Improvements in the performance and availability of commercial instrumentation have made ion mobility-mass spectrometry (IM-MS) an increasingly popular approach for structural analysis ionic species as well separation complex mixtures. Here, a new research instrument is presented which enables experiments, extending current scope IM technology. The based on Waters SYNAPT G2-Si IM-MS platform, with region modified to accept cyclic mobility (cIM) device. cIM consists 98 cm path length,...

The first molecular capsule based on an [Ir(ppy)2]+ unit (ppy = 2-phenylatopyridine) has been prepared. Following the development of a method to resolve rac-[(Ir(ppy)2Cl)2] into its enantiopure forms, homochiral Ir6L4 octahedra where obtained with tritopic 1,3,5-tricyanobenzene. Solution studies and X-ray diffraction show that these capsules encapsulate four six associated counteranions can be exchanged for other anionic guests. Initial photophysical have shown ensemble weakly coordinating...

There is increasing biopharmaceutical interest in oligosaccharides and glycosylation. A key requirement for these sample types the ability to characterize chain length, branching, type of monomers, importantly stereochemistry anomeric configuration. Herein, we showcase multi-function capability a cyclic ion mobility (cIM) separator embedded quadrupole/time-of-flight mass spectrometer (Q-ToF MS). The instrument design enables selective activation mobility-separated precursors followed by cIM...

Abstract Quantum information processing (QIP) would require that the individual units involved—qubits—communicate to other qubits while retaining their identity. In many ways this resembles way supramolecular chemistry brings together molecules into interlocked structures, where assembly has one identity but components are still recognizable. Here a fully modular strategy been link hybrid organic–inorganic [2]- and [3]-rotaxanes larger [4]-, [5]- [7]-rotaxanes. The ring heterometallic...

Ion mobility mass spectrometry (IM-MS) allows separation of native protein ions into "conformational families". Increasing the IM resolving power should allow finer structural information to be obtained and can achieved by increasing length separator. This, however, increases time that spend in gas phase previous experiments have shown initial conformations small proteins lost within tens milliseconds. Here, we report on investigations ion stability using a multipass traveling wave (TW)...

Ion mobility-mass spectrometry (IM-MS) is a powerful technique for structural characterization, e.g., sizing and conformation, particularly when combined with quantitative modeling comparison to theoretical values. Traveling wave IM-MS (TW-IM-MS) has recently become commercially available nonspecialist groups been exploited in the study of large biomolecules, however reliable calibrants anions have not available. Polyoxometalate (POM) species—nanoscale inorganic anions—share many facets...

Ion mobility coupled to mass spectrometry (IM-MS) is widely used study protein dynamics and structure in the gas phase. Increasing energy with which ions are introduced IM cell can induce them unfold, providing information on comparative energetics of unfolding between different proteoforms. Recently, a high-resolution cyclic IM-mass spectrometer (cIM-MS) was introduced, allowing multiple, consecutive tandem experiments (IMn) be carried out. We describe technique for defining detailed...

Mass spectrometry and drift tube ion mobility mass have been used to analyse several isobaric, multicomponent cages yielding information on three dimensional structure, interactions dynamics of assembly in the gas phase.

We present a new variable temperature (VT), high resolution ion mobility (IM) drift tube coupled to commercial mass spectrometer (MS). Ions are generated in an electrospray source with sampling cone interface and two stacked ring RF guides which transfer ions into the analyzer located prior quadrupole time-of-flight spectrometer. The cell can be operated over pressure range of 0.5–3 Torr 150–520 K applied fields typically between 3 14 V cm–1. This makes instrument suitable for rotationally...

In control: Multicomponent stereoisomeric assemblies have been synthesized from asymmetric cyclometalated platinum corner units that exchangeable cis coordination sites with different labilities. A template-free, kinetically controlled approach resulted in the selective formation of trigonal prismatic isomers by changing sequence addition 4,4′-bipyridine (red) and tris(4-pyridyl)triazine (green) to [(LPt)2Cl2] (blue yellow; HL = 2-phenylpyridine). Detailed facts importance specialist readers...

An ion mobility mass spectrometer has been modified to allow optical interrogation of ions with different mass-to-charge ratios and/or mobilities.

The use of charge-reducing reagents to generate lower-charge ions has gained popularity in the field native mass spectrometry (MS) and ion mobility (IM-MS). This is because lower number charged sites decreases propensity for Coulombic repulsions unfolding/restructuring, helping preserve native-like structure. Furthermore, lowering charge state consequently increases mass-to-charge values (m/z), effectively increasing spacing between signals originating from small differences, such as...

Carbohydrate isomers with identical atomic composition cannot be distinguished by mass spectrometry. By separating the ions according to their conformation in gas phase, ion mobility (IM) coupled spectrometry is an attractive approach overcome this issue and extend limits of structural glycosciences. Recent technological developments have significantly increased resolving power separators. One such instrument features a cyclic traveling-wave IM separator integrated quadrupole/time-of-flight...

