Article
Chemistry, Inorganic & Nuclear
Maximilian Muhr, Patricia Heiss, Max Schuetz, Raphael Buehler, Christian Gemel, Mathias H. Linden, H. Bernhard Linden, Roland A. Fischer
Summary: The new setup combining a ThermoFisher Exactive Plus Orbitrap Mass Spectrometer with a LIFDI source allows for the analysis of sensitive organometallic complexes. The detection of oxygen traces and mass spectrometric analysis of Cu/Al cluster mixtures are successfully conducted using this setup.
DALTON TRANSACTIONS
(2021)
Article
Chemistry, Analytical
Qiong Liang, Siyu Liu, Wei Xu, Yanbing Zhai
Summary: In this study, a capillary-in-capillary electrospray ionization (CC-ESI) source was developed for spontaneous liquid sampling and quantitative analysis based on the capillary phenomenon and electrospray ionization mass spectrometry (ESI-MS). The CC-ESI had advantages of cheap price, high portability, disposability, quantitation capability, and adequate sensitivity.
ANALYTICAL CHEMISTRY
(2023)
Article
Chemistry, Analytical
Xiaoping Zhang, Xiang Ren, Yuan Zhong, Konstantin Chingin, Huanwen Chen
Summary: The study detected ketones in exhaled breath using mass spectrometry and developed a fast, sensitive, noninvasive method for ketone analysis. Results showed higher levels of acetone in the breath of smokers compared to non-smokers.
Article
Food Science & Technology
Jinlin Li, Xiangfei Hu, Chengwei Yu, Kai Zeng, Shuanglong Wang, Zongcai Tu
Summary: A rapid characterization method was developed for the unstable hydroperoxyl/hydroxyl group position of lipid hydroperoxides/hydroxides. Eight hydroperoxides/hydroxides derived from standards were identified using nano electrospray ionization coupling with tandem mass spectrometer (NanoESI-MS/MS) and verified by LC-TOF-MS/MS. The method could be used for the instantaneous discrimination of UFAs hydro-peroxides/hydroxides in various edible oils without extraction enrichment (<= 4 min/per sample), providing specific insights to conventional lipid oxidation research.
LWT-FOOD SCIENCE AND TECHNOLOGY
(2023)
Article
Chemistry, Analytical
Daiki Asakawa, Hajime Mizuno, Eiji Sugiyama, Kenichiro Todoroki
Summary: The study focused on the impact of liquid chromatography-tandem mass spectrometry interfaced with electrospray ionization on tryptophan-derived metabolites, revealing fragmentation during ESI. The quantitative analysis used multiple reaction monitoring technology and proposed a method for high sensitivity analysis.
Article
Biochemical Research Methods
Khoa Hoang, Sarah Trimpin, Charles N. McEwen, Milan Pophristic
Summary: A new vacuum ionization source has been developed to provide fast multisample introduction to vacuum and rapid sequential ionization, duplicating the sensitivity and robustness of probe device. This source design allows for ionization using either vMAI or vMALDI, with the ability to switch between ionization modes in seconds. The combination of these two ionization methods improves molecular analyses of sample composition, with the potential for low-cost high-throughput automation.
JOURNAL OF THE AMERICAN SOCIETY FOR MASS SPECTROMETRY
(2021)
Article
Chemistry, Analytical
Derik R. Heiss, Abraham K. Badu-Tawiah
Summary: This study combines accelerated droplet chemistry with conventional LC-MS using a modified electrospray interface (contained-ESI) for online and automated separation, derivatization, and detection of saccharides. The method demonstrates high sensitivity and analytical efficiency, allowing for the detection of abnormalities in saccharide profiles in volume-limited samples.
ANALYTICAL CHEMISTRY
(2022)
Article
Biochemical Research Methods
Cristina Arciniega, Kenneth P. Garrard, Jacob P. Guymon, Jeffrey G. Manni Sr, Alex Apffel, John C. Fjeldsted, David C. Muddiman
Summary: High-throughput screening (HTS) is a technique used by pharmaceutical companies to quickly screen multiple compound libraries for potential drugs. Mass spectrometry (MS) is a popular choice for HTS because it can analyze hundreds to thousands of compounds simultaneously without additional chemical derivatization. In this study, we developed an infrared matrix-assisted laser desorption electrospray ionization (IR-MALDESI) source coupled directly to an Agilent 6545 mass spectrometer for direct analysis from well plates. The source used a laser operating at 100 Hz with high ionization efficiency, and a metal capillary was constructed to improve ion transmission and sensitivity.
