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Rapid communications in mass spectrometry : RCM 20건

  1. [해외논문]   Isotopically labelled paroxetine standard allows for definite structure elucidation of the paroxetine tandem mass spectrum  

    Vay, Manuela , Majewsky, Marius , Mikus, Gerd
    Rapid communications in mass spectrometry : RCM v.32 no.15 ,pp. NA , 2018 , 0951-4198 ,

    초록

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  2. [해외논문]   Cover Image  

    Kennedy, Joseph H. , Palaty, Jan , Gill, Chris G. , Wiseman, Justin M.
    Rapid communications in mass spectrometry : RCM v.32 no.15 ,pp. i - i , 2018 , 0951-4198 ,

    초록

    The cover image, by Joseph H. Kennedy et al., is based on the Research Article Rapid Analysis of Fentanyls and Other Novel Psychoactive Substances (NPS) in Substance Use Disorder Patient Urine using Paper Spray Mass Spectrometry , https://doi.org/10.1002/rcm.8164 . Design Credit: Gregory W. Vandergrift, Applied Environmental Research Laboratories, Chemistry, Vancouver Island University.

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  3. [해외논문]   A mass spectrometry based predictive strategy reveals ADAP1 is phosphorylated at tyrosine 364  

    Reisdorph, Richard (Skaggs School of Pharmacy and Pharmaceutical Sciences, University of Colorado Denver, Anschutz Medical Campus, Aurora, CO, USA) , Littrell‐ (Environment, Safety, Health & Quality Office, National Renewable Energy Laboratory (NREL), 15013 Denver West Parkway, Golden, CO, USA) , Miller, BobbiJo (Skaggs School of Pharmacy and Pharmaceutical Sciences, University of Colorado Denver, Anschutz Medical Campus, Aurora, CO, USA) , Powell, Roger (Skaggs School of Pharmacy and Pharmaceutical Sciences, University of Colorado Denver, Anschutz Medical Campus, Aurora, CO, USA) , Reisdorph, Nichole
    Rapid communications in mass spectrometry : RCM v.32 no.15 ,pp. 1173 - 1180 , 2018 , 0951-4198 ,

    초록

    Rationale The goal of this work was to identify phosphorylation sites within the amino acid sequence of human ADAP1. Using traditional mass spectrometry based techniques we were unable to produce interpretable spectra demonstrating modification by phosphorylation. This prompted us to employ a strategy in which phosphorylated peptides were first predicted using peptide mapping followed by targeted MS/MS acquisition. Methods ADAP1 was immunoprecipitated from extracts of HEK293 cells stably transfected with ADAP1 cDNA. Immunoprecipitated ADAP1 was digested with proteolytic enzymes and analyzed by LC/MS in MS 1 mode by high‐resolution quadrupole time‐of‐flight mass spectrometry (QTOF‐MS). Peptide molecular features were extracted using an untargeted data‐mining algorithm. Extracted peptide neutral masses were matched against the ADAP1 amino acid sequence with phosphorylation included as a predicted modification. Peptides with predicted phosphorylation sites were analyzed by targeted LC/MS 2 . Acquired MS 2 spectra were then analyzed using database search engines to confirm phosphorylation. Spectra of phosphorylated peptides were validated by manual interpretation. Further confirmation was performed by manipulating phospho‐peptide abundance using calf intestinal phosphatase (CIP) and the phorbol ester, phorbol 12‐myristate 13‐acetate (PMA). Results Of five predicted phosphopeptides, one, comprised of the sequence AVDRPMLPQEYAVEAHFK, was confirmed to be phosphorylated on a tyrosine at position 364. Pre‐treatment of cells with PMA prior to immunoprecipitation increased the ratio of phosphorylated to unphosphorylated peptide as determined by area counts of extracted ion chromatograms (EIC). Addition of CIP to immunoprecipitation reactions eliminated the phosphorylated form. Conclusions A novel phosphorylation site was identified at tyrosine 364. Phosphorylation at this site is increased by treatment with PMA. PMA promotes membrane translocation and activation of protein kinase C (PKC), indicating that tyrosine 364 is phosphorylated by a PKC‐dependent mechanism.

