. As forensic protocols require a multi-tiered strategy for chemical evidentiary analysis, the backlog of evidence has become a significant problem in the community. Herein, a fast, sensible, and complementary dual analytical methodology was developed using a single commercial paper substrate for surface-enhanced Raman spectroscopy (SERS) and paper spray mass spectrometry (PS-MS) analysis to identify psychotropic substances added to alcoholic beverages irrefutably...

Decarboxylation is known to be the major fragmentation pathway for the deprotonated carboxylic acids in collision-induced dissociation (CID). However, in the CID mass spectrum of deprotonated benzoic acid (m/z 121) recorded on a Q-orbitrap mass spectrometer, the dominant peak was found to be m/z 93 instead of the anticipated m/z 77. Based on theoretical calculations, 18 O-isotope labeling and MS3 experiments, we demonstrated that the fragmentation of benzoate anion begins with decarboxylation, but the initial phenide anion (m/z 77) can react with trace O2 in the mass analyzer to produce phenolate anion (m/z 93) and other oxygen-containing ions...

Novel mass spectrometry (MS) based analytical platforms have enabled scientists to detect and quantify molecules within biological and environmental samples more accurately. Novel MS instrumentation starts as a prototype and, after years of development, can become a commercial product to be used by the larger MS community. Without the initial prototype, many MS-based instruments today would not be produced. Additionally, biotechnology companies are the main drivers for research, development, and production of novel instruments, but the tools for prototyping instrumentation have never been more accessible...

Increased acceptance of cannabis containing the psychoactive component, Δ9-tetrahydrocannabinol (THC), raises concerns about the potential for impaired drivers and increased highway accidents. In contrast to the "breathalyzer" test, which is generally accepted for determining the alcohol level in a driver, there is no currently accepted roadside test for THC in a motorist. There is a need for an easily collectible biological sample from a potentially impaired driver coupled with an accurate on-site test to measure the presence and quantity of THC in a driver...

High-resolution mass spectrometry and ion mobility spectrometry provide additional confidence in biological marker discovery and elucidation by adding additional peak capacity through physiochemical separation orthogonal to chromatography. Sophisticated analytical techniques have proved valuable in the identification of human skin surface chemicals used by vector mosquitoes to find their human host. Polydimethylsiloxane (PDMS) was used as a non-invasive passive wearable sampler to concentrate skin surface non-volatile and semi-volatile compounds prior to solvent desorption directly in an LC vial, thereby simplifying the link between extraction and analysis...

The presence of coccidiostats in meat products represents an important topic because of the animal administration of these substances, authorized as feed additives for targeted species, in order to prevent and inhibit coccidiosis. Coccidiostats include both ionophores and synthetic molecules characterized by different chemical-physical properties such as polarity. Meat is a matrix characterized by many interfering compound groups, such as proteins, phospholipids, and fats. High-performance liquid chromatography (HPLC) coupled to mass spectrometry (MS) analysis allows the required selectivity and sensitivity for discriminating analytes and matrix interferences...

Mass spectrometry is widely employed in various analytical fields for both compound identification and quantification. While in the case of compound identification, the high-resolution instrument has increased selectivity and characterization efficiency; in the case of quantitative analysis, some critical tasks actually remain. In particular, different compounds exhibit different ionization efficiency, and this introduces the need to have a calibration standard for each analyte. In this paper, we present a new elaborative data technology, which makes it possible to standardize calibration between different instruments and molecules, making it absolute...

Full-thickness cutaneous trauma, due to the lack of dermis, leads to difficulty in epithelialization by keratinocytes, developing a fibrotic scar, with less elasticity than the original skin, which may have disorders in predisposed individuals, resulting in hypertrophic scar and keloids. Biomedical materials have excellent characteristics, such as good biocompatibility and low immunogenicity, which can temporarily replace traditional materials used as primary dressings. In this work, we developed two dermal matrices based on Nile tilapia collagen, with (M_GAG) and without (M) glycosaminoglycans, using a sugarcane polymer membrane as a matrix support...

Fentanyl and its non-pharmaceutical analogues (NPFs) are potent synthetic opioids, traditionally used for pain management, with ever-increasing illicit uses. Tightening the regulation for known fentanyls leads to new synthetic analogues in the opioid market. Furthermore, the Organization for the Prohibition of Chemical Weapons (OPCW) has recently issued a decision regarding aerosolized use of central nervous system (CNS)-acting agents, such as fentanyl and its analogues, under the concern that these materials could be misused for terror or war purposes...

Acetylation of amino acids is important in the molecular biology and biochemistry because they are part of several metabolic pathways. N-acetyl amino acids can form through degradation of N-acetyl proteins or direct acetylation of amino acids by specific enzymes. Acetylation of α-amino acids can be either on the alpha -NH2 or on the side-chain functional group, where both the acetyl products are isomeric and can show different biological roles. Theoretically, all proteinogenic α-amino acids are expected to undergo acetylation and they can be a part of metabolome...

Beta blockers are a class of drugs commonly used to treat heart-related diseases; they are also regulated under the World Anti-Doping Agency. Tandem mass spectrometry is often used in the pharmaceutical industry, clinical analysis laboratory, and antidoping laboratory for detection and characterization of drugs and their metabolites. A deeper chemical understanding of dissociation pathways may eventually lead to an improved ability to predict tandem mass spectra of compounds based strictly on their chemical structure (or vice versa), which is especially important for characterization of unknowns such as emerging designer drugs or novel metabolites...

The problem of modeling the mass peak shape of a quadrupole mass filter (QMF) with round rods is considered. A number of factors leading to the degradation of the mass peak shape are studied, namely, displacement of the electrodes with respect to their original position, changes in the diameter of the electrodes, and asymmetry of the supply potentials. Decomposition of the rod set field on multipole fields allows to obtain an analytical representation of the ion motion equations. Simulations have shown that a parallel shift of one or two electrodes leads to a shift of the peak along the mass number axis and dips at the peak apex...

Dinitrotoluenes (DNTs) and nitrotoluenes (NTs) are found in the environment as metabolites of trinitrotoluene (TNT). When acetone is used as the solvent/eluent in atmospheric pressure chemical ionization-mass spectrometry (APCI-MS), the reactant ion is [2Acetone + O2 ]•- for the negative ion mode. The reactant ion reacts with an analyte to produce M•- and/or [M - H]- under atmospheric pressure. In this study, ionization behaviors of NT (2-, 3-, and 4-NTs) and DNT isomers (2,3-, 2,4-, and 2,6-DNTs) by reactions with [2Acetone + O2 ]•- were investigated...

Saliva is a body fluid that is much easier to collect and analyze than blood. Thus, saliva analysis for the detection of delta 9-tetrahydrocannabinol (delta 9-THC) can serve as a tool for law enforcement agents to detect cannabis consumption by drivers. Fast saliva analysis for the presence of delta 9-THC and/or cannabidiol (CBD) is described with both gas chromatography-mass spectrometry (GC-MS) with Cold electron ionization (EI) with good separation and in 10 min and/or with Open Probe Fast GC-MS with Cold EI in under 1 min full analysis cycle time...

Ribociclib is a cyclin-dependent kinase (CDK4/6) inhibitor and is a standard of care for treating metastatic breast cancer. The drug has moderate oral bioavailability and exhibits permeability-controlled absorption. Novel formulations to enhance ribociclib pharmacokinetics are being developed and tested in rats. This requires developing analytical assays for quantifying ribociclib monitoring in rat plasma. We present a fully validated, sensitive, and simple LC-MS/MS method for measuring ribociclib in rat plasma...