Adeno-associated viruses (AAVs) are at the forefront of biopharmaceutical development as gene therapy vectors. The successful approval these medicines requires robust characterization including an assessment therapeutic content. Using ion mobility–mass spectrometry (IM-MS) techniques, we determine empty:full capsid ratios and explore structural differences in AAV particles relevant to payload. With drift tube IM-MS, demonstrate that empty capsids, while slightly smaller, present more...

Mass spectrometry is widely used in studying the structures of compounds present crude oil. In this study, a novel mass spectrometer incorporating cyclic ion mobility separator was to obtain tandem spectra oil narrow mass-to-charge ratio (m/z) window. Isolation specific peaks performed by combining quadrupole and separation. As result, differing an m/z value 0.1 could be isolated. Tandem with collision-induced dissociation successfully study chemical isolated ions. A series ions ranging from...

Liquid-liquid phase separation (LLPS) is a process by which biomacromolecules, particularly proteins, condense into dense that resembles liquid droplets. Dysregulation of LLPS implicated in disease, yet the relationship between protein conformational changes and remains difficult to discern. This due high flexibility disordered nature many proteins separate under physiological conditions their tendency oligomerize. Here, we demonstrate ion mobility mass spectrometry (IM-MS) overcomes these...

Abstract In this report, we explored the benefits of cyclic ion mobility (cIM) mass spectrometry in analysis isomeric post‐transcriptional modifications RNA. Standard methyl‐cytidine samples were initially utilized to test ability correctly distinguish different structures sharing same elemental composition and thus molecular mass. Analyzed individually, analytes displayed characteristic arrival times (t D ) determined by positions modifying methyl groups onto common cytidine scaffold....

Native mass spectrometry (MS) is proving to be a disruptive technique for studying the interactions of proteins, necessary understanding functional roles these biomolecules. Recent research expanding application native MS towards membrane proteins directly from isolated preparations or purified detergent micelles. The former results in complex spectra comprising several heterogeneous protein complexes; latter enables therapeutic targets screened against multiplexed compound libraries. In...

Oligosaccharides serve many roles in extant life and may have had a significant role prebiotic chemistry on the early Earth. In both these contexts, structural isomeric diversity among carbohydrates presents analytical challenges necessitating improved separations. Here, we showcase chemical derivatization approach, where 3-carboxy-5-nitrophenylboronic acid (3C5NBA) is used to label vicinal hydroxyl groups, amplifying difference between isomers. We explore applicability of state-of-the-art...

The family of compounds general formula [LnIII4TMII8(OH)8(L)8(O2CR)8(MeOH)y](ClO4)4 {[Gd4Zn8(OH)8(hmp)8(O2CiPr)8](ClO4)4 (1a); [Y4Zn8(OH)8(hmp)8(O2CiPr)8](ClO4)4 (1b); [Gd4Cu8(OH)8(hmp)8(O2CiPr)8](ClO4)4 (2a); [Y4Cu8(OH)8(hmp)8(O2CiPr)8](ClO4)4 (2b); [Gd4Cu8(OH)8(hep)8(O2CiPr)8](ClO4)4 (3a); [Gd4Cu8(OH)8(Hpdm)8(O2CtBu)8](ClO4)4 (4a); [Gd4Cu8(OH)8(ea)8(O2CMe)8](ClO4)4 (5a); [Gd4Ni8(OH)8(hmp)8(O2CEt)8(MeOH)6](ClO4)4 (6a); [Y4Ni8(OH)8(hmp)8(O2CEt)8(MeOH)6](ClO4)4 (6b);...

Liquid extraction surface analysis (LESA) is an ambient sampling technique that allows the of intact proteins directly from tissue samples via mass spectrometry. Integration ion mobility separation to LESA spectrometry workflows has shown significant improvements in signal-to-noise ratios resulting protein spectra and hence number detected. Here, we report use a quadrupole-cyclic mobility-time-of-flight spectrometer (Q-cIM-ToF) for mouse brain rat kidney tissues sampled LESA. Among other...

The identification and localization of isomeric peptide modifications is a critical requirement the biopharmaceutical industry. Despite ability liquid chromatography-mass spectrometry to identify many common post translational modifications, isobaric or racemized peptides confounded by modern mass spectrometry-based techniques. Here, we present novel approach combining chromatography with high-resolution ion mobility system differentiate fragments based upon their mass.

Unter Kontrolle: Stereoisomere Mehrkomponentenaggregate wurden aus asymmetrischen cyclometallierten Platin-Eckbausteinen erhalten, die austauschende cis-Koordinationsstellen mit unterschiedlichen Labilitäten aufweisen. Ein templatfreier, kinetisch kontrollierter Ansatz führte durch Änderung der Reihenfolge Zugabe von 4,4′-Bipyridin (rot) und Tris(4-pyridyl)triazin (grün) zu [(LPt)2Cl2] (blau gelb; H2L=2-Phenylpyridin) selektiv trigonal-prismatischen Isomeren.

The gas phase is an idealized laboratory for the study of protein structure, from which it possible to examine stable and transient forms mass-selected ions in absence bulk solvent. With ion mobility–mass spectrometry (IM-MS) apparatus built operate at both cryogenic elevated temperatures, we have examined conformational transitions that occur monomeric proteins: ubiquitin, lysozyme, α-synuclein as a function temperature source activation. We rationalize experimental observations with...