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  4. [해외논문]   Liquid chromatography/electrospray ionization tandem mass spectrometry study of repaglinide and its forced degradation products  

    Purna Chander, C. (National Centre for Mass Spectrometry, CSIR–Indian Institute of Chemical Technology, Hyderabad, 500 007, India) , Raju, B. (National Centre for Mass Spectrometry, CSIR–Indian Institute of Chemical Technology, Hyderabad, 500 007, India) , Ramesh, M. (National Centre for Mass Spectrometry, CSIR–Indian Institute of Chemical Technology, Hyderabad, 500 007, India) , Shankar, G. (National Centre for Mass Spectrometry, CSIR–Indian Institute of Chemical Technology, Hyderabad, 500 007, India) , Srinivas, R. (National Centre for Mass Spectrometry, CSIR–Indian Institute of Chemical Technology, Hyderabad, 500 007, India)
    Rapid communications in mass spectrometry : RCM v.32 no.15 ,pp. 1181 - 1190 , 2018 , 0951-4198 ,

    초록

    Rationale Stress stability studies of drugs have been recognized as an essential part of the drug development process. These studies are used to investigate the intrinsic stability of the drugs and for the development of a selective stability indicating assay method (SIAM). Stress testing is also useful for the formulation and packaging development, shelf‐life determination and designing of manufacturing processes. As per regulatory guidelines, stress degradation studies and structural characterization should be carried out to establish degradation pathways of the drug, which is essential from both the efficacy and safety point of view. As the stress stability studies of repaglinide have not been reported in the literature, the present study has been undertaken. Methods Repaglinide (RP), an oral anti‐diabetic drug, was subjected to hydrolysis (acidic, alkaline and neutral), oxidation, photolysis and thermal stress conditions as per International Conference on Harmonization (ICH) guidelines Q1A (R2). The chromatographic separation of the drug and its degradation products (DPs) was achieved on an Agilent XDB C‐18 column using the gradient elution method with a mobile phase consisting of 20 mM ammonium acetate and acetonitrile at flow rate of 1.0 mL min −1 . The DPs were characterized using liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI‐MS/MS) in combination with accurate mass measurements. Results The drug degraded under hydrolytic and oxidative stress, while it was stable under thermal and photolytic stress conditions. In total, six DPs were formed and the LC/MS method described here can resolve all DPs from the parent as well as from each other under various stress conditions. To elucidate the structures of DPs, fragmentation of the [M + H] + ions of RP and its DPs was studied by using LC/ESI‐MS/MS combined with accurate mass measurements. Conclusions The forced degradation of RP carried out as per ICH guidelines results in the formation of six degradation products which have been characterized using LC/MS/MS in combination with accurate mass measurements.

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  5. [해외논문]   Effects of solvent parameters on the electrospray ionization tandem mass spectrometry response of glucose  

    Thacker, Jonathan B. (Department of Chemistry and Biochemistry, The University of Texas at Arlington, 700 Planetarium Place, Arlington, TX, 76019, USA) , Schug, Kevin A. (Department of Chemistry and Biochemistry, The University of Texas at Arlington, 700 Planetarium Place, Arlington, TX, 76019, USA)
    Rapid communications in mass spectrometry : RCM v.32 no.15 ,pp. 1191 - 1198 , 2018 , 0951-4198 ,

    초록

    Rationale The importance of saccharides, the most abundant biomolecules on Earth, extends beyond their biological roles and to consumer products and industrial processes. Electrospray ionization tandem mass spectrometry (ESI‐MS/MS) is an attractive tool for the analysis of underivatized saccharides (US), but they tend to have relatively low sensitivities due to their low surface activities and lack of easily protonable or deprotonable chemical groups. An understanding of the influences that solvent parameters have on their signal intensities would enhance the usefulness of ESI‐MS/MS for their analysis. Methods Solutions of glucose, a model analyte for US, in various combinations of solvent, additive, additive concentration, and pH were analyzed by flow injection analysis ESI‐MS/MS in both the positive and negative ionization mode. The blank‐corrected signal intensities of the solvent parameter combinations were then compared. Results The addition of acetonitrile led to severe ionization suppression in the positive ionization mode through its competition with glucose for cation adduction. High signal intensity was achieved under wide pH and concentration ranges for methanol: water solutions containing ammonium trifluoroacetate in the positive ionization mode. The highest signal intensities for acetonitrile: water solutions were those containing ammonium formate or lithium fluoride in the negative ionization mode. Conclusions An understanding of the influence of solvent parameters on the signal intensity of a given analyte is useful for guiding the selection process of mobile phases/flow solvents that lead to low limits of detection or the minimization of matrix effects by allowing its detection at high dilution factors.

