Mass spectrometry of peptides and proteins using digestion by a grape cysteine protease at pH 3
AbstractCysteine protease from grapevine (Vitis vinifera) belongs to those resistant proteins, which survive the process of vinification and can therefore be detected as wine components. Its amino acid sequence shows a homology to other members of the papain family but the enzyme has only partially been explored so far. In order to get more biochemical information with the help of MS, wine proteins were collected by ultrafiltration and separated by gel permeation chromatography. The purified enzyme surprisingly displayed a high molecular mass value of around 200 kDa, indicating a possible oligomeric status and aggregation,...
Source: Journal of Mass Spectrometry - October 11, 2019 Category: Chemistry Authors: Zden ěk Perutka, Marek Šebela Tags: SPECIAL ISSUE ‐ RESEARCH ARTICLE Source Type: research

Identification of bifucosylated glycoforms using low ‐energy CID spectra
AbstractWe have used tandem mass spectrometry (MS/MS) ‐based analysis of glycopeptides in order to identify the composition and structure of rare glycoforms. The results illustrate utility of low‐energy MS/MS for structure identification. We have shown the presence of bifucosylated and trifucosylated glycoforms in human α‐1‐acid glycoprotein ( AGP), a major plasma glycoprotein. Fucosylation in the case of AGP always occurs on the antennae; core fucosylation was not observed. (Source: Journal of Mass Spectrometry)
Source: Journal of Mass Spectrometry - October 9, 2019 Category: Chemistry Authors: Andr ás Ács, Lilla Turiák, Ágnes Révész, Károly Vékey, László Drahos Tags: RESEARCH ARTICLE Source Type: research

CTP synthetase activity assay by liquid chromatography tandem mass spectrometry in the multiple reaction monitoring mode
AbstractCytidine 5' ‐triphosphate synthetase (CTPS) is known to be a central enzyme in thede novo synthesis of CTP. We have recently demonstrated that a deficiency in CTPS1 is associated with an impaired capacity of activated lymphocytes to proliferate leading to a combined immunodeficiency disease. In order to better document its role in immunomodulation, we developed a method for measuring CTPS activity in human lymphocytes. Using liquid chromatography ‐mass spectrometry, we quantified CTPS activity by measuring CTP in cell lysates. A stable isotope analog of CTP served as internal standard. We characterized the kine...
Source: Journal of Mass Spectrometry - September 16, 2019 Category: Chemistry Authors: Anne ‐Claire Boschat, Norbert Minet, Emmanuel Martin, Robert Barouki, Sylvain Latour, Sylvia Sanquer Tags: RESEARCH ARTICLE Source Type: research

Mass Spectrometry Imaging of Triglycerides in Biological Tissues by Laser Desorption Ionization from Silicon Nanopost Arrays
AbstractMass spectrometry imaging (MSI) is used increasingly to simultaneously detect a broad range of biomolecules, while mapping their spatial distributions within biological tissue sections. Matrix ‐assisted laser desorption ionization (MALDI) is recognized as the method‐of‐choice for MSI applications due in part to its broad molecular coverage. In spite of the remarkable advantages offered by MALDI, imaging of neutral lipids, such as triglycerides (TGs), from tissue has remained a signi ficant challenge due to ion suppression of TGs by phospholipids, e.g., phosphatidylcholines (PCs). To help overcome this limitat...
Source: Journal of Mass Spectrometry - September 16, 2019 Category: Chemistry Authors: Jarod A. Fincher, Andrew R. Korte, Jacqueline E. Dyer, Sridevi Yadavilli, Nicholas J. Morris, Derek R. Jones, Victoria K. Shanmugam, Russel K. Pirlo, Akos Vertes Tags: SPECIAL ISSUE ‐ RESEARCH ARTICLE Source Type: research

A Tutorial and Comprehensive Computational Study of Acceptance and Transmission of Sinusoidal and Digital Ion Guides
AbstractA quadrupole's acceptance is a measure of its ability to catch ions with certain trajectories. One way to calculate acceptance is the method of ellipses. The method arose partly from a simplification that trajectories could be calculated for an electrode axis independently of others. It has been used to calculate the acceptance and transmission of sine driven quadrupole mass filters for over fifty years. Although the method is straightforward, it is generally described with little detail or presented as a confusing string of equations. As such, it may not be decipherable by all practitioners. For this reason, the f...
Source: Journal of Mass Spectrometry - September 14, 2019 Category: Chemistry Authors: Adam P. Huntley, Gregory F. Brabeck, Peter T.A. Reilly Tags: SPECIAL FEATURE: TUTORIAL Source Type: research

Ruthenium coordination preferences in imidazole ‐containing systems revealed by electrospray ionization mass spectrometry and molecular modeling: possible cues for the surprising stability of the Ru (III)/tris (hydroxymethyl)‐aminomethane/imidazole complexes
AbstractRuthenium is a platinoid that exhibits a range of unique chemical properties in solution, which are exploited in a variety of applications, including luminescent probes, anticancer therapies and artificial photosynthesis. This paper focuses on a recently demonstrated ability of this metal in its +3 oxidation state to form highly stable complexes with tris (hydroxymethyl)aminomethane (H2NC(CH2OH)3, Tris ‐base or T) and imidazole (Im) ligands, where a single RuIII cation is coordinated by two molecules of each T and Im ‐. High‐resolution electrospray ionization mass spectrometry (ESI MS) is used to characterize...
Source: Journal of Mass Spectrometry - September 11, 2019 Category: Chemistry Authors: Igor A. Kaltashov, Anton El ‐Khoury, Chengfeng Ren, Sergey N. Savinov Tags: SPECIAL ISSUE ‐ RESEARCH ARTICLE Source Type: research

