WorldWideScience

Sample records for harper jr ms

  1. Geochronology and paleoenvironment of pluvial Harper Lake, Mojave Desert, California, USA

    Science.gov (United States)

    Garcia, Anna L.; Knott, Jeffrey R.; Mahan, Shannon; Bright, Jordan

    2014-01-01

    Accurate reconstruction of the paleo-Mojave River and pluvial lake (Harper, Manix, Cronese, and Mojave) system of southern California is critical to understanding paleoclimate and the North American polar jet stream position over the last 500 ka. Previous studies inferred a polar jet stream south of 35°N at 18 ka and at ~ 40°N at 17–14 ka. Highstand sediments of Harper Lake, the upstream-most pluvial lake along the Mojave River, have yielded uncalibrated radiocarbon ages ranging from 24,000 to > 30,000 14C yr BP. Based on geologic mapping, radiocarbon and optically stimulated luminescence dating, we infer a ~ 45–40 ka age for the Harper Lake highstand sediments. Combining the Harper Lake highstand with other Great Basin pluvial lake/spring and marine climate records, we infer that the North American polar jet stream was south of 35°N about 45–40 ka, but shifted to 40°N by ~ 35 ka. Ostracodes (Limnocythere ceriotuberosa) from Harper Lake highstand sediments are consistent with an alkaline lake environment that received seasonal inflow from the Mojave River, thus confirming the lake was fed by the Mojave River. The ~ 45–40 ka highstand at Harper Lake coincides with a shallowing interval at downstream Lake Manix.

  2. Ending a HarperCollins Boycott (February 27, 2011-August 7, 2013

    Directory of Open Access Journals (Sweden)

    Brett Bonfield

    2013-08-01

    Full Text Available On February 24, 2011, Joe Atzenberger broke the news that HarperCollins would begin distributing self-destructing ebooks through OverDrive. This was not welcome news.At the time, if public libraries wanted to lend ebooks to the communities they served, signing a contract with OverDrive was the only viable way for them to do it. The fact that OverDrive agreed to this stipulation from HarperCollins meant that libraries had no choice. Any ebooks they licensed from HarperCollins would become inoperable after 26 circulations. If libraries wished to continue to circulate these titles, they would have to pay for a license that granted them another 26 circulations.After reading Atzenberger’s post, Bobbi Newman wrote a post about HarperCollins’ self-destructing ebooks on her widely read blog, Librarian by Day. Over the next week, she updated her post, adding links to responses from OverDrive President and Chief Executive Officer, Steve Potash, as well as responses by dozens of librarians and non-librarians.One of the ideas people raised was a HarperCollins boycott. The day after Bobbi Newman’s post, my friend Gabriel Farrell and I got together and created a website to let the world know that many people were going to boycott HarperCollins until it changed its policies, and to explain why people were making this decision.

  3. Subordinations In “To Kill A Mockingbird” By Harper Lee

    OpenAIRE

    Siregar, Rut Sri Novitawaty

    2011-01-01

    Salah satu yang dipelajari mahasiswa adalah tulis menulis. Secara ilmiah tulis menulis adalah penyampaian informasi dalam bentuk tulisan serta bagaimana informasi itu disampaikan. Judul kertas karya ini adalah Kalimat Subordinat yang ditemukan dalam novel To Kill a Mockingbird karya Harper Lee: SUBORDINATION IN TO KILL A MOCKINGBIRD BY HARPER LEE. Penulis mengangkat hal ini karena penulis tertarik dengan bentuk–bentuk serta fungsi-fungsi kalimat subordinat yang terdapat dalam tulisan-tulisan ...

  4. Topological phase transitions from Harper to Fibonacci crystals

    Science.gov (United States)

    Amit, Guy; Dana, Itzhack

    2018-02-01

    Topological properties of Harper and generalized Fibonacci chains are studied in crystalline cases, i.e., for rational values of the modulation frequency. The Harper and Fibonacci crystals at fixed frequency are connected by an interpolating one-parameter Hamiltonian. As the parameter is varied, one observes topological phase transitions, i.e., changes in the Chern integers of two bands due to the degeneracy of these bands at some parameter value. For small frequency, corresponding to a semiclassical regime, the degeneracies are shown to occur when the average energy of the two bands is approximately equal to the energy of the classical separatrix. Spectral and topological features of the Fibonacci crystal for small frequency leave a clear imprint on the corresponding Hofstadter butterfly for arbitrary frequency.

  5. Ridit Analysis for Cooper-Harper and Other Ordinal Ratings for Sparse Data - A Distance-based Approach

    Science.gov (United States)

    2016-09-01

    412TW-PA-16437 Ridit Analysis for Cooper -Harper & other Ordinal Ratings for Sparse Data – A...2016 2. REPORT TYPE TECHNICAL PAPER 3. DATES COVERED (From - To) 09-19-2016 4. TITLE AND SUBTITLE RIDIT ANALYSIS FOR COOPER -HARPER & OTHER...opinion rankings, are common in many areas of application. In the Air Force, Cooper - Harper ratings are used extensively for the assessment of Flying

  6. The algebraic geometry of Harper operators

    International Nuclear Information System (INIS)

    Li, Dan

    2011-01-01

    Following an approach developed by Gieseker, Knoerrer and Trubowitz for discretized Schroedinger operators, we study the spectral theory of Harper operators in dimensions 2 and 1, as a discretized model of magnetic Laplacians, from the point of view of algebraic geometry. We describe the geometry of an associated family of Bloch varieties and compute their density of states. Finally, we also compute some spectral functions based on the density of states. We discuss the difference between the cases with rational or irrational parameters: for the two-dimensional Harper operator, the compactification of the Bloch variety is an ordinary variety in the rational case and an ind-pro-variety in the irrational case. This gives rise, at the algebro-geometric level of Bloch varieties, to a phenomenon similar to the Hofstadter butterfly in the spectral theory. In dimension 2, the density of states can be expressed in terms of period integrals over Fermi curves, where the resulting elliptic integrals are independent of the parameters. In dimension 1, for the almost Mathieu operator, with a similar argument, we find the usual dependence of the spectral density on the parameter, which gives rise to the well-known Hofstadter butterfly picture. (paper)

  7. The algebraic geometry of Harper operators

    Science.gov (United States)

    Li, Dan

    2011-10-01

    Following an approach developed by Gieseker, Knörrer and Trubowitz for discretized Schrödinger operators, we study the spectral theory of Harper operators in dimensions 2 and 1, as a discretized model of magnetic Laplacians, from the point of view of algebraic geometry. We describe the geometry of an associated family of Bloch varieties and compute their density of states. Finally, we also compute some spectral functions based on the density of states. We discuss the difference between the cases with rational or irrational parameters: for the two-dimensional Harper operator, the compactification of the Bloch variety is an ordinary variety in the rational case and an ind-pro-variety in the irrational case. This gives rise, at the algebro-geometric level of Bloch varieties, to a phenomenon similar to the Hofstadter butterfly in the spectral theory. In dimension 2, the density of states can be expressed in terms of period integrals over Fermi curves, where the resulting elliptic integrals are independent of the parameters. In dimension 1, for the almost Mathieu operator, with a similar argument, we find the usual dependence of the spectral density on the parameter, which gives rise to the well-known Hofstadter butterfly picture.

  8. An Analysis Of Intrinsic Elements In Harper Lee’s To Kill A Mockingbird

    OpenAIRE

    Simbolon, Hendra Halomoan

    2011-01-01

    Skripsi ini berjudul “An Analysis of Intrinsic Elements in Harper Lee’s To Kill A Mockingbird”. Skripsi ini mengenai unsur-unsur intrinsik yakni karakter, plot, setting, tema, sudut pandang dan gaya penulisan yang terdapat pada karya Charles Dickens yang berjudul To Kill A Mockingbird. Di dalam skripsi ini, penulis ingin membuktikan keterkaitan unsur-unsur intrinsik yang terdapat dalam novel To Kill A Mockingbird karya Harper Lee. Adapun metode yang digunakan penul...

  9. The Search for a Cold War Grand Strategy: NSC 68 & 162

    Science.gov (United States)

    2014-05-22

    Harper Collins Publishers, 1990. Chandler , Alfred D., Jr., and Louis Galamos Jr. The Papers of Dwight D. Eisenhower. Baltimore, MD, 1970. Cutler...76Alfred D. Chandler Jr., and Louis Galamos Jr., The Papers of Dwight D. Eisenhower (Baltimore, MD, 1970), Vol. 11, 1312; Vol. 8, 1609. 77Ibid

  10. Geology of the Harper Quadrangle, Liberia

    Science.gov (United States)

    Brock, M.R.; Chidester, A.H.; Baker, M.G.W.

    1974-01-01

    As part of a program undertaken cooperatively by the Liberian Geological Survey (LGS) and the U. S. Geological Survey (USGS), under the sponsorship of the Government of Liberia and the Agency for International Development, U. S. Department of State, Liberia was mapped by geologic and geophysical methods during the period 1965 to 1972. The resulting geologic and geophysical maps are published in ten folios, each covering one quadrangle (see index map). The first systematic mapping in the Harper quadrangle was by Baker, S. P. Srivastava, and W. E. Stewart (LGS) at a scale of 1:500,000 in the vicinity of Harper in the southeastern, and of Karloke in the northeastern part of the quadrangle in 1960-61. Brock and Chidester carried out systematic mapping of the quadrangle at a scale of 1:250,000 in the period September 1971-May 1972; the geologic map was compiled from field data gathered by project geologists and private companies as indicated in the source diagram, photogeologic maps, interpretation of airborne magnetic and radiometric surveys, field mapping, and ground-based radiometric surveys in which hand-held scintillators were used. R. W. Bromery, C. S. Wotorson, and J. C. Behrendt contributed to the interpretation of geophysical data. Total-intensity aeromagnetic and total-count gamma radiation maps (Behrendt and Wotorson, in press a, b), and unpublished data derived from those maps, including the near-surface and the regional magnetic components and aeromagnetic/radiometric correlations, were used in the interpretation.

  11. Hofstadter butterflies in nonlinear Harper lattices, and their optical realizations

    International Nuclear Information System (INIS)

    Manela, Ofer; Segev, Mordechai; Christodoulides, Demetrios N; Kip, Detlef

    2010-01-01

    The ubiquitous Hofstadter butterfly describes a variety of systems characterized by incommensurable periodicities, ranging from Bloch electrons in magnetic fields and the quantum Hall effect to cold atoms in optical lattices and more. Here, we introduce nonlinearity into the underlying (Harper) model and study the nonlinear spectra and the corresponding extended eigenmodes of nonlinear quasiperiodic systems. We show that the spectra of the nonlinear eigenmodes form deformed versions of the Hofstadter butterfly and demonstrate that the modes can be classified into two families: nonlinear modes that are a 'continuation' of the linear modes of the system and new nonlinear modes that have no counterparts in the linear spectrum. Finally, we propose an optical realization of the linear and nonlinear Harper models in transversely modulated waveguide arrays, where these Hofstadter butterflies can be observed. This work is relevant to a variety of other branches of physics beyond optics, such as disorder-induced localization in ultracold bosonic gases, localization transition processes in disordered lattices, and more.

  12. Hofstadter butterflies in nonlinear Harper lattices, and their optical realizations

    Energy Technology Data Exchange (ETDEWEB)

    Manela, Ofer; Segev, Mordechai [Department of Physics and Solid State Institute, Technion, Haifa 32000 (Israel); Christodoulides, Demetrios N [College of Optics/CREOL, University of Central Florida, FL 32816-2700 (United States); Kip, Detlef, E-mail: msegev@tx.technion.ac.i [Department of Electrical Engineering, Helmut Schmidt University, 22043 Hamburg (Germany)

    2010-05-15

    The ubiquitous Hofstadter butterfly describes a variety of systems characterized by incommensurable periodicities, ranging from Bloch electrons in magnetic fields and the quantum Hall effect to cold atoms in optical lattices and more. Here, we introduce nonlinearity into the underlying (Harper) model and study the nonlinear spectra and the corresponding extended eigenmodes of nonlinear quasiperiodic systems. We show that the spectra of the nonlinear eigenmodes form deformed versions of the Hofstadter butterfly and demonstrate that the modes can be classified into two families: nonlinear modes that are a 'continuation' of the linear modes of the system and new nonlinear modes that have no counterparts in the linear spectrum. Finally, we propose an optical realization of the linear and nonlinear Harper models in transversely modulated waveguide arrays, where these Hofstadter butterflies can be observed. This work is relevant to a variety of other branches of physics beyond optics, such as disorder-induced localization in ultracold bosonic gases, localization transition processes in disordered lattices, and more.

  13. Aesthetic Sustainability - Product Design and Sustainable Usage, by Kristine H. Harper

    DEFF Research Database (Denmark)

    Galle, Per

    2017-01-01

    As the window for action against irreversible climate changes is narrowing, Harper offers timely and practical advice on how, as designers and consumers, we can take responsibility for creating a sustainable future. Though informed by a deep understanding of the complexities of aesthetics...

  14. Spectral relationships between kicked Harper and on-resonance double kicked rotor operators

    DEFF Research Database (Denmark)

    Lawton, Wayne; Mouritzen, Anders Sørrig; Wang, Jiao

    2009-01-01

    Kicked Harper operators and on-resonance double kicked rotor operators model quantum systems whose semiclassical limits exhibit chaotic dynamics. Recent computational studies indicate a striking resemblance between the spectra of these operators. In this paper we apply C*-algebra methods to expla...

  15. Rescripting a Troubled Past: John Brown's Family and the Harpers Ferry Conspiracy.

    Science.gov (United States)

    McGlone, Robert E.

    1989-01-01

    Uses autobiographical information constructed by John Brown's family in the aftermath of Harpers Ferry to illustrate the issue of rescripting of history. Points out that this nondeliberate rewriting of the past is a result of the personal need to refocus self-schema and the validation of false memories as authentic. (KO)

  16. Cooper-Harper Experience Report for Spacecraft Handling Qualities Applications

    Science.gov (United States)

    Bailey, Randall E.; Jackson, E. Bruce; Bilimoria, Karl D.; Mueller, Eric R.; Frost, Chad R.; Alderete, Thomas S.

    2009-01-01

    A synopsis of experience from the fixed-wing and rotary-wing aircraft communities in handling qualities development and the use of the Cooper-Harper pilot rating scale is presented as background for spacecraft handling qualities research, development, test, and evaluation (RDT&E). In addition, handling qualities experiences and lessons-learned from previous United States (US) spacecraft developments are reviewed. This report is intended to provide a central location for references, best practices, and lessons-learned to guide current and future spacecraft handling qualities RDT&E.

  17. Keberanian Dalam Novel to Kill a Mockingbird Karya Harper Lee

    OpenAIRE

    Tiolemba, Melissa

    2013-01-01

    The skripsi is entitled “Keberanian dalam Novel To Kill a Mockingbird by Harper Lee”. The objective of this research is to analyze the bravery as the main theme in the novel To Kill a Mockingbird. The data are collected by focusing on the character, plot and setting which describe about the main theme in the story. This research uses the theory of Stanton (1965) in analyzing the data. The writer uses descriptive method intrinsically. Intrinsic approach is to examine the elements within the no...