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  6. [해외논문]   Electrospray ionization study of tricarbonyl fac‐[Re(CO)3(PO)(X)]‐type complexes: influence of ancillary co‐ligands in the release of carbon monoxide  

    Tisato, Francesco (CNR –) , Porchia, Marina (ICMATE, Corso Stati Uniti 4, 35127, Padova, Italy) , Shegani, Antoni (CNR –) , Maina, Theodosia (ICMATE, Corso Stati Uniti 4, 35127, Padova, Italy) , Papadopoulos, Minas S. (INRaSTES, NCSR “Demokritos”, 15310 Ag. Paraskevi Attikis, Athens, Greece) , Seraglia, Roberta (INRaSTES, NCSR “Demokritos”, 15310 Ag. Paraskevi Attikis, Athens, Greece) , Traldi, Pietro (INRaSTES, NCSR “Demokritos”, 15310 Ag. Paraskevi Attikis, Athens, Greece)
    Rapid communications in mass spectrometry : RCM v.32 no.15 ,pp. 1199 - 1206 , 2018 , 0951-4198 ,

    초록

    Rationale fac ‐[Re(CO) 3 (PO)(X)]‐type complexes (PO = chelated bidentate tertiary phosphine (1‐), X = various neutral, mono‐dentate ligands) represent a class of compounds that meets the synthetic criteria for the preparation of potential carbon monoxide (CO) release molecules (CORMs) for medicinal application. The aim of our investigation was to achieve qualitative information whether the nature of the ancillary X ligand might influence the release of CO. Methods The release of CO has been investigated by means of product ion spectrometry of electrospray ionization (ESI)‐generated [M + H] + species, produced by multiple collisional experiments, using an ion trap mass spectrometer. Results Tandem mass spectrometry applied to the protonated species [Re(CO) 3 (PO)(X) + H] + of seven complexes (those including X = OH 2 ( 1 ), isonitrile ( 2 , 3 ), imidazole ( 4 ), pyridine ( 5 ) and phosphine ( 6 , 7 )) shows initial loss of coordinated water ( 1 ) or pyridine ( 5 ), whereas the majority of investigated entries display initial, sequential release of CO groups. The energetics of CO release have been investigated by breakdown curves for selected collisionally activated decomposition processes involving CO, and compared with those involving X groups. Conclusions The nature of the co‐ligand X drives the primary loss in the MS n processes of [Re(CO) 3 (PO)(X) + H] + compounds. When X = solvent, the energetics of these decompositions follow the trend H 2 O n pathways indicate that [Re(PO)] (Re with chelated PO phosphine) constitutes the residual moiety. This behavior indicates that the presence of a functionalized phosphine is essential for a sequential, controlled release of CO.

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  7. [해외논문]   Preliminary assessment of stable nitrogen and oxygen isotopic composition of USGS51 and USGS52 nitrous oxide reference gases and perspectives on calibration needs  

    Ostrom, Nathaniel E. (Department of Integrative Biology and DOE Great Lakes Bioenergy Research Institute, Michigan State University, East Lansing, MI, USA) , Gandhi, Hasand (Department of Integrative Biology and DOE Great Lakes Bioenergy Research Institute, Michigan State University, East Lansing, MI, USA) , Coplen, Tyler B. (U.S. Geological Survey, 431 National Center, Reston, VA, USA) , Toyoda, Sakae (Department of Chemical Science and Engineering, School of Materials and Chemical Technology, Tokyo Institute of Technology, Yokohama, 226‐8502, Japan) , Bö (U.S. Geological Survey, 431 National Center, Reston, VA, USA) , hlke, J.K. (Beutenberg Campus, Max‐Planck‐Institute for Biogeochemistry, P.O. Box 100164, 07701, Jena, Germany) , Brand, Willi A. (Department of Earth System Science, Stanford University, Stanford, CA, USA) , Casciotti, Karen L. , Dyckmans, Jens , Giesemann, Anette , Mohn, Joachim , Well, Reinhard , Yu, Longfei , Yoshida, Naohiro
    Rapid communications in mass spectrometry : RCM v.32 no.15 ,pp. 1207 - 1214 , 2018 , 0951-4198 ,