Structural characterization of the ligstroside aglycone isoforms in virgin olive oils by liquid ‐chromatography‐high resolution Fourier‐transform mass spectrometry and H/D exchange
AbstractA systematic structural characterization of the isomeric forms related to ligstroside aglycone (LA), one of the most relevant secoiridoids contained in virgin olive oils, was performed using reverse phase liquid chromatography with electrospray ionization Fourier ‐transform single and tandem mass spectrometry, operated in negative ion mode (RPLC‐ESI(‐)‐FTMS and FTMS/MS). The high mass resolution and accuracy provided by the adopted orbital trap mass analyzer enabled the recognition of more than 10 different isomeric forms of LA in virgin olive oil ex tracts. They were related to four different types of mole...
Source: Journal of Mass Spectrometry - September 11, 2019 Category: Chemistry Authors: R. Abbattista, I. Losito, C. De Ceglie, G. Basile, C.D. Calvano, F. Palmisano, T.R.I. Cataldi Tags: RESEARCH ARTICLE Source Type: research

Absolute Quantification of Dystrophin Protein in Human Muscle Biopsies using Parallel Reaction Monitoring (PRM)
AbstractThe need for a reliable and accurate method to quantify dystrophin proteins in human skeletal muscle biopsies has become crucial in order to assess the efficacy of dystrophin replacement therapies in Duchenne muscular dystrophy as well as to gain insight into the relationship between dystrophin levels and disease severity in Becker's muscular dystrophy. Current methods to measure dystrophin such as western blot and immunofluorescence, while straightforward and simple, lack precision and sometimes specificity. Here we standardized a targeted mass spectrometry method to determine the absolute amount of dystrophin in ...
Source: Journal of Mass Spectrometry - September 9, 2019 Category: Chemistry Authors: Emily H. Canessa, Mansi V. Goswami, Tchilabalo D. Alayi, Eric P. Hoffman, Yetrib Hathout Tags: SPECIAL ISSUE ‐ RESEARCH ARTICLE Source Type: research

Analysis of tetrahydrocannabinol derivative from Cannabis ‐infused chocolate by QuEChERS‐Thin Layer Chromatography‐Desorption Electrospray Ionization Mass Spectrometry
AbstractRecently in Canada and some states of the United States, marijuana (cannabis) has become fully legalized and regulated, for both medical and recreational purposes. This fact is going to make cannabis products such as edibles even more popular than ever before. Therefore, it is assumed that there will be a high demand for analytical methods which are accurate and sensitive enough to be used in different forensic and pharmaceutical cannabis related applications. Cannabis derivatives have an extreme range and number of constituents with possible interactions with one another. Thus, this characteristic leads to their v...
Source: Journal of Mass Spectrometry - September 9, 2019 Category: Chemistry Authors: Maryam Yousefi ‐Taemeh, Demian R. Ifa Tags: RESEARCH ARTICLE Source Type: research

Formation and hydrolysis of gas ‐phase [UO2(R)]+: R═CH3, CH2CH3, CH═CH2, and C6H5
AbstractThe goals of the present study were (a) to create positively charged organo ‐uranyl complexes with general formula [UO2(R)]+ (eg, R ═CH3 and CH2CH3) by decarboxylation of [UO2(O2C ─R)]+ precursors and (b) to identify the pathways by which the complexes, if formed, dissociate by collisional activation or otherwise react when exposed to gas ‐phase H2O. Collision ‐induced dissociation (CID) of both [UO2(O2C ─CH3)]+ and [UO2(O2C ─CH2CH3)]+ causes H+ transfer and elimination of a ketene to leave [UO2(OH)]+. However, CID of the alkoxides [UO2(OCH2CH3)]+ and [UO2(OCH2CH2CH3)]+ produced [UO2(CH3)]+ and [UO2(C...
Source: Journal of Mass Spectrometry - September 5, 2019 Category: Chemistry Authors: Irena Tatosian, Amanda Bubas, Anna Iacovino, Susan Kline, Luke Metzler, Michael Van Stipdonk Tags: RESEARCH ARTICLE Source Type: research

Identification of bifucosylated glycoforms using low energy CID spectra
AbstractWe have used tandem mass spectrometry based analysis of glycopeptides in order to identify the composition and structure of rare glycoforms. The results illustrate utility of low energy MS/MS for structure identification. We have shown the presence of bi ‐ and tri‐fucosylated glycoforms in human alpha‐1‐acid glycoprotein (AGP), a major plasma glycoprotein. Fucosylation in the case of AGP always occurs on the antennae, core fucosylation was not observed. (Source: Journal of Mass Spectrometry)
Source: Journal of Mass Spectrometry - September 2, 2019 Category: Chemistry Authors: Andr ás Ács, Lilla Turiák, Ágnes Révész, Károly Vékey, László Drahos Tags: RESEARCH ARTICLE Source Type: research

ESI ‐QTof‐MS characterization of hirsutinolide and glaucolide sesquiterpene lactones: fragmentation mechanisms and differentiation based on Na+/H+ adducts interactions in complex mixture
AbstractSesquiterpene lactones (SL) have been reported with various biological effects. Among the described SL skeletons, hirsutinolide and glaucolide have not been extensively studied by mass spectrometry (MS), especially how to distinguish them in organic matrices. Thus, this paper reports i) a strategy of their differentiation based on MS behavior during the ionization and ii) a proposal of the fragmentation pattern for both SL ‐subtypes. ESI(+)‐HRMS data of four isolated SL (hirsutinolides1 and3; glaucolides2 and4) were recorded by direct and UPLC water ‐sample combined injections. These analyses revealed that hi...
Source: Journal of Mass Spectrometry - September 2, 2019 Category: Chemistry Authors: Layzon A.L. Silva, Louis P. Sandjo, Alechania Misturini, Giovanni F. Caramori, Maique W. Biavatti Tags: RESEARCH ARTICLE Source Type: research

