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Daniel Jansson, Susanne Wiklund Lindström, Rikard Norlin, Saphon Hok, Carlos A Valdez, Audrey M Williams, Armando Alcaraz, Calle Nilsson, Crister Åstot
This work is part two of a three-part series in this issue of a Sweden-United States collaborative effort towards the understanding of the chemical attribution signatures of Russian VX (VR) in synthesized samples and complex food matrices. In this study, we describe the sourcing of VR present in food based on chemical analysis of attribution signatures by liquid chromatography-tandem mass spectrometry (LC-MS/MS) combined with multivariate data analysis. Analytical data was acquired from seven different foods spiked with VR batches that were synthesized via six different routes in two separate laboratories...
August 15, 2018: Talanta
Jie An, Joshua J Woodward, Weinan Lai, Mark Minie, Xizhang Sun, Lena Tanaka, Jessica M Snyder, Tomikazu Sasaki, Keith B Elkon
OBJECTIVE: Type I interferon (IFN-I) is strongly implicated in the pathogenesis of Systemic Lupus Erythematosus (SLE) as well as rare monogenic 'interferonopathies' such as Aicardi-Goutieres Syndrome (AGS) caused by mutations in the DNA exonuclease, TREX1. The DNA-activated IFN-I pathway, cyclic GMP-AMP (cGAMP) synthase (cGAS), is linked to subsets of AGS and lupus. We identified inhibitors of DNA-cGAS interaction and tested lead candidate, X6, in a mouse model of AGS. METHODS: Trex1-/- mice were treated orally from birth with either X6 or HCQ for 8 weeks...
May 21, 2018: Arthritis & Rheumatology
Gautham Vivek Sridharan, Matthew D'Alessandro, Shyam Sundhar Bale, Vicky Bhagat, Hugo Gagnon, John M Asara, Korkut Uygun, Martin L Yarmush, Nima Saeidi
Morbidly obese patients often elect for Roux-en-Y gastric bypass (RYGB), a form of bariatric surgery that triggers a remarkable 30% reduction in excess body weight and reversal of insulin resistance for those who are type II diabetic. A more complete understanding of the underlying molecular mechanisms that drive the complex metabolic reprogramming post-RYGB could lead to innovative non-invasive therapeutics that mimic the beneficial effects of the surgery, namely weight loss, achievement of glycemic control, or reversal of non-alcoholic steatohepatitis (NASH)...
September 2017: Technology
Julian Hösl, André Gessner, Nahed El-Najjar
A simple and precise ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the simultaneous analysis of five anti-infective agents used to treat severe infections [three antibiotics (daptomycin, moxifloxacin, ciprofloxacin) and two antifungals (isavuconazole, caspofungin)] in human plasma. Sample preparation was based on protein precipitation with ice cold methanol. All five agents were analyzed with the corresponding isotopically labeled internal standards. All analytes were detected in multiple reactions monitoring (MRM) using API 4000 triple-quadrupole mass spectrometer with electrospray (ESI) source operating in positive mode...
May 12, 2018: Journal of Pharmaceutical and Biomedical Analysis
Xuemei Liu, Pei Hu, Yongsheng Wang, Xizhu Wang, Jinghua Huang, Jin Li, Cheng Li, Hongyun Wang, Ji Jiang
Monocyte locomotion inhibitory factor (MLIF, Met-Gln-Cys-Asn-Ser), a pentapeptide with anti-inflammatory activity, was developed for neural protection in acute ischemic stroke. Determination of MLIF in human plasma samples is of great importance for pharmacokinetic evaluation in clinical studies. A reliable and sensitive method based on ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) was established for the measurement of MLIF in human plasma. Instability of peptide in matrix was the primary challenge in method development, which was properly resolved by addition of acidification reagents like sulfuric acid...
April 10, 2018: Journal of Pharmaceutical and Biomedical Analysis
Xi Zhang, Tianyang Guo, Tong Xiang, Yiyang Dong, Jichuan Zhang, Liqun Zhang
The natural rubber molecule is one of the end products of isoprenoids metabolism in the plant. Dimethylallyl diphosphate (DMAPP) and farnesyl pyrophosphate (FPP) are two typical isoprenoids which control the rate of biosynthesis and the molecular weight of natural rubber. A rapid, nonradioactive method for quantitation of DMAPP and FPP in natural rubber latex by liquid chromatography tandem with mass spectrometry (LC-MS/MS) was reported. DMAPP and FPP were determined in the multiple reaction monitoring mode(MRM)followed by separation with a silica-based C18 column...