  18. Ultra light weight jet engine JR100; Chokeiryo jet engine JR100

    Energy Technology Data Exchange (ETDEWEB)

    Matsuki, M. [Nippon Institute of Technology, Saitama (Japan)

    1999-03-20

    As a part of the jet lift V/STOL research by National Aerospace Laboratory, a study of trial manufacture of ultra light weight jet engine JR 100 started in FY 1964. The study was aimed at obtaining a lift engine for VTOL and founding the base for the future jet lift VTOL, and at taking in the results of the jet engine element study accumulated so far and manufacturing an advanced engine. Decided on the use of domestic materials for JR 100, the materials to be used are almost iron-based ones. Through the efforts for weight reduction in structure and processing, a thrust/weight ratio of 10 was realized. At the same time, the production/processing of light weight materials such as titanium alloys was proceeded with, and by adopting the materials to JR 200 system, a thrust/weight ratio of 15 was realized. Together with these, for the purpose of reducing the fuel consumption rate, studies started on fan for lift fan engine and high temperature turbine (an inlet temperature of 1250 degrees C was achieved), to get low noise/high efficiency fan. By the research results, the basis for jet lift VTOL was established, and it became the basis for the development of turbo fan engine FJR 710. (NEDO)

  19. A garden of orchids: a generalized Harper equation at quadratic irrational frequencies

    International Nuclear Information System (INIS)

    Mestel, B D; Osbaldestin, A H

    2004-01-01

    We consider a generalized Harper equation at quadratic irrational flux, showing, in the strong coupling limit, the fluctuations of the exponentially decaying eigenfunctions are governed by the dynamics of a renormalization operator on a renormalization strange set. This work generalizes previous analyses which have considered only the golden mean case. Projections of the renormalization strange sets are illustrated analogous to the 'orchid' present in the golden mean case

  20. A garden of orchids: a generalized Harper equation at quadratic irrational frequencies

    Energy Technology Data Exchange (ETDEWEB)

    Mestel, B D [Department of Computing Science and Mathematics, University of Stirling, Stirling FK9 4LA (United Kingdom); Osbaldestin, A H [Department of Mathematics, University of Portsmouth, Portsmouth PO1 3HE (United Kingdom)

    2004-10-01

    We consider a generalized Harper equation at quadratic irrational flux, showing, in the strong coupling limit, the fluctuations of the exponentially decaying eigenfunctions are governed by the dynamics of a renormalization operator on a renormalization strange set. This work generalizes previous analyses which have considered only the golden mean case. Projections of the renormalization strange sets are illustrated analogous to the 'orchid' present in the golden mean case.

  1. 77 FR 61003 - Stephen C. Delaney, Jr.: Debarment Order

    Science.gov (United States)

    2012-10-05

    ...] Stephen C. Delaney, Jr.: Debarment Order AGENCY: Food and Drug Administration, HHS. ACTION: Notice... Cosmetic Act (the FD&C Act) debarring Stephen C. Delaney, Jr. for a period of 5 years from importing....35), finds that Mr. Stephen C. Delaney, Jr. has been convicted of a felony under Federal law for...

  2. An Analysis Of American Social Condition In THE Middle Of 20Th Century Viewed In Harper Lee’s Novel To Kill A Mockingbird

    OpenAIRE

    Saragih, Dix Wendy

    2010-01-01

    Skripsi ini berjudul The Analysis of American Social Condition in the Middle of Twentieth Century Viewed in Harper Lee’s Novel To Kill A Mockingbird. Yaitu suatu analisis mengenai kondisi sosial masyarakat di Amerika Serikat pada pertengahan abad 20 yang terlihat dalam novel To Kill A Mockingbird karya dari Harper Lee. Dalam analisis ini, penulis menggunakan pendekatan historis mengenai sejarah Amerika pada pertengahan abad keduapuluh. Adapun metode yang digunakan adalah metode deskriptif ...

  3. Feasibility Study for Establishing a Small Business Management Course at Harper. Volume XVII, Number 3.

    Science.gov (United States)

    Seeck, James K.; Lucas, John A.

    In 1988, a survey was conducted to determine the feasibility of offering a new degree credit program in Small Business Management at William Rainey Harper College, in Illinois. All 3,170 former students who had taken a non-credit seminar in the Small Business Department in Continuing Education were surveyed regarding their interest in small…

  4. A. P. Sloan Jr. and leadership

    Directory of Open Access Journals (Sweden)

    Paul Marinescu

    2014-05-01

    Full Text Available Organizing the manufacturing processes constituted probably the most difficult challenge in the American automotive industry in the 1920s. A. P. Sloan Jr. was one of the greatest captains of industry and shaped General Motors Corporation into the largest automotive manufacturer of the world. His creative approach on how to mix a degree of decentralized responsibility with centralized control remains a useful example for every corporate leader. The aim of our paper is to emphasize the contribution of Sloan Jr. to the development of leadership. The methodological approach is literature review.

  5. Golden mean renormalization for a generalized Harper equation: The Ketoja-Satija orchid

    International Nuclear Information System (INIS)

    Mestel, B.D.; Osbaldestin, A.H.

    2004-01-01

    We provide a rigorous analysis of the fluctuations of localized eigenstates in a generalized Harper equation with golden mean flux and with next-nearest-neighbor interactions. For next-nearest-neighbor interaction above a critical threshold, these self-similar fluctuations are characterized by orbits of a renormalization operator on a universal strange attractor, whose projection was dubbed the ''orchid'' by Ketoja and Satija [Phys. Rev. Lett. 75, 2762 (1995)]. We show that the attractor is given essentially by an embedding of a subshift of finite type, and give a description of its periodic orbits

  6. Fatal hemolytic disease of the fetus and newborn associated with anti-Jr.

    Science.gov (United States)

    Peyrard, Thierry; Pham, Bach-Nga; Arnaud, Lionel; Fleutiaux, Sophie; Brossard, Yves; Guerin, Bénédicte; Desmoulins, Isabelle; Rouger, Philippe; Le Pennec, Pierre-Yves

    2008-09-01

    Jr(a) is a high-prevalence red cell (RBC) antigen. The clinical significance of anti-Jr(a) is controversial. When hemolytic disease of the fetus and newborn (HDFN) occurred, most reported cases were clinically mild. We report the first case of fatal HDFN due to anti-Jr(a). A 28-year-old Caucasian woman with transfusion history was monitored at the 29th week of pregnancy (G4P1). An ultrasound scan showed fetal cardiomegaly and hepatomegaly. An antibody directed against a high-prevalence antigen was detected, but without conclusive identification. An emergency cesarean section was performed at the 36th week. The newborn was hydropic and showed severe anemia. Death occurred 30 hours after birth. Serologic methods were performed to investigate the mother's RBCs and serum. An in vitro functional cellular assay and semiquantitative measurement of anti-Jr(a) were used to determine the clinical significance of the antibody. Anti-Jr(a) was identified in the serum and Jr(a-) phenotype was confirmed. The anti-Jr(a) titer was 1024, with predominant immunoglobulin (Ig)G1 and minor IgG4 subclasses. The functional cellular assay was consistent with an antibody unlikely to cause HDFN. Semiquantitative measurement of anti-Jr(a) showed a reactivity equivalent to a 25 IU per mL (5 microg/mL) concentration of anti-D, a value associated with a significant risk of HDFN. This is the first documented case of fatal HDFN due to anti-Jr(a). Therefore, we recommend close monitoring of pregnant women with a high-titer anti-Jr(a), especially those with an incompatible transfusion history and/or multiple pregnancies. This case report provides new arguments about the clinical significance of anti-Jr(a) in the transfusion setting.

  7. Dr. Martin Luther King, Jr. as Spiritual Leader

    Directory of Open Access Journals (Sweden)

    Andrea Pierce

    2013-09-01

    Full Text Available The purpose of this paper is to explore Dr. Martin Luther King Jr.’s spiritual leadership through his “I Have a Dream” speech. The paper explores the three characteristics of spiritual leadership as posed by Fry’s (2003 spiritual leadership theory: vision, hope/faith and altruistic love. The research draws upon these characteristics through qualitative content analysis of Dr. Martin Luther King Jr.’s “I Have a Dream” speech to illustrate Dr. King’s leadership as that of a spiritual leader. The research advances the spiritual leadership theory by establishing Dr. Martin Luther King Jr. as a spiritual leader. Through the illustration of Dr. King’s spiritual leadership, the characteristics of a spiritual leader are given tangible understanding.

  8. Draft genome sequence of Therminicola potens strain JR

    Energy Technology Data Exchange (ETDEWEB)

    Byrne-Bailey, K.G.; Wrighton, K.C.; Melnyk, R.A.; Agbo, P.; Hazen, T.C.; Coates, J.D.

    2010-07-01

    'Thermincola potens' strain JR is one of the first Gram-positive dissimilatory metal-reducing bacteria (DMRB) for which there is a complete genome sequence. Consistent with the physiology of this organism, preliminary annotation revealed an abundance of multiheme c-type cytochromes that are putatively associated with the periplasm and cell surface in a Gram-positive bacterium. Here we report the complete genome sequence of strain JR.

  9. Placental Vascular Tree as Biomarker of Autism/ASD Risk

    Science.gov (United States)

    2013-09-01

    use the fact that the same biochemistry that controls the branching of nerves also controls branching of blood vessels. Unlike the nerve networks in...Mercer BM, Thorp JM Jr, Malone FD, Harper M, Iams JD, Anderson GD. Eunice Kennedy Shriver National Institute of Child Health and Human Development

  10. Framework for technical assessment in JR Maglev

    Energy Technology Data Exchange (ETDEWEB)

    Seki, Akio [Central Japan Railway Co., Tokyo (Japan); Akahoshi, Toru [Central Japan Railway Co., Tokyo (Japan); Furuki, Tsutomu [Railway Technical Research Inst., Tokyo (Japan)

    1995-12-31

    In the course of development of JR Maglev, various technical assessments are carried out at each stage of development by a system management group of a project team in order to achieve goals of development. For the purpose, guidelines for practicality assessment were prepared at design stage. It is now striven to make test plans necessary for the practicality assessment. This assessment will serve for those to be ultimately implemented by Ministry of Transport (MOT). This paper presents an overview of concepts, methods and procedures of the technical assessments especially focused on the practicality assessment in the development of JR Maglev. (orig.)

  11. Follow-Up Study of Former Materials/Logistics Management Students at Harper College, 1990-1995. Volume XXIV, Number 14.

    Science.gov (United States)

    Lucas, John A.; Magad, Eugene

    In fall 1995, William Rainey Harper College in Illinois conducted a study of former students in the Materials/Logistics Management (MLM) program to determine their evaluation of their educational experiences in the program. The sample consisted of 298 former MLM students from 1990 to 1995, including 119 students who had earned 48 credit hours but…

  12. 78 FR 5247 - Martin Luther King, Jr., Federal Holiday, 2013

    Science.gov (United States)

    2013-01-24

    ..., 2013 Martin Luther King, Jr., Federal Holiday, 2013 By the President of the United States of America A... thousands upon thousands rallying for jobs and freedom, the Reverend Dr. Martin Luther King, Jr., delivered... Constitution and the laws of the United States, do hereby proclaim January 21, 2013, as the Martin Luther King...

  13. The Newest Monument: The Martin Luther King, Jr. National Memorial

    Science.gov (United States)

    Social Studies and the Young Learner, 2011

    2011-01-01

    This article features the newest monument, the Martin Luther King, Jr. National Memorial. The memorial on the National Mall in Washington, D.C., honoring Dr. Martin Luther King, Jr. will be an engaging landscape experience to convey four fundamental and recurring themes throughout Dr. King's life--democracy, justice, hope, and love. Natural…

  14. Case report: massive postpartum transfusion of Jr(a+) red cells in the presence of anti-Jra.

    Science.gov (United States)

    Yuan, S; Armour, R; Reid, A; Abdel-Rahman, K F; Rumsey, D M; Phillips, M; Nester, T

    2005-01-01

    Jr(a) is a high-prevalence antigen. The rare Jr(a-) individuals can form anti-Jr(a) after exposure to the Jr(a) antigen through transfusion or pregnancy. The clinical significance of anti-Jr(a) is not well established. This study reports a case of a 31-year-old woman with a previously identified anti-Jr(a) who required massive transfusion of RBCs after developing life-threatening postpartum disseminated intravascular coagulopathy. Despite the emergent transfusion of 15 units of Jr(a) untested RBCs, she did not develop laboratory or clinical evidence of acute hemolysis. The patient's anti-Jr(a) had a pretransfusion titer of 4 and a monocyte monolayer assay (MMA) reactivity of 68.5% (reactivity > 5% is considered capable of shortening the survival of incompatible RBCs). The titer increased fourfold to 64 and the MMA reactivity was 72.5% on Day 10 posttransfusion. Review of laboratory data showed evidence of a mild delayed hemolytic transfusion reaction by Day 10 posttransfusion. Despite rare reports of hemolytic transfusion reactions due to anti-Jr(a) in the literature, most cases, including this one, report that this antibody is clinically insignificant or causes only mild delayed hemolysis. Clinicians should be advised to balance the risks of withholding transfusion with the small chance of significant hemolysis after transfusion of Jr(a+) RBCs in the presence of anti-Jr(a).

  15. The Words of Martin Luther King, Jr.

    Science.gov (United States)

    Today's Education, 1979

    1979-01-01

    Excerpts from speeches by Dr. Martin Luther King, Jr., are reprinted. Topics discussed include discrimination, the South, education, nonviolent resistance, poverty, economic opportunity, and world peace. (LH)

  16. Elastic-plastic fracture assessment using a J-R curve by direct method

    International Nuclear Information System (INIS)

    Asta, E.P.

    1996-01-01

    In the elastic-plastic evaluation methods, based on J integral and tearing modulus procedures, an essential input is the material fracture resistance (J-R) curve. In order to simplify J-R determination direct, a method from load-load point displacement records of the single specimen tests may be employed. This procedure has advantages such as avoiding accuracy problems of the crack growth measuring devices and reducing testing time. This paper presents a structural integrity assessment approach, for ductile fracture, using the J-R obtained by a direct method from small single specimen fracture tests. The J-R direct method was carried out by means of a developed computational program based on theoretical elastic-plastic expressions. A comparative evaluation between the direct method J resistance curves and those obtained by the standard testing methodology on typical pressure vessel steels has been made. The J-R curves estimated from the direct method give an acceptable agreement with the approach proposed in this study which is reliable to use for engineering determinations. (orig.)

  17. SHOCK-JR: a computer program to analyze impact response of shipping container

    International Nuclear Information System (INIS)

    Ikushima, Takeshi; Nakazato, Chikara; Shimoda, Osamu; Uchino, Mamoru.