Solid phase microextraction as a powerful alternative for screening of secondary metabolites in actinomycetes
AbstractActinobacteria are one of the most promising producers of medically and industrially relevant secondary metabolites. However, screening of such compounds in actinobacteria growth demands simple, fast, and efficient extraction procedures that enable detection and precise quantification of biologically active compounds. In this regard, solid phase microextraction (SPME) emerges as an ideal extraction technique for screening of secondary metabolites in bacteria culture due to its non ‐exhaustive, minimally invasive, and non‐destructive nature; its integrated sample preparation workflow; balanced coverage feature; ...
Source: Journal of Mass Spectrometry - September 2, 2019 Category: Chemistry Authors: Vinicius Ricardo Acquaro Junior, J úlia Pereira Rodrigues, Luiz Alberto Beraldo Moraes Tags: RESEARCH ARTICLE Source Type: research

Erratum: Method development for the analysis of resinous materials with MALDI ‐FT‐ICR‐MS: novel internal standards and a new matrix material for negative ion mode
Journal of Mass Spectrometry, EarlyView. (Source: Journal of Mass Spectrometry)
Source: Journal of Mass Spectrometry - August 30, 2019 Category: Chemistry Tags: ERRATUM Source Type: research

Cover Picture
(Source: Journal of Mass Spectrometry)
Source: Journal of Mass Spectrometry - August 27, 2019 Category: Chemistry Tags: Cover picture Source Type: research

A recommended and verified procedure for in situ tryptic digestion of formalin ‐fixed paraffin‐embedded tissues for analysis by matrix‐assisted laser desorption/ionization imaging mass spectrometry
This month's Special Feature by Judd and colleagues from Vanderbilt University outlines key considerations when preparing formalin ‐fixed paraffin‐embedded (FFPE) tissues for matrix‐assisted laser desorption/ionization (MALDI) imaging mass spectrometry (MALDI IMS). MALDI IMS is a untargeted tool for imaging tissue and providing spatial information about the constituent analytes, but this powerful strategy is yet to reach its full potential. In part this is because before any research tool can successfully transition into the clinical laboratory, rugged and reliable sample preparation protocols have to be developed an...
Source: Journal of Mass Spectrometry - August 26, 2019 Category: Chemistry Authors: Audra M. Judd, Danielle B. Gutierrez, Jessica L. Moore, Nathan Heath Patterson, Junhai Yang, Carrie E. Romer, Jeremy L. Norris, Richard M. Caprioli Tags: Cover story Source Type: research

Paper Spray Mass Spectrometry: A New Drug Checking Tool for Harm Reduction in the Opioid Overdose Crisis
AbstractFentanyl and related psychoactive substances are at the forefront of the opioid overdose crisis, for which a complete solution is not immediately obvious. Drug testing for harm reduction may be an effective approach to both reduce overdoses and importantly, engage people who use drugs (PWUD) with the medical system. Paper spray mass spectrometry (PS ‐MS) is an ambient ionization strategy that is uniquely suited to address this complicated analytical task. This perspectives article presents the merits of PS‐MS, with a focus upon the current state of its use as a candidate drug checking strategy for harm reductio...
Source: Journal of Mass Spectrometry - August 20, 2019 Category: Chemistry Authors: Gregory W. Vandergrift, Chris G. Gill Tags: SPECIAL FEATURE: PERSPECTIVE Source Type: research

Formation and Hydrolysis of Gas ‐phase [UO2(R)]+: R=CH3, CH2CH3, CH=CH2 and C6H5
AbstractThe goals of the present study were (a) to create positively ‐charged organo‐uranyl complexes with general formula [UO2(R)]+ (eg., R=CH3, CH2CH3, etc.) by decarboxylation of [UO2(O2C ‐R)]+ precursors, and (b) identify the pathways by which the complexes, if formed, dissociate by collisional activation, or otherwise react when exposed to gas ‐phase H2O. CID of both [UO2(O2C ‐CH3)]+ and [UO2(O2C ‐CH2CH3)]+ causes H+ transfer and elimination of a ketene to leave [UO2(OH)]+. However, CID of the alkoxides [UO2(OCH2CH3)]+ and [UO2(OCH2CH2CH3)]+ produced [UO2(CH3)]+ and [UO2(CH2CH3)]+, respectively. Isolation ...
Source: Journal of Mass Spectrometry - August 19, 2019 Category: Chemistry Authors: Irena Tatosian, Amanda Bubas, Anna Iacovino, Susan Kline, Luke Metzler, Michael Van Stipdonk Tags: RESEARCH ARTICLE Source Type: research

Vibrating tip spray ionization mass spectrometry for direct sample analysis
AbstractIn this work, a vibrating tip spray ionization source was developed for direct mass spectrometric analysis of raw samples under voltage ‐free condition. A solid tip was mounted on a vibrator, and the solid tip was placed on the front of MS inlet. Liquid, viscous and bulk solid samples could be directly loaded on the tip‐end surface, and then a drop of solvent at microliter level was subsequently loaded on the tip for dissolution and extraction of analytes, and a vibrator was then started to atomize and ionize the analytes under ambient condition. We demonstrated vibrating tip spray mass spectrometry in various ...
Source: Journal of Mass Spectrometry - August 19, 2019 Category: Chemistry Authors: Ya ‐Nan Yao, Lin Wu, Dandan Di, Zi‐Cheng Yuan, Bin Hu Tags: RESEARCH ARTICLE Source Type: research