JOURNAL OF MASS SPECTROMETRY
(2023)
Article
Biochemical Research Methods
Shubhashis Chakrabarty, Weilin L. Shelver, David J. Smith
Summary: This study demonstrates the utility of ESII-MS/MS for quantitatively determining analytes in complex animal matrices without chromatographic separation. ESII-MS/MS provides rapid, sensitive, and accurate analyses of veterinary drugs and environmental contaminants from complex matrices without the need for chromatographic separation.
JOURNAL OF THE AMERICAN SOCIETY FOR MASS SPECTROMETRY
(2021)
Article
Chemistry, Analytical
Weini Huang, Wenya Shao, Yin Ji, Heming Li, Jiajing Chen, Zian Lin
Summary: In this study, an imine-linked-based covalent organic framework (TPB-TFBCOF) was synthesized and used as a solid-phase microextraction (SPME) probe for the efficient enrichment and monitoring of carbamazepine (CBZ) and carbamazepine-10,11-epoxide (CBZEP). The combination of the TPB-TFB-COF-based SPME probe and electrospray ionization mass spectrometry system (ESI/MS) enables rapid screening and sensitive monitoring of the target analytes. The method exhibits good linearity, low detection limits, high enrichment factors, and reliable repeatability.
Review
Chemistry, Multidisciplinary
Xiaoxiao Ma, Wenpeng Zhang, Zishuai Li, Yu Xia, Zheng Ouyang
Summary: Lipids play crucial roles in biological processes and the precise determination of the location and quantity of lipid chains is essential for understanding biological systems. Mass spectrometry has become a powerful tool for lipid analysis, but the structural characterization and quantitation of lipid isomers remain challenging.
ACCOUNTS OF CHEMICAL RESEARCH
(2021)
Article
Biochemical Research Methods
Jiahao Yuan, Weini Huang, Wei Tong, Zihan Chen, Heming Li, Jiajing Chen, Zian Lin
Summary: Tricyclic antidepressants (TCAs) are commonly used as first-line drugs for the clinical treatment of depression, and it is crucial to monitor their concentrations in biological samples. In this study, a novel COF-based SPME probe was developed for rapid and sensitive determination of TCAs in various biosamples. The probe exhibited high specific surface area, regular pores, good hydrophobicity, and stability, resulting in efficient enrichment for TCAs. The combination of the probe with ESI/MS system showed low LODs, high enrichment factors, and low RSDs, demonstrating the promising applicability of the TPB-DVA-COF-SPME-ESI/MS as a powerful tool for drug monitoring.
JOURNAL OF CHROMATOGRAPHY A
(2023)
Article
Pharmacology & Pharmacy
Wei Zhou, Martyna N. Wieczorek, Runshan Will Jiang, Janusz Pawliszyn
Summary: The direct coupling of solid-phase microextraction (SPME) to mass spectrometry (MS) has proven to be effective for the fast screening and quantitative analysis of compounds in complex matrices. The development of three novel SPME-MS techniques and a comprehensive comparison of these technologies were conducted. The comparative analysis helps determine the best option for various applications.
JOURNAL OF PHARMACEUTICAL ANALYSIS
(2023)
Article
Instruments & Instrumentation
M. Salvi, N. N. Uma, Hemanth Dinesan, Abheek Roy, S. Sunil Kumar
Summary: A linear 16-pole ion trap-based experimental setup has been designed to investigate the photophysics of biomolecules in the gas phase. The instrument's versatility and capability are showcased by controlling ion energy and mass selection.
REVIEW OF SCIENTIFIC INSTRUMENTS
(2023)
Article
Biochemical Research Methods
Mathieu Galmiche, Anais Rodrigues, Estelle Motsch, Olivier Delhomme, Yannis-Nicolas Francois, Maurice Millet
Summary: This study introduces a mass spectrometry analysis method based on pseudo-MRM for trace-level determination of non-polar polycyclic aromatic hydrocarbons (PAHs). The results show that pseudo-MRM offers higher sensitivity and selectivity compared to classic MRM for certain mass spectrometers.