    1983-02-01

    The report is provided for using a computer program, SHOCK-JR, which is used to analyze the impact response of shipping containers. Descriptions are the mathematical model, method of analysis, structures of the program and the input and output variables. The program solves the equations of motion for a one-dimensional, lumped mass and nonlinear spring model. The solution procedure uses Runge-Kutta-Gill and Newmark-β methods. SHOCK-JR is a revised version of SHOCK, which was developed by ORNL. In SHOCK-JR, SI dimension is used and graphical output is available. (author)

  18. Analytic Quasi-Perodic Cocycles with Singularities and the Lyapunov Exponent of Extended Harper's Model

    Science.gov (United States)

    Jitomirskaya, S.; Marx, C. A.

    2012-11-01

    We show how to extend (and with what limitations) Avila's global theory of analytic SL(2,C) cocycles to families of cocycles with singularities. This allows us to develop a strategy to determine the Lyapunov exponent for the extended Harper's model, for all values of parameters and all irrational frequencies. In particular, this includes the self-dual regime for which even heuristic results did not previously exist in physics literature. The extension of Avila's global theory is also shown to imply continuous behavior of the LE on the space of analytic {M_2({C})}-cocycles. This includes rational approximation of the frequency, which so far has not been available.

  19. Martin Luther King Jr. contest winning posters to be displayed in downtown Blacksburg

    OpenAIRE

    Shannon, Kelly Baker

    2010-01-01

    Each year as part of the Martin Luther King Jr. celebration at Virginia Tech area kindergarten through 12th grade students are invited to participate in the annual Martin Luther King Jr. poster contest.

  20. Diffusion by extrinsic noise in the kicked Harper map

    International Nuclear Information System (INIS)

    Park, Gunyoung; Chang, C. S.

    2001-01-01

    A significantly improved analytic understanding of the extrinsically driven diffusion process is presented in a nonlinear dynamical system in which the phase space is divided into periodic two-dimensional tiles of regular motion, separated by a connected separatrix network (web) [previously studied by A. J. Lichtenberg and Blake P. Wood, Phys. Rev. Lett. >62, 2213 (1989)]. The system is represented by the usual 'kicked Harper map' with added extrinsic noise terms. Three different diffusion regimes are found depending upon the strength of the extrinsic perturbation l relative to the web and regular motions. When the extrinsic noise is dominant over the intrinsic stochasticity and the regular rotation motions in the tile, diffusion obeys the random phase scaling l 2 . When the extrinsic noise is dominant over the intrinsic stochasticity, but weaker than the regular rotation motion, the diffusion scales as lK 1/2 , where K is the strength of the intrinsic kick. These findings agree well with numerical simulation results. When the extrinsic noise process is weaker than the stochastic web process, we analytically reproduce the well-known numerical result: The web diffusion is reduced by the ratio of phase-space areas of intrinsic to extrinsic stochasticity

  1. Views of Dr. Martin Luther King, Jr.

    Science.gov (United States)

    Davis, Alan H.

    1990-01-01

    Discusses views of Martin Luther King, Jr., including concepts of human rights, related counseling approaches, and ethics. Claims King's views provide helpful insights for counselors and clients. Concludes King invited individuals to view challenging life situations as moral opportunities. (Author/ABL)

  2. Letters of Second Lieutenant Charles Wesley Chapman, Jr. December 19, 1894 - May 3, 1918

    Science.gov (United States)

    2016-04-01

    that every possible channel of communication will be utilized to ascertain the whereabouts of your son. The personal effects of 2nd. Lieut. Charles W...AIR UNIVERSITY AIR FORCE RESEARCH INSTITUTE Letters of Second Lieutenant Charles Wesley Chapman, Jr. December 19, 1894–May 3, 1918 Air Force...in-Publication Data Chapman, Charles Wesley, Jr., 1894–1918. Letters of Second Lieutenant Charles Wesley Chapman, Jr., December 19, 1894–May 3, 1918

  3. 78 FR 57105 - Wm. Wrigley Jr. Company; Filing of Color Additive Petition

    Science.gov (United States)

    2013-09-17

    ... lead in synthetic iron oxide for human food use. DATES: The color additive petition was filed on July.... FDA-2013-C-1008] Wm. Wrigley Jr. Company; Filing of Color Additive Petition AGENCY: Food and Drug... announcing that we have filed a petition, submitted by the Wm. Wrigley Jr. Company, proposing that the color...

  4. Religión y Paz en Martin Luther King Jr.

    OpenAIRE

    Mussio, Ria Stacy

    2016-01-01

    Esta tesis pretende mostrar el rol integral que la religión desempeñaba en la obtención de los derechos civiles para los afroamericanos y, también en el logro de la paz positiva. Martin Luther King Jr. y la mayoría de los manifestantes del movimiento eran cristianos, poniendo su fe en Dios, para el pleno disfrute de sus derechos humanos. King Jr., anclado en su fe, impulsó el avance de los derechos civiles, mediante la resistencia no violenta. El primer capítulo tiene como finalidad orientar ...

  5. Claim on memory : a political biography of Franklin D. Roosevelt, Jr., 1914-1988

    NARCIS (Netherlands)

    Berg, Erik Eduard Willem van den

    2006-01-01

    This dissertation focuses on the political life of Franklin D. Roosevelt, Jr., the third surviving son of Franklin D. Roosevelt and Eleanor Roosevelt. The key question of this study emphasizes how FDR, Jr. interpreted the Roosevelt name and legacy during his life and political career. This book

  6. 3 CFR 8340 - Proclamation 8340 of January 15, 2009. Martin Luther King, Jr., Federal Holiday, 2009

    Science.gov (United States)

    2010-01-01

    ... Proclamation 8340 of January 15, 2009 Proc. 8340 Martin Luther King, Jr., Federal Holiday, 2009By the President of the United States of America A Proclamation On the Martin Luther King, Jr., Federal Holiday, we... Constitution and laws of the United States, do hereby proclaim January 19, 2009, as the Martin Luther King, Jr...

  7. 1997 Arthur Ashe Jr. Sport Scholars Awards.

    Science.gov (United States)

    Roach, Ronald

    1997-01-01

    Winners of the "Black Issues in Higher Education" Arthur Ashe Jr. 1997 athletes of the year, one male and one female, are profiled and Sport Scholars are listed for baseball, softball, basketball, fencing, archery, football, handball, soccer, field hockey, crew, swimming, gymnastics, tennis, squash, golf, volleyball, lacrosse, wrestling, water…

  8. Karl A. Gschneidner Jr (1930–2016)

    International Nuclear Information System (INIS)

    Pecharsky, Vitalij K.

    2016-01-01

    Presented here is the obituary for Karl Albert Gschneidner Jr. He died on 27 April 2016. Nicknamed Mr Rare Earth, he holds an unparalleled place as the renowned authority in just about every aspect related to the science, technology and history of a very special family of elements — the rare earths.

  9. Revisions of the Learning Mastery Systems for the Harper and Row Grades One and Two and the Macmillan Bank Street Grade One Reading Series.

    Science.gov (United States)

    Maeder, Jacqueline; And Others

    The revisions on the Learning Mastery Systems (LMSs) for the Harper & Row grade-one and grade-two and the Macmillan Bank Street grade-one reading programs are outlined in this document. A rationale for the revisions is presented. An LMS is a set of materials and procedures prepared by the southwest Regional Laboratory (SWRL) as an…

  10. The Manuel Lujan Jr. Neutron Scattering Center

    International Nuclear Information System (INIS)

    Goldstone, J.A.

    1994-01-01

    High in the northcentral mountains of Los Alamos, New Mexico, is the Manuel Lujan Jr. Neutron Scattering Center (LANSCE), a pulsed-spallation neutron source located at Los Alamos National Laboratory. At LANSCE, neutrons are produced by spallation when a pulsed 800-MeV proton beam impinges on a tungsten target. The proton pulses are provided by a linear accelerator and an associated Proton Storage Ring (PSR), which alters the intensity, time structure, and repetition rate of the pulses. In October 1986, LANSCE was designated a national user facility, with a formal user program initiated in 1988. In July 1989, the LANSCE facility was dedicated as the Manuel Lujan Jr. Neutron Scattering Center in honor of the long-term Congressman from New Mexico. At present, the PSR operates with a proton pulse width of 0.27 μs at 20 Hz and 80 μA, attaining the highest peak neutron flux in the world and close to its goal of 100 μA, which would yield a peak thermal neutron flux of 10 16 n/cm -2 s -1 . This paper discusses the target/moderator/reflector shield system, the LANSCE instruments, the facility improvement projects, and user programs

  11. Connect the Book. Martin's Big Words: The Life of Dr. Martin Luther King, Jr.

    Science.gov (United States)

    Brodie, Carolyn S.

    2005-01-01

    In honor of Martin Luther King, Jr. Day, this month's featured book is "Martin's Big Words: The Life of Dr. Martin Luther King, Jr." The book was written by Doreen Rappaport and illustrated by Bryan Collier (Jump at the Sun, 2001. 40p. ISBN 0786807148). This pictorial biography of the world-renowned civil rights leader has one of the most striking…

  12. TRUMP3-JR: a finite difference computer program for nonlinear heat conduction problems

    International Nuclear Information System (INIS)

    Ikushima, Takeshi

    1984-02-01

    Computer program TRUMP3-JR is a revised version of TRUMP3 which is a finite difference computer program used for the solution of multi-dimensional nonlinear heat conduction problems. Pre- and post-processings for input data generation and graphical representations of calculation results of TRUMP3 are avaiable in TRUMP3-JR. The calculation equations, program descriptions and user's instruction are presented. A sample problem is described to demonstrate the use of the program. (author)

  13. STS-55 MS3 Harris draws blood sample from Payload Specialist Schlegel

    Science.gov (United States)

    1993-01-01

    STS-55 German Payload Specialist 2 Hans Schlegel (left) serves as a test subject inside the Spacelab Deutsche 2 (SL-D2) science module onboard the Earth-orbiting Columbia, Orbiter Vehicle (OV) 102. Mission Specialist 3 (MS3) Bernard A. Harris, Jr, a physician, performs one of many blood draws designed to help investigate human physiology under microgravity conditions. The two crewmembers use intravehicular activity (IVA) foot restraints (foot loops) in front of Rack 10, a stowage rack, to steady themselves during the procedure. Schlegel represents the German Aerospace Research Establishment (DLR).

  14. Finding the Right Formula: Edwin H. Walker Jr

    Science.gov (United States)

    Keels, Crystal L.

    2005-01-01

    Edwin H. Walker Jr earned his doctorate in chemistry at age 27 and has barely looked back. With 13 publications under his belt before coming out of graduate school, he has also given more than 20 poster presentations in national venues, most recently at the American Chemical Society. He can also include securing a half-million-dollar National…

  15. J.R. SIMPLOT EX-SITU BIOREMEDIATION TECHNOLOGY FOR TREATMENT OF DINOSEB-CONTAMINATED SOILS - INNOVATIVE TECHNOLOGY REPORT

    Science.gov (United States)

    This report summarizes the findings of an evaluation of the J.R. Simplot Ex-Situ Bioremediation Technology on the degradation of dinoseb (2-set-butyl-4,6-dinitrophenol) an agricultural herbicide. This technology was developed by the J.R. Simplot Company (Simplot) to biologically ...

  16. J.R. SIMPLOT EX-SITU BIOREMEDIATION TECHNOLOGY FOR TREATMENT OF TNT-CONTAMINATED SOILS - INNOVATIVE TECHNOLOGY EVALUATION REPORT

    Science.gov (United States)

    This report summarizes the findings of the second evaluation of the J.R. Simplot Ex-situ Bioremediation Technology also known as the Simplot Anaerobic Bioremediation (SABRE™) process. This technology was developed by the J.R. Simplot Company to biologically degrade nitroaromatic...

  17. La política exterior canadiense en el gobierno de Stephen Harper: entre la convicción y la polémica

    OpenAIRE

    Santín Peña, Oliver

    2015-01-01

    Resumen: Este trabajo revisa acontecimientos que han marcado la política exterior canadiense del gobierno del primer ministro Stephen Harper, explicando los orígenes y dinámicas que han posibilitado nuevos posicionamientos en la arena internacional al ir alejándose de postulados tradicionales que privilegiaban el multilateralismo y la protección del medio ambiente, lo cual ha generado polémicas y cuestionamientos al gobierno conservador de Ottawa, sobre todo a raíz de su salida del Protocolo ...

  18. Dynamic J-R Characteristics of RCS Pipe Materials for Ulchin Unit 3/4. (Evaluation of Dynamic Strain Aging Effects)

    Energy Technology Data Exchange (ETDEWEB)

    Hong, Jun Hwa; Lee, Bong Sang; Yoon, Ji Hyun; Oh, Jong Myung; Kim, Jin Won [Korea Atomic Energy Research Institute, Taejon (Korea, Republic of)

    1997-09-01

    5 materials (45 1T-CT specimens) were tested to evaluate dynamic J-R characteristics of RCS Pipe Materials for Ulchin Unit 3/4 (Evaluation of Dynamic Strain Aging Effects). The tests were performed by DCPD method at 316 deg C and 25 deg C. The loading rates were 1000mm/min and 2000mm/min. The objectives of this project were to obtain the dynamic J-R curves data of ferritic steels for application of LBB to the RCS pipes of Ulchin Unit 3/4. The test results showed that all of the tested dynamic J-R curves of 5 materials were above the lower bound curve of static J-R curve of pipe materials for Ulchin Unit 3/4. 10 refs., 4 tabs., 16 figs. (author)

  19. 75 FR 3839 - Martin Luther King, Jr., Federal Holiday, 2010

    Science.gov (United States)

    2010-01-22

    ... Part III The President Proclamation 8473--Martin Luther King, Jr., Federal Holiday, 2010 Proclamation 8474--Religious Freedom Day, 2010 Notice of January 20, 2010--Continuation of the National... only by the power of his words, which still call on us to perfect those sacred ideals enshrined in our...

  20. Aegla rosanae Campos Jr., um novo sinônimo de Aegla paulensis Schmitt (Crustacea, Aeglidae Aegla rosanae Campos Jr., a new synonym of Aegla paulensis Schmitt (Crustacea, Aeglidae

    Directory of Open Access Journals (Sweden)

    Georgina Bond-Buckup

    2000-06-01

    Full Text Available The validity of Aegla rosanae Campos Jr., 1998 as a new species was analysed. On the basis of comparisons with Aegla paulensis Schmitt, A. rosanae was considered its junior synonym.

  1. The quantum group, Harper equation and structure of Bloch eigenstates on a honeycomb lattice

    International Nuclear Information System (INIS)

    Eliashvili, M; Tsitsishvili, G; Japaridze, G I

    2012-01-01

    The tight-binding model of quantum particles on a honeycomb lattice is investigated in the presence of a homogeneous magnetic field. Provided the magnetic flux per unit hexagon is a rational of the elementary flux, the one-particle Hamiltonian is expressed in terms of the generators of the quantum group U q (sl 2 ). Employing the functional representation of the quantum group U q (sl 2 ), the Harper equation is rewritten as a system of two coupled functional equations in the complex plane. For the special values of quasi-momentum, the entangled system admits solutions in terms of polynomials. The system is shown to exhibit a certain symmetry allowing us to resolve the entanglement, and a basic single equation determining the eigenvalues and eigenstates (polynomials) is obtained. Equations specifying the locations of the roots of polynomials in the complex plane are found. Employing numerical analysis, the roots of polynomials corresponding to different eigenstates are solved and diagrams exhibiting the ordered structure of one-particle eigenstates are depicted. (paper)

  2. Evaluation of J-R curve testing of nuclear piping materials using the direct current potential drop technique

    International Nuclear Information System (INIS)

    Hackett, E.M.; Kirk, M.T.; Hays, R.A.