Silver Spray Deposition for AgLDI Imaging MS of Cholesterol and Other Olefins on Thin Tissue Sections
AbstractOlefins such as cholesterol and unsaturated fatty acids play important biological roles. Silver assisted laser desorption ionization (AgLDI) takes advantage of the strong affinity of silver to conjugate with double bonds to selectively ionize these molecules for imaging mass spectrometry experiments (IMS). For IMS studies, two main approaches for silver deposition have been described in the literature: fine coating by silver sputtering and spray deposition of silver nanoparticles. While these approaches allow for extremely high resolution IMS experiments to be conducted, they are not readily available to all labora...
Source: Journal of Mass Spectrometry - August 14, 2019 Category: Chemistry Authors: Ethan Yang, Fr édéric Fournelle, Pierre Chaurand Tags: SPECIAL ISSUE ‐ RESEARCH ARTICLE Source Type: research

Positive and negative ions of the amino acid histidine formed in low ‐energy electron collisions
We report both on the formation of positive ions formed by electron ionisa tion and negative ions induced by electron attachment. The experimental data was complemented by quantum chemical calculations. Specifically, the free energies for possible fragmentation reactions were derived for the τ and the π tautomer of histidine to get insight into the structures of the form ed ions and the corresponding neutrals. We report the experimental ionisation energy of (8.48 ± 0.03) eV for histidine which is in good agreement with the calculated vertical ionisation energy. In the case of negative ions, the dehydrogenated...
Source: Journal of Mass Spectrometry - August 14, 2019 Category: Chemistry Authors: Rebecca Mei ßner, Linda Feketeová, Andreas Bayer, Johannes Postler, Paulo Limão‐Vieira, Stephan Denifl Tags: RESEARCH ARTICLE Source Type: research

ESI ‐MS/MS analysis of protonated N‐methyl Amino Acids and their Immonium ions
In this study, theN‐methyl amino acids of all the amino acids (1‐21; including one isomeric pair) were synthesized and characterized by ESI ‐MS/MS, LC/MS/MS and HRMS. This data could be useful for detection and identification of N‐methyl amino acids in biological systems for future metabolomics studies. The MS/MS spectra of [M+H]+ ions of mostN‐methyl amino acids showed respective immonium ions by the loss of (H2O,CO). The other most common product ions detected were [MH ‐(NH2CH3]+, [MH ‐(RH)]+ (where R = side chain group) ions, and the selective structure indicative product ions due to side chain andN‐meth...
Source: Journal of Mass Spectrometry - August 14, 2019 Category: Chemistry Authors: Pavankumar P., Sudarshana Reddy B., Sai Sachin L., Nagarjuna Chary R., Prabhakar S. Tags: RESEARCH ARTICLE Source Type: research

Rapid MALDI ‐TOF molecular imaging: Instrument enhancements and their practical consequences
AbstractA new high performance linear MALDI ‐TOF mass spectrometer provides both high spatial resolution and high speed. This instrument employs a new ion optics system with a grounded ion source and efficient transfer and detection of ions over a broad mass range. This provides very high sensitivity, precision, and an extended dynamic rang e for both positive and negative ion detection. Here we demonstrate the capabilities of this system by imaging pancreatic tissue samples from rats and mice. (Source: Journal of Mass Spectrometry)
Source: Journal of Mass Spectrometry - August 9, 2019 Category: Chemistry Authors: Marvin Vestal, Lingjun Li, Evgenia Dobrinskikh, Yatao Shi, Bowen Wang, Xudong Shi, Sicheng Li, Christina Vestal, Kenneth Parker Tags: SPECIAL ISSUE ‐ RESEARCH ARTICLE Source Type: research

Unexpected detection of 3 ‐aroylbenzofuran side products in the preparation of 2‐arylbenzofurans: identification, characterization and comparison with chalcone's fragmentation patterns using EI/MSn
This study reports the identification of the by‐product,i.e. the 3 ‐benzoyl‐2‐phenylbenzofuran, on the base of its mass spectrometric behaviour using a combination of electron ionization (EI), exact mass measurement, multiple stage mass spectrometry and labelled compounds. This study reports the common fragmentation pathways and discusses possible fragment st ructures of characteristic ions from a series of 3‐aroyl‐2‐arylbenzofuran derivatives obtained as by‐product under Wittig conditions. Emphasis is laid on the formation and structure investigation of the [M‐H]+ and [M ‐OH]+ ions. Our results showed ...
Source: Journal of Mass Spectrometry - August 1, 2019 Category: Chemistry Authors: Michela Begala, Giovanna Lucia Delogu Tags: RESEARCH ARTICLE Source Type: research

Characterization of stable and reactive metabolites of piperine formed on incubation with human liver microsomes
AbstractBlack pepper, though commonly employed as a spice, has many medicinal properties. It consists of volatile oils, alkaloids, pungent resins,etc., of which piperine is a major constituent. Though safe at low doses, piperine causes alteration in the activity of drug metabolising enzymes and transporters at high dose, and is known to precipitate liver toxicity. It has a potential to form reactive metabolite(s) (RM) owing to the presence of structural alerts, such as methylenedioxyphenyl (MDP), α, β‐unsaturated carbonyl group (Michael acceptor) and piperidine. The present study was designed to detect and cha...
Source: Journal of Mass Spectrometry - July 31, 2019 Category: Chemistry Authors: Pammi Praneetha, Ankit Balhara, Mayurbhai Kathadbhai Ladumor, Dilip Kumar Singh, Amol Patil, Jalvadi Preethi, Sunil Pokharkar, Abhijeet Yashwantrao Deshpande, Sanjeev Giri, Saranjit Singh Tags: RESEARCH ARTICLE Source Type: research

Rapid MALDI ‐TOF Molecular Imaging: Instrument Enhancements & Their Practical Consequences
Journal of Mass Spectrometry, Volume 0, Issue ja, -Not available-. (Source: Journal of Mass Spectrometry)
Source: Journal of Mass Spectrometry - July 17, 2019 Category: Chemistry Authors: Marvin Vestal, Lingjun Li, Evgenia Dobrinskikh, Yatao Shi, Bowen Wang, Xudong Shi, Sicheng Li, Christina Vestal, Kenneth Parker Tags: SPECIAL ISSUE ‐ RESEARCH ARTICLE Source Type: research