RAPID COMMUNICATIONS IN MASS SPECTROMETRY
(2022)
Review
Chemistry, Multidisciplinary
Robin N. Perutz, Sylviane Sabo-Etienne, Andrew S. Weller
Summary: This article introduces the concept of sigma-CAM and a new approach to reaction mechanisms. It focuses on the characteristics and dynamic rearrangements of sigma-bond complexes, providing examples of the sigma-CAM mechanism supported by experimental and computational evidence. The authors also critically compare alternative mechanisms for metathesis of metal-element bonds.
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION
(2022)
Article
Biochemical Research Methods
Anuj Joshi, Charles Killeen, Tanner Thiessen, Harmen S. Zijlstra, J. Scott McIndoe
Summary: Mass spectrometry is a powerful tool in chemistry, but its sensitivity can be a challenge when studying highly reactive organometallic compounds. Creative solutions have been developed to handle reactive samples, including selecting appropriate ionization methods and preventing decomposition caused by oxygen or moisture.
JOURNAL OF MASS SPECTROMETRY
(2022)
Article
Chemistry, Multidisciplinary
James J. J. Race, Alex Heyam, Matthew A. A. Wiebe, J. Diego-Garcia Hernandez, Charlotte E. E. Ellis, Shixing Lei, Ian Manners, Andrew S. S. Weller
Summary: An amphiphilic block copolymer of polyphos-phinoborane has been synthesized using a mechanism-led strategy and its self-assembly behavior has been studied.
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION
(2023)
Article
Chemistry, Applied
Antonio Rosales Martinez, Lourdes Enriquez, Martin Jaraiz, Tanner Thiessen, Jaspreet Sidhu, J. Scott McIndoe, Ignacio Rodriguez-Garcia
Summary: Reduction of Cp2TiCl2 with manganese dust in dry THF results in a green solution that turns deep blue when traces of water are added. Mass spectrometric analysis and DFT calculations were used to gain a better understanding of the species present after water interacts with reduced Cp2TiCl2. The deep blue solution serves as a convenient visual indicator for qualitative determination of water in THF.
APPLIED ORGANOMETALLIC CHEMISTRY
(2023)
Article
Chemistry, Physical
M. Arif Sajjad, Stuart A. Macgregor, Andrew S. Weller
Summary: Non-covalent interactions surrounding cationic Rh s-alkane complexes in crystal structures were analyzed using QTAIM and IGMH approaches. Both structures showed the cations residing in an octahedral array of [BAr4F](-) anions, with the [1-NBA](+) cation system exhibiting more C-HF contacts to the anions. QTAIM and IGMH analyses revealed the strongest atom-atom non-covalent interactions between the cation and anion. The IGMH approach highlighted the directionality of C-HF contacts and the significance of C-Hπ interactions.
FARADAY DISCUSSIONS
(2023)
Article
Chemistry, Multidisciplinary
Tobias Kramer, F. Mark Chadwick, Stuart A. Macgregor, Andrew S. Weller
Summary: This study uses density functional theory calculations to model the selective exo-H/D exchange in a Rh sigma-alkane complex. The results show that exo-H/D exchange is kinetically more accessible than endo-H/D exchange, and the solid-state environment significantly affects the calculated energetics.
HELVETICA CHIMICA ACTA
(2023)
Article
Chemistry, Multidisciplinary
Matthew R. Gyton, Cameron G. Royle, Simon K. Beaumont, Simon B. Duckett, Andrew S. Weller
Summary: The heterogeneous solid-gas reactions of crystals of [Rh(L-2)(propene)][BAr4F] with H-2 and different alkenes and alkynes were investigated using gas-phase NMR spectroscopy. The study provides insights into catalytic pairwise para-H-2 transfer, molecular-level changes in the crystalline catalyst, and the production of high-quality gas-phase spectra. The results reveal the formation of dimeric [Rh(L-2)(H)(mu-H)](2)[BAr4F](2) upon reaction with H-2 and the conversion of NMR silent para-H-2 to NMR active ortho isomer. The hydrogenation of propene and other alkenes and alkynes showed high levels of initial polarization and strong PHIP effects.