    1986-08-01

    A method is described for developing J-R curves for nuclear piping materials using the DC Potential Drop (DCPD) technique. Experimental calibration curves were developed for both three point bend and compact specimen geometries using ASTM A106 steel, a type 304 stainless steel and a high strength aluminum alloy. These curves were fit with a power law expression over the range of crack extension encountered during J-R curve tests (0.6 a/W to 0.8 a/W). The calibration curves were insensitive to both material and sidegrooving and depended solely on specimen geometry and lead attachment points. Crack initiation in J-R curve tests using DCPD was determined by a deviation from a linear region on a plot of COD vs. DCPD. The validity of this criterion for ASTM A106 steel was determined by a series of multispecimen tests that bracketed the initiation region. A statistical differential slope procedure for determination of the crack initiation point is presented and discussed. J-R curve tests were performed on ASTM A106 steel and type 304 stainless steel using both the elastic compliance and DCPD techniques to assess R-curve comparability. J-R curves determined using the two approaches were found to be in good agreement for ASTM A106 steel. The applicability of the DCPD technique to type 304 stainless steel and high rate loading of ferromagnetic materials is discussed. 15 refs., 33 figs

  3. Herbert L. Pick Jr. (1930-2012).

    Science.gov (United States)

    Rieser, John J; Lockman, Jeffrey J

    2013-01-01

    Presents an obituary for Herbert L. Pick Jr. For 49 years at the University of Minnesota's Institute of Child Development, new students were often greeted by an unassuming guy who rode to work on his bike, helped them carry boxes of books to their offices, and turned out to be a famous professor. Herbert L. Pick Jr. was a fabulous mentor, teacher, and developmental scientist. His work on perception and perceptual development spanned basic and applied science, laboratory and real-world settings. He was honored with the Division 7 (Developmental Psychology) Mentor Award from the American Psychological Association in 1998. He was honored again in 2002, jointly with his wife Anne D. Pick, with a volume of the Minnesota Symposium on Child Psychology based on a central theme of their work and titled "Action as an Organizer of Learning and Development." Two weeks before his death he was honored yet again with a Festschrift titled "Realism to Relevance: An Ecological Approach to Perception, Action and Cognition." Former students and academic admirers gave talks focused on the scientific themes Herb championed, namely, effects of experience on learning and development, organism-environment fit, environmental structure, and societal applications of research about basic psychological processes. He gave the final talk, and after thanking everyone in his typically humble way, he discussed his new research on visual-locomotor coordination. Herb died on June 18, 2012. He is greatly missed by Anne, his wife of 50 years; his sister Barbara; his daughters (and their husbands) Cindy (Jon), Karen (John), and Gretchen (Michael); and his grandchildren Alex, Ted, Katy, Joe, Eva, Sam, Rowan, and Culley. He is also missed by his many students, colleagues, friends, and admirers.

  4. Defense Science Board 2003 Summer Study on DoD Roles and Missions in Homeland Security. Volume 1

    Science.gov (United States)

    2003-11-01

    were used to develop a web-based "deployment picture." (A little money -a few million dollars-can go a long way in the combatant commands). OSD critical...AND MISSIONS f1 HOMELAND SECURJTY 91 APP8VD&XH Dr. Mark Harper U.S. Naval Academy Mr. Art Money Private Consultant Mr. Walter Morrow, Jr. MIT Lincoln...Protection BrigGen Irv Halter Discussion Mr. John Lauder Overview of NRO support to Homeland Security Mr. Brian Hack and Mr. Alan NRO Comms - NRO backbone

  5. Paleomagnetism of the Neoproterozoic Mount Harper Volcanic Complex, Canada

    Science.gov (United States)

    Eyster, A. E.; Macdonald, F. A.; O'Connell, R. J.

    2012-12-01

    Paleomagnetism can be used to identify apparent polar wander, which involves contributions from plate tectonics and true polar wander. True polar wander events have been suggested to have played an important role throughout Earth's history. The Neoproterozoic Mount Harper Volcanic Complex (MHVC) provides paleomagnetic data that bears on this issue. The MHVC is located in the southern Ogilvie Mountains in the Yukon Territory, on the north-west corner of the Laurentian craton. The MHVC involves up to 1200 m of basaltic and andesitic flows. The MHVC reflects the propagating rifting event involved in the breakup of the supercontinent Rodinia. The MHVC is well dated with an age of 717.43± 0.14Ma from the top (Macdonald et al., Science, 2010). Below the MHVC are alluvial fan conglomerate and sandstone from Proterozoic normal faulting. Above the MHVC is a glacial diamictite dated to 716.47± 0.24 Ma and related to Snowball Earth glaciation (Macdonald et al., Science, 2010). Both block and core samples were collected from different members of the MHVC for paleomagnetic study. Included in the sampling were several stratigraphic sections. Alternating field and thermal stepwise demagnetization methods were used to analyze specimens. Magnetic components were determined using principal component analysis and Fisher statistical procedures were used to calculate mean directions. The stratigraphically sampled basalt flows yielded two components. One was a common secondary overprint, and the other was a high stability component which yielded two different directions. One pole is the same as the accepted Neoproterozoic Laurentian grand mean pole and the other is ˜50 degrees away from this grand mean pole. Several possible interpretations are explored- tectonic rotation, true polar wander or the presence of a non-dipolar geomagnetic field.

  6. The application of DCPD method to evaluating dynamic J-R fracture resistance characteristics

    International Nuclear Information System (INIS)

    Yoon, Ji Hyun; Hong, Jun Hwa; Lee, Bong Sang; Chi, Se Whan; Kim, Joo Hag; Oh, Yong Jun; Kwun, Sun Chil; Oh, Jong Myung

    1999-06-01

    The reliable DCPD (Direct Current Potential Drop) test and data acquisition system were developed on the basis of analysis of various technical problems to accompanied with the application of DCPD method to J-R fracture resistance test. The test system contains electric insulation rod and high performance data acquisition system. The test and analysis method was applied to J-R fracture resistance test for SA516-Gr.70 steel for nuclear primary coolant system elbow. The reliabilities of test and analysis method were confirmed through the load-ratio method in case of dynamic loading test, and through the standard unloading compliance test in case of static loading test. (author). 17 refs., 1 tab., 18 figs

  7. The application of DCPD method to evaluating dynamic J-R fracture resistance characteristics

    Energy Technology Data Exchange (ETDEWEB)

    Yoon, Ji Hyun; Hong, Jun Hwa; Lee, Bong Sang; Chi, Se Whan; Kim, Joo Hag; Oh, Yong Jun; Kwun, Sun Chil; Oh, Jong Myung

    1999-06-01

    The reliable DCPD (Direct Current Potential Drop) test and data acquisition system were developed on the basis of analysis of various technical problems to accompanied with the application of DCPD method to J-R fracture resistance test. The test system contains electric insulation rod and high performance data acquisition system. The test and analysis method was applied to J-R fracture resistance test for SA516-Gr.70 steel for nuclear primary coolant system elbow. The reliabilities of test and analysis method were confirmed through the load-ratio method in case of dynamic loading test,and through the standard unloading compliance test in case of static loading test. (author). 17 refs., 1 tab., 18 figs.

  8. MILLS B. LANE, JR. AND ENTERPRISE IN A NEW SOUTH

    Directory of Open Access Journals (Sweden)

    Randall L. Patton

    2009-01-01

    Full Text Available For a century, Citizens & Southern Bank was a fixture in Georgia. In 1991, the C&S brand name disappeared in a merger with North Carolina National Bank. This was one of the bittersweet consequences of the slow, confusing swirl of bank deregulation after 1970, when institutions such as C&S simply disappeared, swallowed by the “winners” in the new competitive environment of interstate banking in the 1980s and 1990s. Even earlier, however, the Lane family had ceased to control the bank started by Mills Lane, Sr. in 1891. Mills B. Lane, Jr. was the last member of the Lane family to run C&S. After his retirement in 1973, Mills handpicked his successor and tried to retain some influence, but the bank began slipping away from the Lanes. By the early 80s, a decade before Hugh McColl’s NCNB acquired C&S, Mills Lane, Jr. was deeply alienated from the institution that had been, according to many, “Georgia’s cornerstone bank.”

  9. Writing, Teaching, and Researching: An Interview with Rene Saldana, Jr.

    Science.gov (United States)

    Saldana, Rene, Jr.; Moore, David W.

    2010-01-01

    Rene Saldana, Jr., an assistant professor at Texas Tech University, is a writer of short stories, poetry, and novels. In order to get his storytelling right, he has relied on his memory when writing memoirs and consulted popular culture and family when writing fiction. In order to get his university teaching right, he reads seminal texts on…

  10. Obituary: Edward W. Burke, Jr. (1924-2011)

    Science.gov (United States)

    Bloomer, Raymond, Jr.

    2011-12-01

    Dr. Edward W. Burke Jr. passed away on June 15, 2011, after suffering a heart attack. Dr. Burke devoted his professional life to the research and teaching of physics and astronomy at King College in Bristol, Tennessee. Edward W. Burke, Jr., was born in Macon, Georgia, on September 16, 1924. He was a Navy veteran, having been commissioned as an ensign in 1944. He served in the Pacific near the end of World War II. He proceeded to complete his undergraduate degree in mathematics from Presbyterian College in 1947 and pursued the M.S. and Ph.D. in physics (1949 and 1954, respectively) at the University of Wisconsin. Under the direction of Professor Julian Mack, his thesis was titled "Isotope Shift in the Spectra of Boron." Although he did research in atomic spectra in the early part of his career, his interest in astronomy and variable stars in particular were his primary interests during his long academic career. Dr. Burke began his illustrious career at King College in 1949. He initiated the astronomy program there in 1950, included constructing a 12.5 inch Newtonian telescope, homemade as was most everything in those days. Many of his students learned about photometry at the Burke Observatory on the college campus. Burke was known for his trips to the Kitt Peak and Lowell observatories accompanied by undergraduate students on his trips, all of which were made by automobile which he preferred over flying. His initial interest in Ap stars later broadened into variable and especially eclipsing binary stars. His motivation was maintained by his desire to have his students experience basic research and to spark their interest in advanced degrees. Numerous students achieved advanced science and medical degrees because of Burke's encouragement and mentoring. In 1959, Dr. Burke was awarded a Fulbright professorship and traveled to Chile where he taught physics for a year in the Engineering School at the University of Chile in Santiago. He worked to establish a physics

  11. Sensitivity of GC-EI/MS, GC-EI/MS/MS, LC-ESI/MS/MS, LC-Ag(+) CIS/MS/MS, and GC-ESI/MS/MS for analysis of anabolic steroids in doping control.

    Science.gov (United States)

    Cha, Eunju; Kim, Sohee; Kim, Ho Jun; Lee, Kang Mi; Kim, Ki Hun; Kwon, Oh-Seung; Lee, Jaeick

    2015-01-01

    This study compared the sensitivity of various separation and ionization methods, including gas chromatography with an electron ionization source (GC-EI), liquid chromatography with an electrospray ionization source (LC-ESI), and liquid chromatography with a silver ion coordination ion spray source (LC-Ag(+) CIS), coupled to a mass spectrometer (MS) for steroid analysis. Chromatographic conditions, mass spectrometric transitions, and ion source parameters were optimized. The majority of steroids in GC-EI/MS/MS and LC-Ag(+) CIS/MS/MS analysis showed higher sensitivities than those obtained with other analytical methods. The limits of detection (LODs) of 65 steroids by GC-EI/MS/MS, 68 steroids by LC-Ag(+) CIS/MS/MS, 56 steroids by GC-EI/MS, 54 steroids by LC-ESI/MS/MS, and 27 steroids by GC-ESI/MS/MS were below cut-off value of 2.0 ng/mL. LODs of steroids that formed protonated ions in LC-ESI/MS/MS analysis were all lower than the cut-off value. Several steroids such as unconjugated C3-hydroxyl with C17-hydroxyl structure showed higher sensitivities in GC-EI/MS/MS analysis relative to those obtained using the LC-based methods. The steroids containing 4, 9, 11-triene structures showed relatively poor sensitivities in GC-EI/MS and GC-ESI/MS/MS analysis. The results of this study provide information that may be useful for selecting suitable analytical methods for confirmatory analysis of steroids. Copyright © 2015 John Wiley & Sons, Ltd.

  12. Effects of solidified microstructures on J-R fracture resistances of the surge line pipe welds

    International Nuclear Information System (INIS)

    Youn, J. H.; Lee, B. S.; Yoo, W.

    2003-01-01

    The cause of the difference in J-R fracture resistances of AISI Type 347 GTAW welds which had almost same amounts of chromium carbides were investigated by the microstructural observations. As a result, the difference in the fracture resistances with the morphologies of the retained δ-ferrites in Type 347 welds were observed. The fracture resistance of the weld which had mostly vermicular type δ-ferrites was inferior to the weld which has lacy and acicular mixed type δ-ferrites. Therefore, it was deduced that the morphology of δ-ferrites affected the J-R fracture resistances of Type 347 welds

  13. Mounting a Curricular Revolution: An Interview with Henry Louis Gates, Jr.

    Science.gov (United States)

    von Zastrow, Claus

    2009-01-01

    This article presents an interview with Henry Louis Gates, Jr., Harvard professor and cultural critic who has captured 25 million viewers with his PBS documentary series, African American Lives (WNET). Using genealogical research and DNA science, Gates traces the family history of 19 famous African Americans. What results is a rich and moving…

  14. Constructing the ScratchJr Programming Language in the Early Childhood Classroom

    Science.gov (United States)

    Portelance, Dylan J.; Strawhacker, Amanda L.; Bers, Marina Umaschi

    2016-01-01

    This paper seeks to contribute to the growing literature on children and computer programming by focusing on a programming language for children in Kindergarten through second grade. Sixty-two students were exposed to a 6-week curriculum using ScartchJr. They learned foundational programming concepts and applied those concepts to create personally…

  15. Hip-Hop to Health Jr. for Latino preschool children.

    Science.gov (United States)

    Fitzgibbon, Marian L; Stolley, Melinda R; Schiffer, Linda; Van Horn, Linda; KauferChristoffel, Katherine; Dyer, Alan

    2006-09-01

    Hip-Hop to Health Jr. was a diet/physical activity intervention designed to reduce gains in BMI (kilograms per meter squared) in preschool minority children. Twelve predominantly Latino Head Start centers participated in a group-randomized trial conducted between Fall 2001 and Winter 2003. Six centers were randomized to a culturally proficient 14-week (three times weekly) diet/physical activity intervention. Parents participated by completing weekly homework assignments. The children in the other six centers received a general health intervention that did not address either diet or physical activity. The primary outcome was change in BMI, and secondary outcomes were changes in dietary intake and physical activity. Measures were collected at baseline, post-intervention, and at Years 1 and 2 follow-up. There were no significant differences between intervention and control schools in either primary or secondary outcomes at post-intervention, Year 1, or Year 2 follow-ups. When Hip-Hop to Health Jr. was conducted in predominantly black Head Start centers, it was effective in reducing subsequent increases in BMI in preschool children. In contrast, when the program was conducted in Latino centers, it was not effective. Although the intervention did not prevent excessive weight gain in Latino children, it was very well received. Future interventions with this population may require further cultural tailoring and a more robust parent intervention.