A fast and simple approach for the quantification of 40 illicit drugs, medicines, and pesticides in blood and urine samples by UHPLC ‐MS/MS
Based on data collected by the “Information System on Diseases of Compulsory Declaration”, an agency responsible for poisoning notifications in Brazil, just short of 500,000 humans in that country were exposed to xenobiotics during the period 2013‐2017. The most commonly detected substances included medications (e.g., analg esics, benzodiazepines, antidepressants, anticonvulsants), drugs of abuse and pesticides. In this month's Special Feature, a group of investigators report a fast and simple UHPLC‐MS/MS approach for the quantification of 40 of the most important components in the context of emergency toxi...
Source: Journal of Mass Spectrometry - July 16, 2019 Category: Chemistry Authors: Sarah C. W. S. E. Franco de Oliveira, Alexandre D. Zucoloto, Carolina D. R. Oliveira, Edna M. M. Hernandez, Ligia V. G. Fruchtengarten, Tiago F. Oliveira, Mauricio Yonamine Tags: Cover story Source Type: research

Cover Picture
(Source: Journal of Mass Spectrometry)
Source: Journal of Mass Spectrometry - July 16, 2019 Category: Chemistry Tags: Cover picture Source Type: research

The improved performance of MALDI ‐TOF MS on the analysis of herbal saponins by using DHB‐GO composite matrix
AbstractMatrix ‐assisted laser desorption/ionization time‐of‐flight mass spectrometry (MALDI‐TOF MS) is an excellent analytical technique for rapid analysis of a variety of molecules with straightforward sample pretreatment. The performance of MALDI‐TOF MS is largely dependent on matrix type, and the dev elopment of novel MALDI matrices has aroused wide interest. Herein, we devoted to seek more robust MALDI matrix for herbal saponins than previous reported, and ginsenoside Rb1, Re and notoginsenoside R1 were used as model saponins. At the beginning of the present study, 2, 5‐dihydroxybenzoic acid (DHB) was foun...
Source: Journal of Mass Spectrometry - July 4, 2019 Category: Chemistry Authors: Zhangpei Zhu, Jiajia Shen, Yangfan Xu, Huimin Guo, Dian Kang, Tengjie Yu, He Wang, Wenshuo Xu, Guangji Wang, Yan Liang Tags: RESEARCH ARTICLE Source Type: research

A recommended and verified procedure for in situ tryptic digestion of formalin ‐fixed paraffin‐embedded tissues for analysis by matrix‐assisted laser desorption/ionization imaging mass spectrometry
AbstractMatrix ‐assisted laser desorption/ionization imaging mass spectrometry (MALDI IMS) is a molecular imaging technology uniquely capable of untargeted measurement of proteins, lipids, and metabolites while retaining spatial information about their locationin situ. This powerful combination of capabilities has the potential to bring a wealth of knowledge to the field of molecular histology. Translation of this innovative research tool into clinical laboratories requires the development of reliable sample preparation protocols for the analysis of proteins from formalin ‐fixed paraffin embedded (FFPE) tissues, the st...
Source: Journal of Mass Spectrometry - June 28, 2019 Category: Chemistry Authors: Audra M. Judd, Danielle B. Gutierrez, Jessica L. Moore, Nathan Heath Patterson, Junhai Yang, Carrie E. Romer, Jeremy L. Norris, Richard M. Caprioli Tags: SPECIAL FEATURE: TUTORIAL Source Type: research

Nucleic acid and SNP detection via template ‐directed native chemical ligation and inductively coupled plasma mass spectrometry
AbstractDetection of nucleic acids and single nucleotide polymorphisms (SNPs) is of pivotal importance in biology and medicine. Given that the biological effect of SNPs often are enhanced in combination with other SNPs, multiplexed SNP detection is desirable. We show proof of concept of the multiplexed detection of SNPs based on the template ‐directed native chemical ligation (NCL) of PNA‐probes carrying a metal tag allowing detection using ICP‐MS. For the detection of ssDNA oligonucleotides (30 bases), two probes, one carrying the metal tag and a second one carrying biotin for purification are covalently ligated. Th...
Source: Journal of Mass Spectrometry - June 25, 2019 Category: Chemistry Authors: Pablo Lores Lareo, Michael W. Linscheid, Oliver Seitz Tags: RESEARCH ARTICLE Source Type: research

Characterization and tentative identification of new flunitrazepam metabolites in authentic human urine specimens using liquid chromatography ‐Q Extractive‐HF Hybrid Quadrupole‐Orbitrap‐mass spectrometry (LC‐QE‐HF‐MS)
AbstractFlunitrazepam (FNZ) is a potent hypnotic, sedative and amnestic drug used to treat severe insomnia. In our recent study, flunitrazepam (FNZ) metabolic profiles were investigated carefully. Six authentic human urine samples were purified using solid phase extraction (SPE) without enzymatic hydrolysis and urine extracts were then analyzed by liquid chromatography ‐Q Extractive‐HF Hybrid Quadrupole‐Orbitrap‐mass spectrometry (LC‐QE‐HF‐MS), using the full scan positive ion mode and targeted MS/MS (ddms2) technique to make accurate mass measurements. There were 25 metabolites, including 13 phase I and 12 p...
Source: Journal of Mass Spectrometry - June 24, 2019 Category: Chemistry Authors: Shiyang Qin, Guobin Xin, Yuanfeng Wang, Jing Qiao, Wenfang Zhang, Duoqi Xu, Zizhen Xu, Yongtao Liu, Ying Zhang, Jianghai Lu Tags: RESEARCH ARTICLE Source Type: research