    초록

    Rationale Despite a long history and growing interest in isotopic analyses of N 2 O, there is a lack of isotopically characterized N 2 O isotopic reference materials (standards) to enable normalization and reporting of isotope‐delta values. Here we report the isotopic characterization of two pure N 2 O gas reference materials, USGS51 and USGS52, which are now available for laboratory calibration ( https://isotopes.usgs.gov/lab/referencematerials.html ). Methods A total of 400 sealed borosilicate glass tubes of each N 2 O reference gas were prepared from a single gas filling of a high vacuum line. We demonstrated isotopic homogeneity via dual‐inlet isotope‐ratio mass spectrometry. Isotopic analyses of these reference materials were obtained from eight laboratories to evaluate interlaboratory variation and provide preliminary isotopic characterization of their δ 15 N, δ 18 O, δ 15 N α , δ 15 N β and site preference ( S P ) values. Results The isotopic homogeneity of both USGS51 and USGS52 was demonstrated by one‐sigma standard deviations associated with the determinations of their δ 15 N, δ 18 O, δ 15 N α , δ 15 N β and S P values of 0.12 mUr or better. The one‐sigma standard deviations of S P measurements of USGS51 and USGS52 reported by eight laboratories participating in the interlaboratory comparison were 1.27 and 1.78 mUr, respectively. Conclusions The agreement of isotope‐delta values obtained in the interlaboratory comparison was not sufficient to provide reliable accurate isotope measurement values for USGS51 and USGS52. We propose that provisional values for the isotopic composition of USGS51 and USGS52 determined at the Tokyo Institute of Technology can be adopted for normalizing and reporting sample data until further refinements are achieved through additional calibration efforts.

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  8. [해외논문]   Intra‐ and inter‐tooth variation in strontium isotope ratios from prehistoric seals by laser ablation multi‐collector inductively coupled plasma mass spectrometry  

    Glykou, A. (Archaeological Research Laboratory, Stockholm University, SE‐10691, Stockholm ) , Eriksson, G. (Archaeological Research Laboratory, Stockholm University, SE‐10691, Stockholm ) , Storå (Osteoarchaeological Research Laboratory, Stockholm University, SE‐10691, Stockholm ) , , J. (Osteoarchaeological Research Laboratory, Stockholm University, SE‐10691, Stockholm ) , Schmitt, M. (Osteoarchaeological Research Laboratory, Stockholm University, SE‐10691, Stockholm ) , Kooijman, E. (Archaeological Research Laboratory, Stockholm University, SE‐10691, Stockholm) , Lidé , n, K.
    Rapid communications in mass spectrometry : RCM v.32 no.15 ,pp. 1215 - 1224 , 2018 , 0951-4198 ,

    초록

    Rationale Strontium isotope ratios ( 87 Sr/ 86 Sr) in modern‐day marine environments are considered to be homogeneous (~0.7092). However, in the Baltic Sea, the Sr ratios are controlled by mixing seawater and continental drainage from major rivers discharging into the Baltic. This pilot study explores if variations in Sr can be detected in marine mammals from archaeological sites in the Baltic Sea. Methods 87 Sr/ 86 Sr ratios were measured in tooth enamel from three seal species by laser ablation multi‐collector inductively coupled plasma mass spectrometry (LA‐MC‐ICP‐MS). The method enables micro‐sampling of solid materials. This is the first time that the method has been applied to marine samples from archaeological collections. Results The analyses showed inter‐tooth 87 Sr/ 86 Sr variation suggesting that different ratios can be detected in different regions of the Baltic Sea. Furthermore, the intra‐tooth variation suggests possible different geographic origin or seasonal movement of seals within different regions in the Baltic Sea through their lifetime. Conclusions The method was successfully applied to archaeological marine samples showing that: (1) the 87 Sr/ 86 Sr ratio in marine environments is not uniform, (2) 87 Sr/ 86 Sr differences might reflect differences in ecology and life history of different seal species, and (3) archaeological mobility studies based on 87 Sr/ 86 Sr ratios in humans should therefore be evaluated together with diet reconstruction.

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  9. [해외논문]   Spatial and trophic preferences of jumbo squid Dosidicus gigas (D'Orbigny, 1835) in the central Gulf of California: ecological inferences using stable isotopes  

    Trasviñ (Centro Interdisciplinario de Ciencias Marinas, Instituto Politécnico Nacional, Av. IPN s/n, C.P. 23096, La Paz, Baja California Sur, Mexico) , a‐ (Centro Interdisciplinario de Ciencias Marinas, Instituto Politécnico Nacional, Av. IPN s/n, C.P. 23096, La Paz, Baja California Sur, Mexico) , Carrillo, L.D. (Instituto de Ecología, Pesquerías y Oceanografía del Golfo de México, Universidad Autónoma de Campeche (EPOMEX‐UAC), Campus 6. Av. Héroe de Nacozari #480, C.P. 24029, Campeche, Camp, Mexico) , Herná (Centro Interdisciplinario de Ciencias Marinas, Instituto Politécnico Nacional, Av. IPN s/n, C.P. 23096, La Paz, Baja California Sur, Mexico) , ndez‐ (Centro Interdisciplinario de Ciencias Marinas, Instituto Politécnico Nacional, Av. IPN s/n, C.P. 23096, La Paz, Baja California Sur, Mexico) , Herrera, A. , Torres‐ , Rojas, Y.E. , Galvá , n‐ , Magañ , a, F. , Sá , nchez‐ , Gonzá , lez, A. , Aguí , ñ , iga‐ , Garcí , a, S.
    Rapid communications in mass spectrometry : RCM v.32 no.15 ,pp. 1225 - 1236 , 2018 , 0951-4198 ,