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY
(2023)
Article
Chemistry, Multidisciplinary
Mathew J. Cross, Claire N. Brodie, Dana G. Crivoi, Joe C. Goodall, David E. Ryan, Antonio J. Martinez-Martinez, Alice Johnson, Andrew S. Weller
Summary: The formation of nanoparticles during the selective production of polyaminoborane [H2BNMeH](n) using [Rh(L1)(η(2):η(2)-H3B center dot NRH2)] [OTf] and [Rh(L1)(NMeH2)][OTf] as catalysts is observed, but there is ambiguity as to whether the catalysis is solely nanoparticle promoted or if there is a molecular homogeneous component.
CHEMISTRY-A EUROPEAN JOURNAL
(2023)
Article
Chemistry, Multidisciplinary
Joe C. Goodall, M. Arif Sajjad, Emily A. Thompson, Samuel J. Page, Adam M. Kerrigan, Huw T. Jenkins, Jason M. Lynam, Stuart A. Macgregor, Andrew S. Weller
Summary: The group 7 complexes [M(& kappa;(3)-2,6-(R2PO)(2)C5H3N)(CO)(2)L][BAr4F] [M = Mn, R = Pr-i, L = THF; M = Re, R = Bu-t, L = vacant site] undergo solid-gas reactivity with CO in the crystals to form THF substitution products or CO addition products. The [BAr4F] anions show large, local, adaptive changes for M = Mn, while the changes are smaller and remote to the site of reactivity for M = Re.
CHEMICAL COMMUNICATIONS
(2023)
Article
Chemistry, Physical
Charles Killeen, Jie Liu, Harmen S. S. Zijlstra, Florian Maass, James Piers, Reid Adams, Allen Oliver, J. Scott McIndoe
Summary: Ring-closing metathesis (RCM) is a versatile method for forming cyclic structural elements. Real-time analysis using electrospray ionization mass spectrometry (ESI-MS) was applied to study the RCM reaction, revealing the presence of by-products and the decomposition of the catalyst. Isomerization reactions play a significant role in affecting the yield of the desired product, especially in slow RCM reactions.
CATALYSIS SCIENCE & TECHNOLOGY
(2023)
Article
Chemistry, Multidisciplinary
Oliver P. E. Townrow, Andrew S. Weller, Jose M. Goicoechea
Summary: Using Zintl clusters as starting materials, eleven- and twelve-vertex homo- and hetero-multimetallic clusters were synthesized through reactions and stepwise methods. The proposed mechanism based on density functional theory calculations explains the formation of these clusters. These studies provide important insights into the assembly mechanisms of Zintl clusters in solution.
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION
(2023)
Article
Chemistry, Multidisciplinary
Peter J. H. Williams, Charles Killeen, Ian C. Chagunda, Brett Henderson, Sofia Donnecke, Wil Munro, Jaspreet Sidhu, Denaisha Kraft, David A. Harrington, J. Scott McIndoe
Summary: Continuous addition kinetic elucidation (CAKE) is a method to address the challenges in catalytic reactions by continuously injecting a catalyst and monitoring reaction progress, reducing workload and improving reproducibility.
Review
Chemistry, Multidisciplinary
Gilian T. Thomas, Sofia Donnecke, Ian C. Chagunda, J. Scott McIndoe
Summary: Pressurized sample infusion is a simple and effective method for continuously introducing a solution to a mass spectrometry source, allowing real-time data acquisition. It is applicable for various reactions that require real-time information.
Article
Education, Scientific Disciplines
Jaspreet Sidhu, J. Scott McIndoe
Summary: Understanding molecular scale is crucial for chemistry students. Using 3D printing to scale up molecules allows students to better comprehend the difference between molecular scale and handheld scale.
CHEMISTRY TEACHER INTERNATIONAL
(2022)
Article
Chemistry, Multidisciplinary
Oliver P. E. Townrow, Simon B. Duckett, Andrew S. Weller, Jose M. Goicoechea
Summary: The ligand exchange reactions lead to clusters with coordinatively unsaturated rhodium(i) centers, which can act as catalysts for H/D exchange and alkene isomerisation. Protonation of these clusters results in cationic rhodium-hydride complexes, showing their activity in both H-H and C-H bond activation processes.