May 3, 2018: Journal of Chromatography. A
Leonardo Di Donna, Lucia Bartella, Anna Napoli, Giovanni Sindona, Fabio Mazzotti
Monacolin K, the active ingredient present in dietary supplement, is a nutraceutical whose health benefits have been widely documented. A fast approach for the assay of lovastatin in both form, lactone and acid, by mass spectrometry is presented. The quantitative assay is carried out by HPLC-MS/MS using the multiple reaction monitoring (MRM) mode and simvastatin and pravastatin as internal standards. The accuracy values ranged from 97 to 101%; the analytical parameters values of LOQ, LOD, recovery and reproducibility, were calculated analyzing fortified samples, confirming the reliability of the proposed approach...
May 16, 2018: Journal of Mass Spectrometry: JMS
Mariana Younes Tramontina, Maria Beatriz Ferreira, Mauro Silveira de Castro, Isabela Heineck
This article aims to investigate the morbidities related to medications, their risk factors and causes detected in patients who seek the Hospital Emergency Service of a University in the South of Brazil. Data collection was based on application of a questionnaire to patients of a minimum age of 18 years, that signing the Term of Free and Informed Consent (TFIC), during the period from October 2013 to March 2014, and analysis of electronic record charts. Cases were evaluated by pharmacists and a doctor to define whether it was a case of medication related morbidity (MRM) and to establish its possible causes...
May 2018: Ciência & Saúde Coletiva
Lidija Brkljačić, Ivanka Jerić
Chemical derivatization of carbonyl compounds is a prerequisite for their determination in environmental and biological samples by LC-MS/MS analysis. The main requirements in regard to the good derivatization reagent are fast, selective and quantitative reaction with carbonyl compounds, and efficient fragmentation upon collision-induced dissociation (CID). We have prepared glutamic acid-related hydrazine reagent, and optimized derivatization procedure with benzaldehyde as a model carbonyl compound. The CID spectrum of the obtained hydrazone gave rich fragmentation pattern with numerous abundant fragment ions...
May 15, 2018: Journal of Mass Spectrometry: JMS
Junhui Lee, Jiwon Park, Ahra Go, Heesung Moon, Sujin Kim, Sohee Jung, Wonjoon Jeong, Heesun Chung
To intoxicated patients in the emergency room, toxicological analysis can be considerably helpful for identifying the involved toxicants. In order to develop a urine multi-drug screening (UmDS) method, gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS-MS) were used to determine targeted and unknown toxicants in urine. A GC-MS method in scan mode was validated for selectivity, limit of detection (LOD) and recovery. An LC-MS-MS multiple reaction monitoring (MRM) method was validated for lower LOD, recovery and matrix effect...
May 14, 2018: Journal of Analytical Toxicology
Pallab Bhowmick, Yassene Mohammed, Christoph H Borchers
Motivation: Multiple Reaction Monitoring (MRM)-based targeted proteomics is increasingly being used to study the molecular basis of disease. When combined with an internal standard, MRM allows absolute quantification of proteins in virtually any type of sample but the development and validation of an MRM assay for a specific protein is laborious. Therefore, several public repositories now host targeted proteomics MRM assays, including NCI's Clinical Proteomic Tumor Analysis Consortium assay portals, PeptideAtlas SRM Experiment Library, SRMAtlas, PanoramaWeb, and PeptideTracker, with all of which contain different levels of information...
May 14, 2018: Bioinformatics
Nirupama Samanmalie Jayasinghe, Himasha Mendis, Ute Roessner, Daniel Anthony Dias
Gas chromatography coupled with triple quadrupole mass spectrometry (GC-QqQ-MS) can be used to accurately quantify endogenous small molecules extracted from biological samples such as plants and human fluids including sera and urine. In order to quantify primary metabolites typically from central carbon metabolism such as sugars from glycolysis and the pentose phosphate pathway; and organic acids involved in the tricarboxylic acid (TCA) cycle; polar endogenous metabolites must be extracted from the samples of interest, chemically derivatized and quantified against a linear calibration curve to a corresponding authentic standard...
2018: Methods in Molecular Biology
Tiago F Jorge, Carla António
Phosphorylated carbohydrates are central metabolites involved in key plant metabolic pathways, such as glycolysis and central carbon metabolism. Such pathways influence plant growth, development, and stress responses to environmental changes, and ultimately, reflect the plant's energy status. The high polarity of these metabolites, the variety of isomeric structures (e.g., glucose-1-phosphate (G1P)/fructose-6-phosphate (F6P)/mannose-6-phosphate (M6P)/G6P, sucrose-6-phosphate (S6P)/T6P), and rapid metabolic turnover makes their analysis particularly challenging...