  16. ANALYSIS OF TRANSLATION METHODS ON HARPER LEE‟S NOVEL TO KILL A MOCKINGBIRD FROM ENGLISH INTO INDONESIAN

    Directory of Open Access Journals (Sweden)

    Rudi Hartono

    2017-04-01

    Full Text Available The goal of this research was to analyze the translation methods used in translating Harper Lee‘s Novel entitled To Kill a Mockingbird (TKM from English into Indonesian. The research method used was Descriptive Qualitative Research. This study analyzed 47 idioms, 25 metaphors, and 42 personifications. The research instrument used was translation data of idioms, metaphors, and personifications taken from the novel. The data collection technique was collecting and tabulating the data from the novel. The data analysis technique used is Interactive Model (Miles and Huberman, 1984. Based on the research it is shown that the translation methods used in translating the idioms are wordfor- word (21%, literal (36,2%, semantic (2,1%, free (12,8%, and 46,8%, used in translating the metaphors are literal (80%, semantic (4%, and free (16%, while used in translating the personifications are literal (88%, faithful (4,8%, semantic (4,8%, and communicative (2,4%.

  17. Spectral relationships between kicked Harper and on-resonance double kicked rotor operators

    International Nuclear Information System (INIS)

    Lawton, Wayne; Mouritzen, Anders S.; Wang Jiao; Gong Jiangbin

    2009-01-01

    Kicked Harper operators and on-resonance double kicked rotor operators model quantum systems whose semiclassical limits exhibit chaotic dynamics. Recent computational studies indicate a striking resemblance between the spectra of these operators. In this paper we apply C*-algebra methods to explain this resemblance. We show that each pair of corresponding operators belongs to a common rotation C*-algebra B α , prove that their spectra are equal if α is irrational, and prove that the Hausdorff distance between their spectra converges to zero as q increases if α=p/q with p and q coprime integers. Moreover, we show that corresponding operators in B α are homomorphic images of mother operators in the universal rotation C*-algebra A α that are unitarily equivalent and hence have identical spectra. These results extend analogous results for almost Mathieu operators. We also utilize the C*-algebraic framework to develop efficient algorithms to compute the spectra of these mother operators for rational α and present preliminary numerical results that support the conjecture that their spectra are Cantor sets if α is irrational. This conjecture for almost Mathieu operators, called the ten Martini problem, was recently proven after intensive efforts over several decades. This proof for the almost Mathieu operators utilized transfer matrix methods, which do not exist for the kicked operators. We outline a strategy, based on a special property of loop groups of semisimple Lie groups, to prove this conjecture for the kicked operators

  18. A quality approach to maintain the properties of S235 JR structural carbon steel in Lebanon

    International Nuclear Information System (INIS)

    Sidawi, J.A.; Al Khatib, H.

    2004-01-01

    Full text.S235JR carbon steel is one of the most popular steels used in Lebanon. It is imported by steel dealers and is widely used by all fabricators and manufacturers of steels for many structural purposes and applications. This kind of steel has good ductile properties as well as excellent weldability. It is still known by its previous designation St 37-2 or E 24-2. S235JR is produced in many shapes and thicknesses such as steel plates, sheets, angles and different other geometric shapes. Standard chemical and mechanical tests were conducted and reported on S235JR hot-rolled structural low-carbon mild steel specimens collected from Lebanese steel market. The main objective of this work is to assure the compliance of these properties with those set by the steel manufacturer. The above mentioned tests were performed at the laboratories of the Industrial Research Institute (IR) in Lebanon to assure the quality and credibility of the results. related European and American standards were presented as references and compared with the achieved results. Discussion was presented to show the similarities and differences between S235JR steel samples and standard requirements. Some of the reasons for such differences were discussed. Sufficient data was furnished through this work for the public and mainly for the Lebanese Standard Organization LIBNOR to easily adopt and implement the EN 10025:1993 European standard that can be applied in Lebanon concerning the most commonly used hot rolled low carbon structural steel. A follow up concerning adopting and implementing EN 10025:1993 will be briefed

  19. 77 FR 6825 - NASA Advisory Council; Information Technology Infrastructure Committee; Meeting.

    Science.gov (United States)

    2012-02-09

    ...; Information Technology Infrastructure Committee; Meeting. AGENCY: National Aeronautics and Space... Information Technology Infrastructure Committee of the NASA Advisory Council. DATES: Wednesday, March 7, 2012... CONTACT: Ms. Karen Harper, Executive Secretary for the Information Technology Infrastructure Committee...

  20. The somatostatin receptor 2 antagonist 64Cu-NODAGA-JR11 outperforms 64Cu-DOTA-TATE in a mouse xenograft model

    Science.gov (United States)

    Rylova, Svetlana N.; Stoykow, Christian; Del Pozzo, Luigi; Abiraj, Keelara; Tamma, Maria Luisa; Kiefer, Yvonne; Fani, Melpomeni; Maecke, Helmut R.

    2018-01-01

    Copper-64 is an attractive radionuclide for PET imaging and is frequently used in clinical applications. The aim of this study was to perform a side-by-side comparison of the in vitro and in vivo performance of 64Cu-NODAGA-JR11 (NODAGA = 1,4,7-triazacyclononane,1-glutaric acid,4,7-acetic acid, JR11 = p-Cl-Phe-cyclo(D-Cys-Aph(Hor)-D-Aph(cbm)-Lys-Thr-Cys)D-Tyr-NH2), a somatostatin receptor 2 antagonist, with the clinically used sst2 agonist 64Cu-DOTA-TATE ((TATE = D-Phe-cyclo(Cys-Tyr-D-Trp-Lys-Thr-Cys)Thr). In vitro studies demonstrated Kd values of 5.7±0.95 nM (Bmax = 4.1±0.18 nM) for the antagonist 64/natCu-NODAGA-JR11 and 20.1±4.4. nM (Bmax = 0.48±0.18 nM) for the agonist 64/natCu-DOTA-TATE. Cell uptake studies showed the expected differences between agonists and antagonists. Whereas 64Cu-DOTA-TATE (the agonist) showed very effective internalization in the cell culture assay (with 50% internalized at 4 hours post-peptide addition under the given experimental conditions), 64Cu-NODAGA-JR11 (the antagonist) showed little internalization but strong receptor-mediated uptake at the cell membrane. Biodistribution studies of 64Cu-NODAGA-JR11 showed rapid blood clearance and tumor uptake with increasing tumor-to-relevant organ ratios within the first 4 hours and in some cases, 24 hours, respectively. The tumor washout was slow or non-existent in the first 4 hours, whereas the kidney washout was very efficient, leading to high and increasing tumor-to-kidney ratios over time. Specificity of tumor uptake was proven by co-injection of high excess of non-radiolabeled peptide, which led to >80% tumor blocking. 64Cu-DOTA-TATE showed less favorable pharmacokinetics, with the exception of lower kidney uptake. Blood clearance was distinctly slower and persistent higher blood values were found at 24 hours. Uptake in the liver and lung was relatively high and also persistent. The tumor uptake was specific and similar to that of 64Cu-NODAGA-JR11 at 1 h, but release from the tumor

  1. Isolation and Fermentation of Lactobacillus plantarum JR64 as an Omega 6 Probiotic Producer

    Directory of Open Access Journals (Sweden)

    Lanjar Sumarno

    2011-12-01

    Full Text Available Application of lactic acid probiotic bacteria in health food diversification currently is progressing rapidly.  It is encouraged the study of searching the potential strains from local resources (Ponorogo Residence namely noni fruits (badeg pace and noni wine.  Aims of this study were to perform the isolation, identification, and production of  probiotic Lactobacillus sp. JR64 fermentation process as a producer of Omega-6 (ω-6 lowering cholesterol and design of probiotic creamy product.   Beginning stages of research was strains isolating and in-vitro testing, the best result were used in  molecular  identification technology development for the production of metabolites through the manipulation of environmental variation  of glucose 20 g / l, 30 g / l and 40 g / l that influenced the substrate concentration of linoleic acid productivity. The result of new isolates isolation showed that isolates that obtained from noni wine, Lactobacillus plantarum JR64, was potential as probiotic condidate.   The effieciency of fermentation  substrates using  Yx/s and Yp /s  in the exponential phase was the highest value for the fermentation of 24 hours of  Yx/ s; 17.03% and Y p/s; 74.72%, while the results of design and the best formulation for viability cells of lactobacillus  plantarum probiotics JR64 was composed of 15 g and 50g butter 15 g icing sugar as well as during storage of the refrigerant temperature was 8.92 x 108 CFU / ml.  [Key Words : Omega-6,  Lactobacillus plantarum JR64, fermentation

  2. Hermeneutic Haunting: E. D. Hirsch, Jr. and the Ghost of Interpretive Validity

    Science.gov (United States)

    O'Neill, Linda

    2011-01-01

    This article applies criteria for validity in interpretation to Eric Donald Hirsch, Jr.'s interpretations of John Dewey. Specifically, three criteria that Hirsch, himself, established in his earlier work are used to evaluate Hirsch's interpretation of John Dewey as a member of a class (romantics) who embraced a naive naturalism (trait) more often…

  3. LANSCE '90: the Manuel Lujan Jr. Neutron Scattering Center

    International Nuclear Information System (INIS)

    Pynn, Roger

    1991-01-01

    This paper describes progress that has been made at the Manuel Lujan Jr. Neutron Scattering Center (LANSCE) during the past two years. Presently, LANSCE provides a higher peak neutron flux than any other pulsed spallation neutron source. There are seven spectrometers for neutron scattering experiments that are operated for a national user program sponsored by the U.S. Department of Energy. Two more spectrometers are under construction. Plans have been made to raise the number of beam holes available for instrumentation and to improve the efficiency of the target/moderator system. (author)

  4. LANSCE '90: The Manuel Lujan Jr. Neutron Scattering Center

    International Nuclear Information System (INIS)

    Pynn, R.

    1990-01-01

    This paper describes progress that has been made at the Manuel Lujan Jr. Neutron Scattering Center (LANSCE) during the past two years. Presently, LANSCE provides a higher peak neutron flux than any other pulsed spallation neutron source. There are seven spectrometers for neutron scattering experiments that are operated for a national user program sponsored by the US Department of Energy. Two more spectrometers are under construction. Plans have been made to raise the number of beam holes available for instrumentation and to improve the efficiency of the target/moderator system. 9 refs., 4 figs

  5. Gino Marinuzzi Jr : electronics and early multimedia mentality in Italy

    OpenAIRE

    Corbella, M.

    2015-01-01

    In this essay I reassess the complexity of the convergence between electronic music and media practices in Rome in the 1950s and 1960s, through the reconstruction of the experience of composer Gino Marinuzzi Jr (1920-96). His engagement with technology as a structuring device of compositional processes is fundamental and inescapable, and brings to the fore crucial issues of ‘applied’ music’s troublesome reputation in the Italian cultural discourse. In reviewing Marinuzzi’s biography over the ...

  6. O Vigia de O Sol é Para Todos: representações do racismo e das relações raciais sulistas na obra de Harper Lee

    OpenAIRE

    Goulart, Henrique Rodrigues de Paula

    2017-01-01

    O presente trabalho dedica-se a uma leitura crítica de O Sol é Para Todos, célebre romance publicado em 1960 pela escritora norte-americana Harper Lee e adaptado para o cinema em 1962. A  proposta consiste em compreender as representações históricas produzidas pelas obras – literária e fílmica – acerca dos embates raciais atravessados pelo Sul dos Estados Unidos no contexto do Movimento pelos Direitos Civis. Por último, pretende-se comparar tais representações às de Vá, Coloque um Vigia, vers...

  7. Sharing the Gift of Jazz: An Interview with Willie L. Hill Jr.

    Science.gov (United States)

    Howe, Brad

    2011-01-01

    This article presents an interview with Willie L. Hill Jr., founder and director of the Society for Jazz Education. Currently a professor of music education at the University of Massachusetts-Amherst and the director of the UMass Fine Arts Center, Hill has served as director of education for the Thelonious Monk Institute of Jazz. He is a past…

  8. 75 FR 53861 - Airworthiness Directives; Robert E. Rust, Jr. Model DeHavilland DH.C1 Chipmunk 21, DH.C1 Chipmunk...

    Science.gov (United States)

    2010-09-02

    ... Airworthiness Directives; Robert E. Rust, Jr. Model DeHavilland DH.C1 Chipmunk 21, DH.C1 Chipmunk 22, and DH.C1...). ACTION: Final rule. SUMMARY: We are adopting a new airworthiness directive (AD) for all Robert E. Rust... CFR part 39) to include an AD that would apply to all Robert E. Rust, Jr. Models DeHavilland DH.C1...

  9. Martin Luther King, Jr., General Hospital and community involvement.

    Science.gov (United States)

    Humphrey, M M

    1973-07-01

    Community involvement is not just one facet of the new Martin Luther King, Jr., General Hospital's existence. It is the mainstream from which all other activities flow. In addition to meeting the conventional needs of a conventional hospital staff with the core collection of texts and journals, this library goes one step further. It acts as a resource for its community health workers, dietitians, and nurses in their various outreach programs. It serves as a stimulus for the high school or community college student who may be curious about a health career. It also finds time to provide reading material for its patients.

  10. The Harper Government's New Right Neoliberal Agenda and the Dismantling of Status of Women Canada and the Family Violence Initiative

    Directory of Open Access Journals (Sweden)

    Ruth M Mann

    2016-06-01

    Full Text Available This paper situates the Harper government’s 2006 restructuring and effective dismantling of Status of Women Canada and its 2011 take down of the approximate 12,000 volume online library of the federal Family Violence Initiative in relation to two developments. These are the ascendant influence of men’s rights and other antifeminist activism in Canada and globally; and the concurrent rise of a Hayekian-animated New Right neoliberal agenda intent on subordinating civil society and democratic rule to the forces of twenty-first century global capitalism. The paper contends that anti-feminism is among a host of neoconservative forces that the New Right instrumentalizes to augment and advance and its neoliberal agenda. For the New Right, however, the enemy is not gender equality or feminism per se but rather the market inhibiting commitment to social justice that feminism participates in and advances.