    초록

    Rationale The jumbo squid Dosidicus gigas is a fishery resource of considerable economic and ecological importance in the Mexican Pacific. Studies on its habitat preferences are needed to understand recent fluctuations in the abundance and availability of the species. Stable isotope analysis allows us to infer ecological aspects such as spatial distribution and trophic preferences. Methods We used an isotope ratio mass spectrometer, automated for carbonate analysis, and coupled to an elemental analyzer, to determine the isotopic composition of statoliths (δ 18 O and δ 13 C values) and beaks (δ 13 C and δ 15 N values) from 219 individuals caught over two fishing seasons (2007 and 2009) off the coast of Santa RosalIa, in the central Gulf of California. We used these isotopic ratios to assess variation in spatial and trophic preferences by sex, size, and fishing season. Results In the 2009 group, we observed significant differences in statolith δ 13 C values and beak δ 13 C and δ 15 N values between males and females. Between size groups, we observed significant differences in statolith δ 18 O and δ 13 C values in 2007 and in beak δ 13 C and δ 15 N values during both seasons. Both seasons were characterized by high overlap in δ 18 O and δ 13 C values between sexes and in 2009 between size groups. We observed low trophic overlap between sexes in 2009 and between size groups during both seasons. Conclusions The isotopic ratios from statoliths and beaks indicate that D. gigas has changed its spatial and trophic preferences, a shift that is probably related to changes in the species' diet. This intraspecific variation in preferences could be related to characteristics such as size, which may influence squid distribution preferences.

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  10. [해외논문]   A simplified silver phosphate extraction method for oxygen isotope analysis of bioapatite  

    Shabaga, Brandi M. (University of Manitoba, Department of Geological Sciences, 125 Dysart Road, 240 Wallace Building, Winnipeg, R3T 2N2, Canada) , Gough, Hilary (University of Manitoba, Department of Anthropology, 432 Fletcher Argue Building, 15 Chancellor Circle, Winnipeg, R3T 2N2, Canada) , Fayek, Mostafa (University of Manitoba, Department of Geological Sciences, 125 Dysart Road, 240 Wallace Building, Winnipeg, R3T 2N2, Canada) , Hoppa, Robert D. (University of Manitoba, Department of Anthropology, 432 Fletcher Argue Building, 15 Chancellor Circle, Winnipeg, R3T 2N2, Canada)
    Rapid communications in mass spectrometry : RCM v.32 no.15 ,pp. 1237 - 1242 , 2018 , 0951-4198 ,

    초록

    Rationale Although phosphatic materials are chemically complex and are prone to exchange oxygen isotopes with their environments, the phosphate (PO 4 3− ) component of these materials is robust and retains its original oxygen isotopic composition. As a result, there are currently several methods for the isolation of phosphate oxygen through the precipitation of silver phosphate (Ag 3 PO 4 ). However, some of these techniques produce Ag 3 PO 4 of questionable purity, while nearly all are lengthy and/or require relatively large sample sizes. Methods Five milligrams of bioapatite from modern cow teeth (enamel and cementum) were pre‐treated for removal of organic material prior to digestion in 2 M HF. The digested samples were titrated with silver ammine solution at 50°C to precipitate Ag 3 PO 4 . Oxygen isotopic data were collected using a Thermal Combustion Elemental Analyzer (TC/EA) paired with a Delta V Plus isotope ratio mass spectrometer via a ConFlo III universal interface. Results The quality of Ag 3 PO 4 is dependent on effective removal of organic material and the volume of silver ammine solution used during titration. A two‐step pre‐treatment of 2.5% NaOCl, followed by a 0.125 M NaOH solution, is the most effective treatment for the removal of organic material from both enamel and cementum. Optimal yields of Ag 3 PO 4 were achieved using 1.8 mL of silver ammine solution. The reproducibility of the phosphate δ 18 O compositions ranges from 0.3 to 0.4‰ (1σ) for modern cow teeth. Conclusions We present a simplified method for phosphate extraction from organic‐rich phosphatic material. Our method gave reproducible δ 18 O values for enamel and cementum from cows' teeth.

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