Novel approach to enhance sensitivity in surface ‐assisted laser desorption/ionization mass spectrometry imaging using deposited organic‐inorganic hybrid matrices
AbstractSample pretreatment is key to obtaining good data in matrix ‐assisted laser desorption/ionization mass spectrometry imaging (MALDI‐MSI). Although sublimation is one of the best methods for obtaining homogenously fine organic matrix crystals, its sensitivity can be low due to the lack of a solvent extraction effect. We investigated the effect of incorpora ting a thin film of metal formed by zirconium (Zr) sputtering into the sublimation process for MALDI matrix deposition for improving the detection sensitivity in mouse liver tissue sections treated with olanzapine. The matrix‐enhanced surface‐assisted laser...
Source: Journal of Mass Spectrometry - June 17, 2019 Category: Chemistry Authors: Kazuyoshi Nozaki, Yuji Nakabayashi, Tatsuya Murakami, Akio Miyazato, Issey Osaka Tags: RESEARCH ARTICLE Source Type: research

Electric modeling and characterization of pulsed high ‐voltage nanoelectrospray ionization sources by a miniature ion trap mass spectrometer
AbstractA better understanding of nanoelectrospray ionization (nano ‐ESI) would be beneficial in further improving the performances of nano‐ESI. In this work, the pulsed high‐voltage (HV) nano‐ESI has been electrically modeled and then systematically characterized by both voltage‐current and mass spectrometry measurements. First, the equivalent resistance of a nano‐ESI source changes with respect to both emitter tip diameter and the HV applied. Increased voltage could improve both spray current and ionization efficiency of the pulsed HV nano‐ESI. Compared with conventional DC HV method, a pulsed HV has less h...
Source: Journal of Mass Spectrometry - June 17, 2019 Category: Chemistry Authors: Zuqiang Xu, Hanyan Wu, Yang Tang, Wei Xu, Yanbing Zhai Tags: RESEARCH ARTICLE Source Type: research

Electrospray ionization collision induced dissociation of thiocarbocyanine and selenocarbocyanine dyes
AbstractThe effect of the properties of sulphur and selenium atoms, the composition and location of substituents ( ―CH3, ―OCH3, ―C2H5, and ―C3H6―((N+Br−)C5H5)), and the charge state on the collision induced dissociation (CID) behaviour of ions generated by electrospray ionization (ESI) of thiocarbocyanine and selenocarbocyanine dyes have been investigated. The results show that, for of all the examined singly charged ions, the main dissociation channel was related to the formation of distonic ions, generated as a result of cleavages within the dimethine bridge. In the case of doubly charged ions (with propy...
Source: Journal of Mass Spectrometry - June 17, 2019 Category: Chemistry Authors: Ma łgorzata A. Kaczorowska, Beata Jędrzejewska Tags: RESEARCH ARTICLE Source Type: research

A fast and simple approach for the quantification of 40 illicit drugs, medicines, and pesticides in blood and urine samples by UHPLC ‐MS/MS
AbstractA fast and simple approach to overcome challenges in emergency toxicological analysis, using ultra ‐high performance liquid chromatography–tandem mass spectrometry (UHPLC‐MS/MS) has been developed, for the detection of analytes in blood and urine samples from the following drug classes: analgesics, benzodiazepines, antidepressants, anticonvulsants, drugs of abuse, and pesticides. These subs tances are relevant in the context of emergency toxicology in Brazil. The sample preparation procedure was relatively easy and fast to perform. The method was fully validated giving limits of in the range of 0.5 and 20...
Source: Journal of Mass Spectrometry - June 17, 2019 Category: Chemistry Authors: Sarah C. W. S. E. Franco de Oliveira, Alexandre D. Zucoloto, Carolina D. R. Oliveira, Edna M. M. Hernandez, Ligia V. G. Fruchtengarten, Tiago F. Oliveira, Mauricio Yonamine Tags: RESEARCH ARTICLE Source Type: research

Proposal for a chemically consistent way to annotate ions arising from the analysis of reference compounds under ESI conditions: A prerequisite to proper mass spectral database constitution in metabolomics
AbstractNowadays, high ‐resolution mass spectrometry is widely used for metabolomic studies. Thanks to its high sensitivity, it enables the detection of a large range of metabolites. In metabolomics, the continuous quest for a metabolite identification as complete and accurate as possible has led during the last decade to an ever increasing development of public MS databases (including LC‐MS data) concomitantly with bioinformatic tool expansion. To facilitate the annotation process of MS profiles obtained from biological samples, but also to ease data sharing, exchange, and exploitation, the standardization and harmoni...
Source: Journal of Mass Spectrometry - June 17, 2019 Category: Chemistry Authors: Annelaure Damont, Marie ‐Françoise Olivier, Anna Warnet, Bernard Lyan, Estelle Pujos‐Guillot, Emilien L. Jamin, Laurent Debrauwer, Stéphane Bernillon, Christophe Junot, Jean‐Claude Tabet, François Fenaille Tags: SPECIAL FEATURE: TUTORIAL Source Type: research

Rapid Detection of Pesticides in Honey by Solid ‐Phase Micro‐extraction Coupled with Electrospray Ionization Mass Spectrometry
In this study, solid phase micro‐extraction fibres were used to rapidly extract and enrich pesticides in honey, a popular agricultural product with complex matrix, and then directly coupled with electrospray i onization mass spectrometry for qualitative and quantitative analysis. Three pesticides, i.e., atrazine, benalaxyl and pirimicarb, were investigated using the technique and their analytical performances were evaluated. The limits of detection and limits of quantitation of all the three pesticides co uld fulfil the cut‐off values of the international standard. Linear calibration curves were constructed with good R...
Source: Journal of Mass Spectrometry - June 10, 2019 Category: Chemistry Authors: Yi ‐Ching Choi, Tsz‐Tsun Ng, Bin Hu, Rong Li, Zhong‐Ping Yao Tags: SPECIAL ISSUE ‐ RESEARCH ARTICLE Source Type: research