  11. Martin Luther King, Jr.: A Lesson with Interdisciplinary Connections for Middle-Level Music Students.

    Science.gov (United States)

    Early, Mary Frances; Terry, Cynthia

    This lesson begins with a very brief biography of Martin Luther King, Jr. The lesson identifies its educational objectives; addresses National Standards for Music Education; lists materials needed; details six step-by-step classroom procedures for lesson implementation; and provides curriculum connections for language arts, visual art, physical…

  12. Comparative assessment of cyclic J-R curve determination by different methods in a pressure vessel steel

    Energy Technology Data Exchange (ETDEWEB)

    Chowdhury, Tamshuk, E-mail: tamshuk@gmail.com [Deep Sea Technologies, National Institute of Ocean Technology, Chennai, 600100 (India); Sivaprasad, S.; Bar, H.N.; Tarafder, S. [Fatigue & Fracture Group, Materials Science and Technology Division, CSIR-National Metallurgical Laboratory, Jamshedpur, 831007 (India); Bandyopadhyay, N.R. [School of Materials Science and Engineering, Indian Institute of Engineering, Science and Technology, Shibpur, Howrah, 711103 (India)

    2016-04-15

    Cyclic J-R behaviour of a reactor pressure vessel steel using different methods available in literature has been examined to identify the best suitable method for cyclic fracture problems. Crack opening point was determined by moving average method. The η factor was experimentally determined for cyclic loading conditions and found to be similar to that of ASTM value. Analyses showed that adopting a procedure analogous to the ASTM standard for monotonic fracture is reasonable for cyclic fracture problems, and makes the comparison to monotonic fracture results straightforward. - Highlights: • Different methods of cyclic J-R evaluation compared. • A moving average method for closure point proposed. • η factor for cyclic J experimentally validated. • Method 1 is easier, provides a lower bound and direct comparison to monotonic fracture.

  13. Walter Rowe Courtenay, Jr. (1933–2014)

    Science.gov (United States)

    Benson, Amy J.

    2016-01-01

    WALTER R. COURTENAY, JR., ichthyologist and retired professor, Florida Atlantic University, Boca Raton, Florida, died in Gainesville, Florida, on 30 January 2014 at age 80. Walt was born in Neenah, Wisconsin, on 6 November 1933, son of Walter and Emily Courtenay. Walt's interest in fish began at a young age as evidenced by a childhood diary in which at 13 years of age he wrote about his first catch—a two-and-a-half pound “pike” from Lake Winnebago. When Walt turned ten, the family moved from Wisconsin to Nashville, Tennessee, the move precipitated by his father accepting a position as pastor of the First Presbyterian Church. During those early days in Nashville, Walt's father would take summers off and travel to Michigan to teach at Camp Miniwanca along the shore of Lake Michigan where father and son honed their angling skills. It was also at that time Walt's father had definite views on what his son should be doing in adult life—in Walt's case it was to become a medical doctor. However, his Woods Hole internship in marine biology and oceanography toward the end of his undergraduate years was a transformative experience for him so much so that he abandoned all ideas of becoming a medical doctor and instead specialized in ichthyology and oceanography. Apart from the inherent interest and opportunities Woods Hole opened to him, being back at the shore of a large body of water, in this case the Atlantic Ocean, was far more interesting than sitting in lectures on organic chemistry. With that, Walt completed his B.A. degree at Vanderbilt University in 1956. In 1960 while in graduate school in Miami, Walt met and married Francine Saporito, and over the next several years had two children, Walter III and Catherine. He went on to receive his M.S. in 1961 from The Rosenstiel School of Marine and Atmospheric Science at the University of Miami on the systematics of the genus Haemulon (grunts) and his Ph.D. degree in 1965 working under his advisor C. Richard

  14. Cicero's de legibus and Martin Luther King, Jr.’s Stride toward freedom

    Directory of Open Access Journals (Sweden)

    Boleslav s. Povšič

    1979-12-01

    Full Text Available He who reads carefully Cicero'sDe Legibus and Martin Luther King, Jr.'s Stride Toward Freedom is surprised to find, mutatis mutandis, on how many points these two great men agree. The historical circumstances are different, but the essential ideas are very similar. The purpose of this paper is to show on what precisely they agree and on what they differ.

  15. Has the Dream Been Fulfilled? Dr. Martin Luther King, Jr. & President Barack Hussein Obama

    Science.gov (United States)

    Robinson, Nichelle Boyd; Moore, Virginia J.; Williams-Black, Thea H.

    2015-01-01

    Equality for all was the dream of Dr. Martin Luther King, Jr. and he knowingly laid the foundation for and inspired the first African-American President of the United States of America, Barack Hussein Obama, who also had the dream of "Change" for America. These men exhibited how working together can make dreams become reality. For the…

  16. A Long View of the Literary Debate: E. D. Hirsch Jr. and His Forebears.

    Science.gov (United States)

    Reynolds, Richard J.

    An immediate best seller when it was published in 1987, E. D. Hirsch, Jr.'s "Cultural Literacy: What Every American Needs To Know" galvanized legions on both sides of the sociopolitical aisle that divides education. The book has become a revered text regularly referenced by those scholars who take up a position that may be loosely…

  17. Success as Failure and Failure as Success: The Cultural Literacy of E. D. Hirsch, Jr.

    Science.gov (United States)

    Sledd, Andrew E.; Sledd, James H.

    1989-01-01

    Examines the logic and rhetoric of E. D. Hirsch, Jr., in "Cultural Literacy." Attempts to answer the question of how intellectual failure guarantees success in the marketplace. Concludes with an alternative vision of the American society that Hirsch describes and the suggestion that Hirsch's cultural literacy is cross-cultural…

  18. Final Environmental Statement and Supplemental Information for Aquilla Lake, Aquilla Creek, Hill County, Texas.

    Science.gov (United States)

    1976-04-13

    P. Gregory Mr. Joe Yelderman, Jr. B. M. and Jan J. Jean Mr. James W. Wight Ms. Mary Ann Sulak Johnson County Rural Water Supply J. R. Joplin Mr. Loyd...Gregory Mr. Joe Yelderman, Jr. B. M. and Jan J. Jean Mr. James W. Wight Ms. Mary Ann Sulak Johnson County Rural Water Supply J. R. Joplin Mr. Loyd S

  19. Astronaut Curtis L. Brown, Jr., pilot, works with his life raft during emergency bailout training

    Science.gov (United States)

    1996-01-01

    STS-77 TRAINING VIEW --- Astronaut Curtis L. Brown, Jr., pilot, works with his life raft during emergency bailout training for crew members in the Johnson Space Centers (JSC) Weightless Environment Training Facility (WET-F). Brown will join five other astronauts for nine days aboard the Space Shuttle Endeavour next month.

  20. The United States Army Medical Department Journal. July-September 2010

    Science.gov (United States)

    2010-09-01

    wide range of dedicated healthcare professionals who collaborate time and again to advance the state-of-the- art of care for our Warriors who...2010. 5. Bsisu MS. The Arab Table. New York, NY: HarperCollins; 2005. 6. Zubaida S, Tapper R, eds. A Taste of Thyme: Culinary Cultures of the

  1. 76 FR 71048 - Sixth Annual Philip S. Chen, Jr. Distinguished Lecture on Innovation and Technology Transfer

    Science.gov (United States)

    2011-11-16

    ... present ``Treatment of Cancer with Recombinant Immunotoxins: From Technology Transfer to the Patient.'' Dr. Pastan is an NIH Distinguished Investigator and Chief, Laboratory of Molecular Biology, National Cancer Institute Center for Cancer Research. This annual series honors Dr. Philip S. Chen, Jr. for his almost 50...

  2. Analysis of phytochemical variations in dioecious Tinospora cordifolia stems using HPLC/QTOF MS/MS and UPLC/QqQLIT -MS/MS.

    Science.gov (United States)

    Bajpai, Vikas; Singh, Awantika; Chandra, Preeti; Negi, M P S; Kumar, Nikhil; Kumar, Brijesh

    2016-01-01

    The stem of dioecious Tinospora cordifolia (Menispermaceae) is a commonly used traditional Ayurvedic medicine in India having several therapeutic properties. To develop and validate LC-MS methods for the identification and simultaneous quantitation of various secondary metabolites and to study metabolomic variations in the stem of male and female plants. Ethanolic extract of stems were analysed by HPLC/ESI-QTOF-MS/MS for rapid screening of bioactive phytochemicals. High resolution MS and MS/MS in positive ESI mode were used for structural investigation of secondary metabolites. An UPLC/ESI-QqQ(LIT) -MS/MS method in MRM mode was developed and validated for the simultaneous quantitation of five bioactive alkaloids. Identification and characterisation of 36 metabolites including alkaloids, sesquiterpenes and phytoecdysteroids were performed using LC-MS and MS/MS techniques. The bioactive alkaloids such as jatrorrhizine, magnoflorine, isocorydine, palmatine and tetrahydropalmatine were successfully quantified in male and female plants. The mean abundances of magnoflorine jatrorrhizine, and oblongine were significantly (P Phytochemicals in the stem of male and female Tinospora cordifolia showed significant qualitative and quantitative variations. LC-MS and MS/MS methods can be used to differentiate between male and female plants based on their chemical profiles and quantities of the marker bioactive alkaloids. This chemical composition difference was also evident during vegetative stage when there were no male and female flowers. Copyright © 2015 John Wiley & Sons, Ltd.

  3. Determination of Glyphosate Levels in Breast Milk Samples from Germany by LC-MS/MS and GC-MS/MS

    NARCIS (Netherlands)

    Steinborn, Angelika; Alder, Lutz; Michalski, Britta; Zomer, Paul; Bendig, Paul; Martinez, Sandra Aleson; Mol, Hans G.J.; Class, Thomas J.; Costa Pinheiro, Nathalie

    2016-01-01

    This study describes the validation and application of two independent analytical methods for the determination of glyphosate in breast milk. They are based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS), respectively. For

  4. 77 FR 14355 - Notice of Availability of Final Environmental Impact Statement for a Proposed Highway Between I...

    Science.gov (United States)

    2012-03-09

    ...: James A. Barlow, JR., Ph.D., Regulatory Branch, phone (504) 862-2250 or email at james.a.barlow@usace... schedule an appointment please contact either James A. Barlow, JR., phone (504) 862-2250 or Ms. Brenda...

  5. Finding of pesticides in fashionable fruit juices by LC-MS/MS and GC-MS/MS.

    Science.gov (United States)

    Tran, Kevin; Eide, David; Nickols, Susan M; Cromer, Michele R; Sabaa-Srur, Armando; Smith, Robert E

    2012-10-15

    Products labelled as containing extracts from two mushrooms (cordyceps plus reishi) and the juices from açaí, goji, mangosteen, noni, pomegranate, and sea buckthorn have been analysed for 174 different pesticides, using the validated QuEChERS method for sample preparation and electrospray LC-MS/MS in the positive ion mode for analysis. Pesticides were found in 10 of the 21 samples analysed. Most pesticides found were below the tolerance levels (1-6 μg/g, depending on the pesticide), but some were not. This included boscalid, dimethomorph, iprovalicarb, pyridaben, pyrimethanil, and imazalil, for which there is no tolerance reported or zero tolerance in any fruit. However, genuine açaí that was harvested in the state of Pará and lyophilised in Rio de Janeiro had no detectable pesticides, when analysed by both LC-MS/MS and GC-MS/MS, which can detect 213 more pesticides and industrial chemicals. Likewise no pesticides were found in one sample each of cordyceps plus reishi, sea buckthorn and noni. Published by Elsevier Ltd.

  6. Evaluation of low-cost commercial-off-the-shelf autopilot systems for SUAS operations

    Science.gov (United States)

    Brown, Calvin Thomas

    With this increase in unmanned aircraft system (UAS) operations, there is a need for a structured process to evaluate different commercially available systems, particularly autopilots. The Remotely Operated Aircraft Management, Interpretation, and Navigation from Ground or ROAMING scale was developed to meet this need. This scale is a modification of the widely accepted Handling Qualities Rating scale developed by George Cooper and Robert Harper Jr. The Cooper-Harper scale allows pilots to rate a vehicle's performance in completing some task. Similarly, the ROAMING scale allows UAS operators to evaluate the management and observability of UAS in completing some task. The standardized evaluative process consists of cost, size, weight, and power (SWAP) analysis, ease of implementation through procedural description of setup, ROAMING scale rating, a slightly modified NASA TLX rating, and comparison of manual operation to autonomous operation of the task. This standard for evaluation of autopilots and their software will lead to better understanding of the workload placed on UAS operators and indicate where improvements to design and operational procedures can be made. An assortment of low-cost commercial-off-the-shelf (COTS) autopilots were selected for use in the development of the evaluation and results of these tests demonstrate the commonalities and differences in these systems.

  7. Pediatric MS

    Science.gov (United States)

    ... Pediatric MS Share this page Facebook Twitter Email Pediatric MS Pediatric MS Pediatric MS Support Pediatric Providers ... system through the Pediatric MS Support Group . Treating pediatric MS In 2018 the U.S. Food and Drug ...

  8. The leadership principles of Dr. Martin Luther King, Jr. and their relevance to surgery.

    Science.gov (United States)

    Brunicardi, F Charles; Cotton, Ronald T; Cole, George W; Martinez, George

    2007-01-01

    In order to face the challenges in healthcare this century, it is essential that surgeons understand modern leadership principles. One of the greatest leaders in history was Dr. Martin Luther King, Jr., who provides a shining example of level-5 leadership for us to study. The study of leadership principles of great leaders can provide us with practical methods of conflict resolution as well as inspiration to keep us engaged and focused. As leaders of the medical community, we face numerous challenges, including discovering and implementing new treatments for disease, providing care for the indigent, overcoming educational challenges such as incorporating the ACGME Core Competencies into our surgical training and promoting diversity in education. Achieving these goals is often hindered by the environment in which we labor-nearly 50 million are uninsured, the rising cost of medical care is currently at 16% of the GNP, and reimbursement rates are falling-which makes the practice of surgery a significant challenge. Effective leadership will be paramount in achieving these goals. In this editorial, which summarizes a presentation given to the Surgical Section of the annual National Medical Association meeting, five important leadership principles that are important for surgeons have been selected and related to the outstanding leadership of Dr. Martin Luther King, Jr.

  9. 75 FR 16513 - B&C Corporation, JR Engineering Division, Including B&C Distribution Center, Including On-Site...

    Science.gov (United States)

    2010-04-01

    ... Engineering Division, Including B&C Distribution Center, Including On-Site Leased Workers From B&C Services... occurred during the relevant time period at the B&C Distribution Center, Inc. of the B&C Corporation, JR Engineering Division, Barberton, Ohio. The B&C Distribution Center provides distribution and logistical...