2018: Methods in Molecular Biology
D Luque-Córdoba, M Calderón-Santiago, M D Luque de Castro, F Priego-Capote
Endocannabinoids are lipids with a key role in physiological processes such as the immune response or the metabolism. This involvement explains their association to pathologies such as cancer, obesity or multiple sclerosis. The determination of endocannabinoids constitutes a challenge for clinical laboratories due to the variety of biological matrices and the wide range of concentrations at which they can be found. This research deals with the comparison of three sample preparation strategies (viz., on-line SPE, off-line SPE for interferents removal, and protein precipitation) for subsequent LC-MS/MS analysis of 14 endocannabinoids and analogous compounds in serum...
August 1, 2018: Talanta
Kahina Slimani, Yvette Pirotais, Pierre Maris, Jean-Pierre Abjean, Dominique Hurtaud-Pessel
A novel and reliable method to quantify residual levels of N-(3-aminopropyl)-N-dodecylpropane-1,3-diamine in dairy products using ion-pairing reversed-phase liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed and fully validated. Sample extraction was done with salting-out technique using acetonitrile and sodium chloride. For LC-MS/MS, the analyte was detected using positive electrospray ionization (ESI+) and two multiple reaction monitoring (MRM) transitions were monitored. The method was validated in the 5-150 µg kg-1 range using total error approach...
October 1, 2018: Food Chemistry
Xiangsheng Zhao, Jianhe Wei, Meihua Yang
Morinda officinalis is an important herbal medicine and functional food, and its main constituents include anthraquinone and iridoid glycosides. Quantification of the main compounds is a necessary step to understand the quality and therapeutic properties of M. officinalis , but this has not yet been performed based on liquid chromatography/tandem mass spectrometry (LC-MS/MS). Analytes were extracted from M. officinalis by reflux method. Ultrahigh-performance liquid chromatography coupled with a triple quadrupole mass spectrometry (UPLC-QqQ-MS) using multiple reaction monitoring (MRM) mode was applied for quantification...
May 3, 2018: Molecules: a Journal of Synthetic Chemistry and Natural Product Chemistry
Rahul Mondal, Ayan Mukherjee, Subrata Biswas, Ramen Kumar Kole
A liquid-liquid extraction (LLE) for water and modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method for sediment combined with gas chromatography-tandem mass spectrometry (GC-MS/MS) detection in multiple reaction monitoring (MRM) mode was standardized for determination of 31 pesticides. Performance characteristics for the selected pesticides were acceptable according to European Commission's (EC) guidelines for method validation (recovery 70-120%, RSD <20% and R2 value ≥ 0.99)...
April 30, 2018: Chemosphere
Michael Hellwig, Falco Beer, Sophia Witte, Thomas Henle
Glycation reactions (Maillard reactions) during the malting and brewing processes are important for the development of the characteristic color and flavor of beer. Recently, free and protein-bound Maillard reaction products (MRPs) such as pyrraline, formyline, and maltosine were found in beer. Furthermore, these amino acid derivatives are metabolized by Saccharomyces cerevisiae via the Ehrlich pathway. In this study, a method was developed for quantitation of individual Ehrlich intermediates derived from pyrraline, formyline, and maltosine...
May 10, 2018: Journal of Agricultural and Food Chemistry
Fatemeh Mahmoodani, Conrad O Perera, Grant Abernethy, Bruno Fedrizzi, Hong Chen
Vitamin D3 levels are known to sometimes decline in fortified products, which could be due to its degradation, although the exact mechanism is unknown. In this study, the influence of processing and storage conditions on lipid oxidation and vitamin D3 degradation were studied. Simulated whole milk powders with and without heat treatment were stored for 12 months at two different storage temperatures (20 °C and 40 °C). Stored samples without heat treatment showed higher lipid oxidation products analyzed by PV and TBARS values compared to those with heat treatment...
September 30, 2018: Food Chemistry
Jin Xiang, Qin Yu, Mao-Zhi Liang, Yong-Ping Qin, Feng Nan
OBJECTIVE: To establish a method for the determination of 5-hydroxy tryptamine (5-HT),adrenalin (AD) and noradrenalin (NA) in human plasma using pre-column derivatization HPLC-MS/MS. Methods Derivatives of the plasma samples were produced with dansyl chloride under pH 10.5,and then extracted and enriched with ethyl acetate. The detected chemicals were separated using Ultimate C₁₈ (50 mm×4.6 mm,5 μm) with acetonitrile-water-formic acid=95∶5∶0.05 ( V∶V∶V ) at 0.2 mL/min. The HPLC-MS//MS system was operated under a multiple reaction monitoring mode (MRM) using the electrospray ionization technique in positive mode...
March 2018: Sichuan da Xue Xue Bao. Yi Xue Ban, Journal of Sichuan University. Medical Science Edition
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