Coupled Si and O isotope measurements of meteoritic material by laser fluorination isotope ratio mass spectrometry
We present a procedure for the determination of the isotopic ratios of silicon and oxygen from the same aliquot of anhydrous silicate material. The sample is placed in a bromine pentafluoride atmosphere as it is heated with a CO2 laser system releasing silicon tetrafluoride and oxygen gases. The oxygen gas is then purified to remove other reaction by ‐products through several liquid nitrogen traps before being captured onto a molecular sieve and transferred to an isotope ratio mass spectrometer. The silicon tetrafluoride gas is then purified using a supplementary line by repeatedly freezing to ‐196°C with liquid ni...
Source: Journal of Mass Spectrometry - June 10, 2019 Category: Chemistry Authors: Patrick J.A. Hill, Neil R. Banerjee, Arshad Ali, Iffat Jabeen, Gordon R. Osinski, Fred J. Longstaffe Tags: RESEARCH ARTICLE Source Type: research

Molecular level comparison of water extractives of maple and oak with negative and positive ion ESI FT ‐ICR mass spectrometry
AbstractSoluble extractives in wood function to protect living trees from destructive agents and also contribute to wood color and fragrance. Some extractive components have biological activities with medical applications. They also play important roles in wood processing and related applications. To increase the knowledge of wood chemistry, maple and oak were extracted by water. Ultraviolet/visible (UV/vis) spectroscopy indicated the presence of a phenolic compound, resorcinol, in maple extractives having higher molecular mass and more aromatic components than oak extractives. Negative and positive electrospray ionization...
Source: Journal of Mass Spectrometry - June 8, 2019 Category: Chemistry Authors: Zhongqi He, Rachel L. Sleighter, Patrick G. Hatcher, Shasha Liu, Fengchang Wu, Haixuan Zou, O. Modesto Olanya Tags: RESEARCH ARTICLE Source Type: research

Combined Use of Tandem Mass Spectrometry and Computational Chemistry to Study 2H ‐Chromenes from Piper aduncum
AbstractNatural 2H‐chromenes were isolated from the crude extract ofPiper aduncum (Piperaceae) and analyzed by electrospray ionization tandem mass spectrometry (ESI ‐MS/MS) applying collision‐induced dissociation. Density functional theory (DFT) calculations were used to explain the preferred protonation sites of the 2H‐chromenes based on thermochemical parameters, including atomic charges, proton affinity and gas‐phase basicity. After identifying the nucleophilic sites, the pathways were proposed to justify the formation of the diagnostic ions under ESI‐MS/MS conditions. The calculated relative energy for e ac...
Source: Journal of Mass Spectrometry - May 30, 2019 Category: Chemistry Authors: Amauri Alves Souza, Ricardo Vessecchi, Ian Castro ‐Gamboa, Maysa Furlan Tags: RESEARCH ARTICLE Source Type: research

Ion Mobility ‐Mass Spectrometry for the Separation and Analysis of Procyanidins
AbstractProcyanidins are polymeric flavan ‐3‐ones occurring in many plants with antioxidant and other beneficial bioactivities. Composed of catechin and epicatechin monomeric units connected by single carbon‐carbon B‐type linkages or A‐type linkages containing both carbon‐carbon and carbon‐oxygen‐carbon bonds. Their polymeri c structure makes analysis of procyanidin mixtures always difficult. Evaluation of procyanidins according to degree of polymerization (DP) using HPLC is time consuming and at best has resolved polymeric families up to DP‐17. To expedite studies of procyanidins, the utility of positive...
Source: Journal of Mass Spectrometry - May 30, 2019 Category: Chemistry Authors: Emily A. Rue, Jan A. Glinski, Vitold B. Glinski, Richard B. Breemen Tags: SPECIAL ISSUE ‐ RESEARCH ARTICLE Source Type: research

A comparative study of the electrospray ionization response of β‐O‐4′ lignin model compounds
AbstractElectrospray ionization mass spectrometry has recently become the technique of choice for rapid characterization of lignin degradation products. However, the fundamental question of the relationship between lignin structure and ionization efficiency has not been explored. In this work, we studied the electrospray ionization response of five structurally similar β‐O‐4′ model lignin compounds using lithium cationization in the positive electrospray ionization mode. The studied compounds have the same β‐O‐4′ backbone structure but differ at the α‐position by increasing nonpolar si...
Source: Journal of Mass Spectrometry - May 29, 2019 Category: Chemistry Authors: Shardrack O. Asare, Bert C. Lynn Tags: RESEARCH ARTICLE Source Type: research

Treasure hunt for peptides with undefined chemical modifications: Proteomics identification of differential albumin adducts of 2 ‐nitroimidazole‐indocyanine green in hypoxic tumor
In this study, we deployed a biotin conjugate of 2‐nitroimidazole‐indocyanine green (2‐nitro‐ICG) for the investigation ofin vivo hypoxia ‐probing mechanism of 2‐nitro‐ICG compounds. By implementing mass spectrometry‐based proteomics and exhaustive data‐mining, we report that 2‐nitro‐ICG and its fragments modify mouse serum albumin as the primary protein target, but at two structurally‐distinct sites and possibly via t wo different mechanisms. The identification of probe‐modified peptides not only contributes to the understanding of thein vivo metabolism of 2 ‐nitroimidazole compounds but also d...
Source: Journal of Mass Spectrometry - May 25, 2019 Category: Chemistry Authors: Lei Wang, Christopher Dietz, Feifei Zhou, Mohsen Erfanzadeh, Quing Zhu, Michael B. Smith, Xudong Yao Tags: RESEARCH ARTICLE Source Type: research