  10. Pragmatic Analyses of Martin Luther King (Jr)'s Speech: "I Have a Dream"--An Introspective Prognosis

    Science.gov (United States)

    Josiah, Ubong E.; Oghenerho, Gift

    2015-01-01

    This paper investigates the speech of Martin Luther King (Jr.) titled: "I Have a Dream", presented in 1963 at the Lincoln Memorial. This speech is selected for use because it involves a speaker and an audience who belong to a particular speech community. The speech is about the failed promises by the Americans whose dream advocate…

  11. The use of acetonitrile as the sole nitrogen and carbon source by Geotrichum sp. JR1 Uso de acetonitrila como única fonte de carbono e nitrogênio por Geotrichum sp. JR1

    Directory of Open Access Journals (Sweden)

    Rachel Passos Rezende

    2004-06-01

    Full Text Available A yeast strain identified as Geotrichum sp. JR1 was able to use acetonitrile as the sole carbon and nitrogen source. The strain grew in 0.5 to 2M acetonitrile. Ammonia generation as enzymatic product during the strain growth indicates the presence of an acetonitrile degrading enzyme. Acetic acid and acetamide were detected during assays with the resting cells cultivated in acetonitrile, indicating the presence of nitrile and amide degrading enzymes. This paper is the first to describe the use of acetonitrile as the sole carbon and nitrogen source by a yeast.Uma linhagem de levedura identificada como Geotrichum sp. JR1 foi capaz de utilizar acetonitrila, em concentrações de 0,5 a 2M, como única fonte de carbono e de nitrogênio. A geração de amônia durante o crescimento do microrganismo indica a presença de sistema enzimático capaz de degradar acetonitrila. Durante os ensaios enzimáticos, com células cultivadas em acetonitrila, foram detectados ácido acético e acetamida como produtos indicando a presença de sistema enzimático capaz de degradar acetonitrila e acetamida. Este trabalho é o primeiro a descrever a utilização de acetonitrila como única fonte de carbono e de nitrogênio por uma levedura.

  12. Study, Stance, and Stamina in the Research on Teachers' Lives: A Rejoinder to Robert V. Bullough, Jr.

    Science.gov (United States)

    Kelchtermans, Geert

    2008-01-01

    Robert V. Bullough, Jr.'s article demonstrated in an impressive way how autobiographical accounts, as well as single person narratives, are intertwined with much larger issues in society, international politics, and economical interests, as well as consequences for people in general and educators in particular. The way he proves capable of…

  13. The Limits of Master Narratives in History Textbooks: An Analysis of Representations of Martin Luther King, Jr.

    Science.gov (United States)

    Alridge, Derrick P.

    2006-01-01

    In this study, I argue that American history textbooks present discrete, heroic, one-dimensional, and neatly packaged master narratives that deny students a complex, realistic, and rich understanding of people and events in American history. In making this argument, I examine the master narratives of Martin Luther King, Jr., in high school history…

  14. A expansão e a eficiência da escola rural em São Paulo: atuação e posicionamentos de Almeida Jr. a partir de estatísticas oficiais - The expansion and the efficiency of the rural school in São Paulo: the performance and the thinking of Almeida Jr. based o

    Directory of Open Access Journals (Sweden)

    Luciana Maria Viviani

    2011-07-01

    Full Text Available O objetivo deste estudo é analisar os discursos produzidos por Almeida Jr. sobre o ensino rural, entre as décadas de 1930 e 1940, e as formas sob as quais ele utilizou dados estatísticos para sustentar as suas opiniões e a sua atuação como administrador do ensino paulista. O estudo dessas questões pretende colaborar na ampliação do entendimento acerca das propostas para o ensino rural, tema bastante debatido nesse período. Por meio da análise de publicações oficiais paulistas e de artigos da Revista Brasileira de Estudos Pedagógicos, verificou-se que Almeida Jr., médico e educador ligado ao grupo dos chamados renovadores do ensino, defendia propostas voltadas para a qualidade do ensino e para a organização de uma escola básica comum, ainda que adaptada ao meio rural.Palavras-chave: educação rural, estatísticas educacionais, intelectuais da educação. THE EXPANSION AND THE EFFICIENCY OF THE RURAL SCHOOL IN SÃO PAULO: THE PERFORMANCE AND THE THINKING OF ALMEIDA JR. BASED ON OFFICIAL STATISTICSAbstractThe objective of this paper is to analyze de speeches made by Almeida Jr. about the rural education, between the decades of 1930 and 1940, and the way under which he used the statistics data to sustain his opinions and his performance as the manager of education in São Paulo. By analyzing the São Paulo’s official publications and the articles published in the Revista Brasileira de Estudos Pedagógicos, it has been found that Almeida Jr., a doctor and an educator connected to the group composed by some men who were called the renewers of education, sustained proposals which were bent to the good quality of education and to the organization of a unique elementary school, though to fit the country environment.Key-words: rural education, educational statistics, intellectuals in education. LA EXPANSIÓN Y LA EFICIENCIA DE LA ESCUELA RURAL EN SAN PABLO: ACTUACIÓN Y OPINIONES DE ALMEIDA JR. A PARTIR DE ESTAD

  15. Dansyl-peptides matrix-assisted laser desorption/ionization mass spectrometric (MALDI-MS) and tandem mass spectrometric (MS/MS) features improve the liquid chromatography/MALDI-MS/MS analysis of the proteome.

    Science.gov (United States)

    Chiappetta, Giovanni; Ndiaye, Sega; Demey, Emmanuelle; Haddad, Iman; Marino, Gennaro; Amoresano, Angela; Vinh, Joëlle

    2010-10-30

    Peptide tagging is a useful tool to improve matrix-assisted laser desorption/ionization tandem mass spectrometric (MALDI-MS/MS) analysis. We present a new application of the use of the dansyl chloride (DNS-Cl). DNS-Cl is a specific primary amine reagent widely used in protein biochemistry. It adds a fluorescent dimethylaminonaphthalene moiety to the molecule. The evaluation of MALDI-MS and MS/MS analyses of dansylated peptides shows that dansylation raises the ionization efficiency of the most hydrophilic species compared with the most hydrophobic ones. Consequently, higher Mascot scores and protein sequence coverage are obtained by combining MS and MS/MS data of native and tagged samples. The N-terminal DNS-Cl sulfonation improves the peptide fragmentation and promotes the generation of b-fragments allowing better peptide sequencing. In addition, we set up a labeling protocol based on the microwave chemistry. Peptide dansylation proved to be a rapid and cheap method to improve the performance of liquid chromatography (LC)/MALDI-MS/MS analysis at the proteomic scale in terms of peptide detection and sequence coverage. Copyright © 2010 John Wiley & Sons, Ltd.

  16. Comparison of NASA-TLX scale, Modified Cooper-Harper scale and mean inter-beat interval as measures of pilot mental workload during simulated flight tasks.

    Science.gov (United States)

    Mansikka, Heikki; Virtanen, Kai; Harris, Don

    2018-04-30

    The sensitivity of NASA-TLX scale, modified Cooper-Harper (MCH) scale and the mean inter-beat interval (IBI) of successive heart beats, as measures of pilot mental workload (MWL), were evaluated in a flight training device (FTD). Operational F/A-18C pilots flew instrument approaches with varying task loads. Pilots' performance, subjective MWL ratings and IBI were measured. Based on the pilots' performance, three performance categories were formed; high-, medium- and low-performance. Values of the subjective rating scales and IBI were compared between categories. It was found that all measures were able to differentiate most task conditions and there was a strong, positive correlation between NASA-TLX and MCH scale. An explicit link between IBI, NASA-TLX, MCH and performance was demonstrated. While NASA-TLX, MCH and IBI have all been previously used to measure MWL, this study is the first one to investigate their association in a modern FTD, using a realistic flying mission and operational pilots.

  17. Gino Marinuzzi Jr: Electronics and Early Multimedia Mentality in Italy

    Directory of Open Access Journals (Sweden)

    Maurizio Corbella

    2015-08-01

    Full Text Available In this essay I reassess the complexity of the convergence between electronic music and media practices in Rome in the 1950s and 1960s, through the reconstruction of the experience of composer Gino Marinuzzi Jr (1920-96. His engagement with technology as a structuring device of compositional processes is fundamental and inescapable, and brings to the fore crucial issues of ‘applied’ music’s troublesome reputation in the Italian cultural discourse. In reviewing Marinuzzi’s biography over the period 1949-75, my goal is to exemplify the key phases of this transitional period in Italian music history, in which technology, through the spreading of media and their increasing importance in cultural representations, came to constitute a new value of musical activity and at the same time renewed old questions concerning music’s aesthetic autonomy.

  18. MALDI-TOF MS/MS measurements of PMMA

    NARCIS (Netherlands)

    Becer, C.R.; Baumgaertel, A.; Gottschaldt, M.; Schubert, U.S.

    2008-01-01

    The polymer poly(Me methacrylate) (PMMA) was analyzed using the matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) technique. The MALDI-TOF MS app. was coupled with a collision-induced dissocn. (CID) unit. The performance of the MALDI-TOF/TOF MS method in

  19. "I Just Want to Do God's Will:" Teaching Martin Luther King, Jr. as a Religious Leader

    Science.gov (United States)

    Neumann, David

    2018-01-01

    Teachers often respond to the perils of teaching about religion by simply avoiding the subject. An investigation of secondary lesson plans on three prominent Martin Luther King, Jr. websites reveals little attention to the ideology of the civil rights movement, especially those touching on religious ideas. Ignoring King's religious views risks…

  20. Determination of J-R curve from only one experimental test on one sample

    International Nuclear Information System (INIS)

    Lebey, J.; Roche, R.L.

    1983-01-01

    Increasing attention has been given in fracture mechanics to the use of the J concept not only as a criterion of the onset of crack propagation, but also as an aid in the study of propagation stability. As a consequence, there is a need to determine the variation of J with crack extension, this being usually presented in curves known as J-R curves. Earlier methods for determining such curves used several specimens. The present paper describes a procedure avoiding any direct measurement of the crack length and giving a correct value of J when crack propagation occurs. (author)

  1. Critical Void Volume Fraction fc at Void Coalescence for S235JR Steel at Low Initial Stress Triaxiality

    Science.gov (United States)

    Grzegorz Kossakowski, Paweł; Wciślik, Wiktor

    2017-10-01

    The paper is concerned with the nucleation, growth and coalescence of microdefects in the form of voids in S235JR steel. The material is known to be one of the basic steel grades commonly used in the construction industry. The theory and methods of damage mechanics were applied to determine and describe the failure mechanisms that occur when the material undergoes deformation. Until now, engineers have generally employed the Gurson-Tvergaard- Needleman model. This material model based on damage mechanics is well suited to define and analyze failure processes taking place in the microstructure of S235JR steel. It is particularly important to determine the critical void volume fraction fc , which is one of the basic parameters of the Gurson-Tvergaard-Needleman material model. As the critical void volume fraction fc refers to the failure stage, it is determined from the data collected for the void coalescence phase. A case of multi-axial stresses is considered taking into account the effects of spatial stress state. In this study, the parameter of stress triaxiality η was used to describe the failure phenomena. Cylindrical tensile specimens with a circumferential notch were analysed to obtain low values of initial stress triaxiality (η = 0.556 of the range) in order to determine the critical void volume fraction fc . It is essential to emphasize how unique the method applied is and how different it is from the other more common methods involving parameter calibration, i.e. curve-fitting methods. The critical void volume fraction fc at void coalescence was established through digital image analysis of surfaces of S235JR steel, which involved studying real, physical results obtained directly from the material tested.

  2. A new methodology for the evaluation of the J-R curve

    International Nuclear Information System (INIS)

    Donoso, J. R.; Zahr, J.; Landes, J. D.

    2005-01-01

    A new methodology for the construction of J-R curves for ductile materials, based upon the analytical integration of the P-ν relation, is presented. This method is based on the Common and Concise Formats, and on a postulated crack growth law, that relates the amount of stable crack growth with plastic displacement. The model developed, denoted asnC and C, reproduces quite well the experimentally obtained P-ν, Δa-ν and J-Δa curves. The results suggest that the amount of stable crack growth in a ductile material follows a power-law behaviour in its dependence with plastic displacement. This methodology may be used to evaluate instability conditions, through the adequate analytical treatment of the P-ν and J-Δa relations. (Author) 35 refs

  3. LC-MS (/MS) in clinical toxicology screening methods.

    Science.gov (United States)

    Viette, Véronique; Hochstrasser, Denis; Fathi, Marc

    2012-01-01

    Toxicological screening is the analysis of biological samples to detect and identify unknown compounds. The high selectivity and sensitivity of liquid chromatography (LC) coupled to mass spectrometry (MS) or tandem mass spectrometry (MS/MS) technology provide an attractive alternative to the current methods (LC-UV, GC/MS, etc.). For these reasons, an increasing number of applications are being published. This paper is a brief overview of LC-MS(/MS) screening methods developed for clinical toxicology in recent years. Various sample treatments, chromatographic separations and detection by mass spectrometry can be combined to obtain screening methods adapted to the constraints and needs of clinical toxicology laboratories. Currently the techniques are in the hands of specialists, mainly in academic institutions. However, the evolution in technology should allow application of these techniques as a tool in toxicology laboratories, thus allowing a more widespread exploitation of their potential.

  4. Health Care Fraud: Characteristics, Sanctions, and Prevention. Briefing Report to the Honorable William V. Roth, Jr., U.S. Senate.

    Science.gov (United States)

    General Accounting Office, Washington, DC. Accounting and Financial Management Div.

    At the request of Senator William Roth, Jr., the General Accounting Office (GAO) reviewed Medicare and Medicaid fraud investigations that agency inspectors general referred to the Department of Justice for prosecution to identify characteristics of alleged fraud against the government and to determine actions taken against those caught defrauding…

  5. Validity and reliability of Verbal Online Subjective Opinion (VOSO and Modified Cooper-Harper scales in measuring of mental workload

    Directory of Open Access Journals (Sweden)

    Reza Charkhandaz Yeganeh

    2016-12-01

    Full Text Available Introduction: High mental workload is one of the important factors that results in errors in safety and occupational health scope and its measurement has high importance. So, this study aimed to determine validity and reliability of Verbal Online Subjective Opinion (VOSO and Modified Cooper-Harper (MCH scales in measuring mental workload. Methods: This study was conducted on 90 male students of Iran University of Medical Sciences. In this study, the Forward-Backward translation was used for translation of scales. Moreover, Content Validity Ratio (CVR and Content Validity Index (CVI were calculated by having suggestion of 6 Ergonomics and Occupational health experts. The Hybrid Memory Search Task software was used to create mental workload. Convergent validity of scales was calculated using correlation of scales with reaction time and then Test-Retest method was used to determine the reliability of scales. Results: Content and convergent validity of scales were confirmed and correlation of both scales with reaction time were higher than 0.8. Moreover for determination of scales reliabilities, Pearson correlation coefficient between scales values in test and retest trials were 0.86 and 0.91 for VOSO and MCH respectively. Conclusion: It seems that in regard to confirmation of validity and reliability of VOSO and MCH in this study and their high correlation with reaction time, it can use these scales in measurement of mental workload.

  6. Obituary: Ernest Hurst Cherrington, Jr., 1909-1996

    Science.gov (United States)

    Osterbrock, Donald E.