Label ‐free cervicovaginal fluid proteome profiling reflects the cervix neoplastic transformation
AbstractCervicovaginal fluid (CVF) is a valuable source of clinical information about the female reproductive tract in both non ‐pregnant and pregnant women. The aim of this study is to specify the CVF proteome at different stages of cervix neoplastic transformation by label‐free quantitation approach based on LC‐MS/MS method. The proteome composition of CVF from 40 women of reproductive age with HPV‐associated cervi x neoplastic transformation (LSIL, HSIL, CANCER) was investigated. Hierarchical clustering and principal component analysis (PCA) of the proteomic data obtained by a label‐free quantitation approach ...
Source: Journal of Mass Spectrometry - May 22, 2019 Category: Chemistry Authors: Natalia L. Starodubtseva, Alexander G. Brzhozovzkiy, Anna E. Bugrova, Alexey S. Kononikhin, Maria I. Indeykina, Kiril I. Gusakov, Vitaliy V. Chagovets, Niso M. Nazarova, Vladimir E. Frankevich, Gennady T. Sukhikh, Eugene N. Nikolaev Tags: RESEARCH ARTICLE Source Type: research

norHarmane containing ionic liquid matrices for low molecular weight MALDI ‐MS carbohydrate analysis: The perfect couple with α‐cyano‐4‐hydroxycinnamic acid
AbstractCinnamic acid derivatives, particularly α‐cyano‐4‐hydroxycinnamic acid (E ‐α‐cyano‐4‐hydroxycinnamic acid or (E) ‐2‐cyano‐3‐(4‐hydroxyphenyl)prop‐2‐enoate; CHCA) has been extensively used especially for protein and peptide analysis. Together with the introduction of ionic liquid MALDI matrix (ILM) started the study of applications of IL prepared with CHCA and a counter organic base (i.e., aliphat ic amines) in which CHCA moiety is the chromophore responsible of UV‐laser absorption. Although the extensive studies of norharmane (9H‐pyrido[3,4‐b]indole; nHo) applications a...
Source: Journal of Mass Spectrometry - May 21, 2019 Category: Chemistry Authors: Tob ías Schmidt De León, María L. Salum, Rosa Erra‐Balsells Tags: RESEARCH ARTICLE Source Type: research

Determination of enantiomeric excess of amino acids using photodissociation of cold gas ‐phase Na+‐containing clusters
Journal of Mass Spectrometry, Volume 0, Issue ja, -Not available-. (Source: Journal of Mass Spectrometry)
Source: Journal of Mass Spectrometry - May 15, 2019 Category: Chemistry Authors: Doan Thuc Nguyen, Narumi Oki, Akimasa Fujihara Tags: JMS LETTERS Source Type: research

Development and comparison of liquid –liquid extraction and accelerated solvent extraction methods for quantitative analysis of chloramphenicol, thiamphenicol, florfenicol, and florfenicol amine in poultry eggs
AbstractAccelerated solvent extraction was investigated as a novel alternative technology for the separation and quantitative analysis of chloramphenicol, thiamphenicol, florfenicol, and florfenicol amine from poultry eggs, and the results were compared with the results of liquid –liquid extraction. Rapid quantification of the target compounds was carried out by ultra‐performance liquid chromatography‐electrospray ionization tandem triple quadrupole mass spectrometry. This optimized method was validated according to the requirements defined by the European Union and th e United States Food and Drug Administration...
Source: Journal of Mass Spectrometry - May 14, 2019 Category: Chemistry Authors: Bo Wang, Maoda Pang, Xia Zhao, Kaizhou Xie, Peiyang Zhang, Genxi Zhang, Tao Zhang, Xuezhong Liu, Guojun Dai Tags: APPLICATION NOTE Source Type: research

Mass spectral databases for metabolomics: How to build a consistently annotated mass spectral database from pure reference compounds analyzed under electrospray ionization conditions?
AbstractNowadays, high ‐resolution mass spectrometry is widely used for metabolomic studies. Thanks to its high sensitivity, it enables the detection of a large range of metabolites. In metabolomics, the continuous quest for a metabolite identification as complete and accurate as possible has led during the last decade to an ever increasing development of public MS databases (including LC‐MS data) concomitantly with bioinformatic tool expansion. To facilitate the annotation process of MS profiles obtained from biological samples, but also to ease data sharing, exchange and exploitation, the standardization and h armoni...
Source: Journal of Mass Spectrometry - May 13, 2019 Category: Chemistry Authors: Annelaure Damont, Marie ‐Françoise Olivier, Anna Warnet, Bernard Lyan, Estelle Pujos‐Guillot, Emilien L. Jamin, Laurent Debrauwer, Stéphane Bernillon, Christophe Junot, Jean‐Claude Tabet, François Fenaille Tags: SPECIAL FEATURE: TUTORIAL Source Type: research

Mass spectrometry combined with affinity probes for the identification of CP4 EPSPS in genetically modified soybeans
AbstractSample preparation methods used for genetically modified organisms (GMO) analysis are often time consuming, require extensive manual manipulation and result in limited amounts of purified protein which may complicate the detection of low abundance GM protein. A robust sample pretreatment method prior to mass spectrometry (MS) detection of the transgenic protein (5 ‐enolpyruvylshikimate‐3‐phosphate synthase CP4 EPSPS) present in Roundup ReadyTM soya is investigated. Liquid chromatography ‐multiple reaction monitoring tandem mass spectrometry (nano LC‐MS/MS‐MRM) was used for the detection and quantificati...
Source: Journal of Mass Spectrometry - May 11, 2019 Category: Chemistry Authors: Shobha Devi, Pei ‐Yu Chu, Po‐Hung Wu, Yen‐Peng Ho Tags: SPECIAL ISSUE ‐ RESEARCH ARTICLE Source Type: research