    2003-12-01

    Ernest H. Cherrington, Jr., a long-time member of the AAS, died in San Jose, California on 13 July 1996, following a long illness. He had a short but active career as a research astronomer at Perkins Observatory at Ohio Wesleyan University in Delaware, Ohio before World War II, in which he served as an officer in the Army Air Force. After the war ended he turned to full-time teaching and administration at the University of Akron, and then at Hood College in Frederick, Maryland. Ernest was born on 10 September 1909 in Westerville, Ohio, where his father, Ernest H. Cherrington, Sr., was a leader in the temperance movement and publisher of "American Issue", a Prohibitionist magazine. Ernest Jr.'s mother, Betty Clifford (née Denny) Cherrington, was a homemaker. He was an outstanding student in high school and at Ohio Wesleyan University, which he entered in 1927. The little university's Perkins Observatory with its 69-inch reflector, briefly the second largest telescope in the United States, had just been built and gone into operation. After graduating with a BA magna cum laude in astronomy in 1931, Ernest stayed on one more year and earned his MS with a thesis on the motion of material in the tail of Comet Morehouse, supervised by Nicholas T. Bobrovnikoff. In 1932 Ernest entered the University of California at Berkeley as a graduate student, with a one-year teaching assistantship in the Astronomical Department. This was followed by a two-year Lick Observatory Fellowship. In June 1933 he married Ann McAfee Naylor, who had been a classmate at Delaware High School and Ohio Wesleyan. Ernest did his PhD thesis on spectrophotometry of the Mg I b lines in the solar spectrum, using a high-resolution grating spectrograph on the Berkeley campus, designed by C. Donald Shane, his adviser. In this thesis, Ernest tested and improved the then current theory of strong absorption lines in stellar atmospheres. He also spent several short periods at Lick Observatory on Mount Hamilton

  7. Analysis of acrylamide by LC-MS/MS and GC-MS in processed Japanese foods.

    Science.gov (United States)

    Ono, H; Chuda, Y; Ohnishi-Kameyama, M; Yada, H; Ishizaka, M; Kobayashi, H; Yoshida, M

    2003-03-01

    Acrylamide concentrations in processed foods (63 samples covering 31 product types) from Japan were analysed by LC-MS/MS and GC-MS methods. The limit of detection and limit of quantification of acrylamide were 0.2 ng x ml(-1) (6 fmol) and 0.8 ng x ml(-1) (22 fmol), respectively, by LC-MS/MS, and those of 2,3-dibromopropionamide derived from acrylamide were 12 ng x ml(-1) (52 fmol) and 40 ng x ml(-1) (170 fmol), respectively, by GC-MS. Repeatability given as RSD was 1000 microg x kg(-1). The concentrations in non-whole potato-based snacks, rice crackers processed by grilling or frying, and candied sweet potatoes were lower compared with those in the potato crisps and the whole potato-based fried snacks. One of the whole potato-based fried snacks, however, showed low acrylamide concentration (instant precooked noodles and won-tons were <100 microg x kg(-1) with only one exception. Roasted barley grains for 'Mugi-cha' tea contained 200-600 microg x kg(-1) acrylamide.

  8. Urinary amino acid analysis: a comparison of iTRAQ-LC-MS/MS, GC-MS, and amino acid analyzer.

    Science.gov (United States)

    Kaspar, Hannelore; Dettmer, Katja; Chan, Queenie; Daniels, Scott; Nimkar, Subodh; Daviglus, Martha L; Stamler, Jeremiah; Elliott, Paul; Oefner, Peter J

    2009-07-01

    Urinary amino acid analysis is typically done by cation-exchange chromatography followed by post-column derivatization with ninhydrin and UV detection. This method lacks throughput and specificity. Two recently introduced stable isotope ratio mass spectrometric methods promise to overcome those shortcomings. Using two blinded sets of urine replicates and a certified amino acid standard, we compared the precision and accuracy of gas chromatography/mass spectrometry (GC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) of propyl chloroformate and iTRAQ derivatized amino acids, respectively, to conventional amino acid analysis. The GC-MS method builds on the direct derivatization of amino acids in diluted urine with propyl chloroformate, GC separation and mass spectrometric quantification of derivatives using stable isotope labeled standards. The LC-MS/MS method requires prior urinary protein precipitation followed by labeling of urinary and standard amino acids with iTRAQ tags containing different cleavable reporter ions distinguishable by MS/MS fragmentation. Means and standard deviations of percent technical error (%TE) computed for 20 amino acids determined by amino acid analyzer, GC-MS, and iTRAQ-LC-MS/MS analyses of 33 duplicate and triplicate urine specimens were 7.27+/-5.22, 21.18+/-10.94, and 18.34+/-14.67, respectively. Corresponding values for 13 amino acids determined in a second batch of 144 urine specimens measured in duplicate or triplicate were 8.39+/-5.35, 6.23+/-3.84, and 35.37+/-29.42. Both GC-MS and iTRAQ-LC-MS/MS are suited for high-throughput amino acid analysis, with the former offering at present higher reproducibility and completely automated sample pretreatment, while the latter covers more amino acids and related amines.

  9. IG Statement: Arthur A. Elkins, Jr., on OIG report Early Warning Report: Main EPA Headquarters Warehouse in Landover, Maryland, Requires Immediate EPA Attention

    Science.gov (United States)

    Statement of Inspector General Arthur A. Elkins, Jr., on the Office of Inspector General (OIG) report Early Warning Report: Main EPA Headquarters Warehouse in Landover, Maryland, Requires Immediate EPA Attention.

  10. Urinary Amino Acid Analysis: A Comparison of iTRAQ®-LC-MS/MS, GC-MS, and Amino Acid Analyzer

    Science.gov (United States)

    Kaspar, Hannelore; Dettmer, Katja; Chan, Queenie; Daniels, Scott; Nimkar, Subodh; Daviglus, Martha L.; Stamler, Jeremiah; Elliott, Paul; Oefner, Peter J.

    2009-01-01

    Urinary amino acid analysis is typically done by cation-exchange chromatography followed by post-column derivatization with ninhydrin and UV detection. This method lacks throughput and specificity. Two recently introduced stable isotope ratio mass spectrometric methods promise to overcome those shortcomings. Using two blinded sets of urine replicates and a certified amino acid standard, we compared the precision and accuracy of gas chromatography/mass spectrometry (GC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) of propyl chloroformate and iTRAQ® derivatized amino acids, respectively, to conventional amino acid analysis. The GC-MS method builds on the direct derivatization of amino acids in diluted urine with propyl chloroformate, GC separation and mass spectrometric quantification of derivatives using stable isotope labeled standards. The LC-MS/MS method requires prior urinary protein precipitation followed by labeling of urinary and standard amino acids with iTRAQ® tags containing different cleavable reporter ions distinguishable by MS/MS fragmentation. Means and standard deviations of percent technical error (%TE) computed for 20 amino acids determined by amino acid analyzer, GC-MS, and iTRAQ®-LC-MS/MS analyses of 33 duplicate and triplicate urine specimens were 7.27±5.22, 21.18±10.94, and 18.34±14.67, respectively. Corresponding values for 13 amino acids determined in a second batch of 144 urine specimens measured in duplicate or triplicate were 8.39±5.35, 6.23±3.84, and 35.37±29.42. Both GC-MS and iTRAQ®-LC-MS/MS are suited for high-throughput amino acid analysis, with the former offering at present higher reproducibility and completely automated sample pretreatment, while the latter covers more amino acids and related amines. PMID:19481989

  11. Selenium speciation analysis of Misgurnus anguillicaudatus selenoprotein by HPLC-ICP-MS and HPLC-ESI-MS/MS

    Science.gov (United States)

    Analytical methods for selenium (Se) speciation were developed using high performance liquid chromatography (HPLC) coupled to either inductively coupled plasma mass spectrometry (ICP-MS) or electrospray ionization tandem mass spectrometry (ESI-MS/MS). Separations of selenomethionine (Se-Met) and sel...

  12. MassSieve: Panning MS/MS peptide data for proteins

    OpenAIRE

    Slotta, Douglas J.; McFarland, Melinda A.; Markey, Sanford P.

    2010-01-01

    We present MassSieve, a Java-based platform for visualization and parsimony analysis of single and comparative LC-MS/MS database search engine results. The success of mass spectrometric peptide sequence assignment algorithms has led to the need for a tool to merge and evaluate the increasing data set sizes that result from LC-MS/MS-based shotgun proteomic experiments. MassSieve supports reports from multiple search engines with differing search characteristics, which can increase peptide sequ...

  13. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... Area Donate Donate Search v What Is MS? Definition of MS What Causes MS? Who Gets MS? ... Support Personal Stories d What Is MS? d Definition of MS Myelin Immune-Mediated Disease T Cells ...

  14. Metabolic profiling of roots of liquorice (Glycyrrhiza glabra) from different geographical areas by ESI/MS/MS and determination of major metabolites by LC-ESI/MS and LC-ESI/MS/MS.

    Science.gov (United States)

    Montoro, Paola; Maldini, Mariateresa; Russo, Mariateresa; Postorino, Santo; Piacente, Sonia; Pizza, Cosimo

    2011-02-20

    Liquid chromatography electrospray mass spectrometry (LC-ESI/MS) has been applied to the full characterization of saponins and phenolics in hydroalcoholic extracts of roots of liquorice (Glycyrrhiza glabra). Relative quantitative analyses of the samples with respect to the phenolic constituents and to a group of saponins related to glycyrrhizic acid were performed using LC-ESI/MS. For the saponin constituents, full scan LC-MS/MS fragmentation of the protonated (positive ion mode) or deprotonated (negative ion mode) molecular species generated diagnostic fragment ions that provided information concerning the triterpene skeleton and the number and nature of the substituents. On the basis of the specific fragmentation of glycyrrhizic acid, an LC-MS/MS method was developed in order to quantify the analyte in the liquorice root samples. Chinese G. glabra roots contained the highest levels of glycyrrhizic acid, followed by those from Italy (Calabria). Copyright © 2010 Elsevier B.V. All rights reserved.

  15. Immunopathogenesis of allergic rhinitis

    African Journals Online (AJOL)

    EL-HAKIM

    Druce HM. Allergic and non allergic rhinitis. In: Middleton EM Jr, Reed CE, Ellis EF, Adkinson NF. Jr, Yunginger JW, Busse WW, eds. Allergy: Principles and Practice. 5th ed. St. Louis,. Mo: Mosby, Year-Book;1998.p.1005-16. 3. Blaiss MS. Quality of life in allergic rhinitis. Ann. Allergy Asthma Immunol 1999;83(5):449-54. 4.

  16. Analysis of poly-beta-hydroxybutyrate in environmental samples by GC-MS/MS.

    Science.gov (United States)

    Elhottová, D; Tríska, J; Petersen, S O; Santrůcková, H

    2000-05-01

    Application of gas chromatography-mass spectrometry (GC-MS) can significantly improve trace analyses of compounds in complex matrices from natural environments compared to gas chromatography only. A GC-MS/MS technique for determination of poly-beta-hydroxybutyrate (PHB), a bacterial storage compound, has been developed and used for analysis of two soils stored for up to 319 d, fresh samples of sewage sludge, as well as a pure culture of Bacillus megaterium. Specific derivatization of beta-hydroxybutyrate (3-OH C4:0) PHB monomer units by N-tert-butyl-dimethylsilyl-N-methyltrifluoracetamide (MTBSTFA) improved chromatographic and mass spectrometric properties of the analyte. The diagnostic fragmentation scheme of the derivates tert-butyldimethylsilyl ester and ether of beta-hydroxybutyric acid (MTBSTFA-HB) essential for the PHB identification was shown. The ion trap MS was used, therefore the scan gave the best sensitivity and with MS/MS the noise decreased, so the S/N was better and also with second fragmentation the amount of ions increased compared to SIM. The detection limit for MTBSTFA-HB by GC-MS/MS was about 10(-13) g microL(-1) of injected volume, while by GC (FID) and GC-MS (scan) it was around 10(-10) g microL(-1) of injected volume. Sensitivity of GC-MS/MS measurements of PHB in arable soil and activated sludge samples was down to 10 pg of PHB g(-1) dry matter. Comparison of MTBSTFA-HB detection in natural soil sample by GC (FID), GC-MS (scan) and by GC-MS/MS demonstrated potentials and limitations of the individual measurement techniques.

  17. Edward Sapir e Mattoso Câmara Jr.: intersecçõesDOI:10.5007/1984-8420.2011v12n2p15

    Directory of Open Access Journals (Sweden)

    Lovania Roehrig Teixeira

    2011-03-01

    Full Text Available O conceito de linguagem perpassa diferentes abordagens teóricas e diferentes cientistas sem ser, no entanto, consensual na Linguística. Todavia, algumas características similares acerca do fenômeno da linguagem são encontradas nas abordagens de Edward Sapir e Mattoso Câmara Jr., principalmente, por este último ter realizado traduções de duas obras de Sapir e ter convivido diretamente com grandes linguistas estruturalistas, nos Estados Unidos. O presente artigo descreve e discute algumas das principais aproximações entre as ideias de Mattoso Câmara Jr. e Sapir, que sugerem a filiação do primeiro ao segundo. A partir disso, buscaram-se os aspectos de convergência das concepções linguísticas e identificaram-se três, relacionados à (i linguagem e pensamento, (ii linguagem e arte e (iii linguagem e deriva linguística.

  18. Gunshot wounds to the hand. The Martin Luther King, Jr, General Hospital experience.

    Science.gov (United States)

    Phillips, P; Hansraj, K K; Cox, E E; Ashley, E M

    1995-01-01

    This article is a retrospective review of patients who presented to Martin Luther King, Jr./Drew Medical Center with gunshot wounds and had either isolated or associated injuries to the hand. The following is an account of those injuries noting the location, soft-tissue or bony involvement, and interventional methods that were implemented in the treatment of these patients who resided primarily in South Central Los Angeles. Prompt evaluation and initiation of treatment is essential in the management of both high- and low-velocity gunshot wounds so as to decrease the potential morbidity that often follows. Society must also look at the prevalence of these injuries and address the underlying issues that often are the root of the acts of violence.

  19. Cannabinoids determination in oral fluid by SPME-GC/MS and UHPLC-MS/MS and its application on suspected drivers.

    Science.gov (United States)

    Anzillotti, Luca; Castrignanò, Erika; Strano Rossi, Sabina; Chiarotti, Marcello

    2014-12-01

    The confirmation of Δ9-tetrahydrocannabinol (THC) in oral fluid (OF) is an important issue for assessing Driving Under the Influence of Drugs (DUID). The aim of this research was to develop a highly sensitive method with minimal sample pre-treatment suitable for the analysis of small OF volumes (100 μL) for the confirmation of cannabinoids in DUID cases. Two methods were compared for the confirmation of THC in residual OF samples, obtained from a preliminary on-site screening with commercial devices. An ultra high performance LC-MS (UHPLC-MS/MS) method and an SPME-GC/MS method were hence developed. 100 μL of the residual mixture OF/preservative buffer or neat OF was simply added to 10 μL of THC-D3 (1 μg/mL) and submitted to the two different analyses: A - direct injection of 10 μL in UHPLC-MS/MS in positive electrospray ionisation (ESI) mode and B - sampling for 30 min with SPME (100 μm polydimethylsiloxane or PDMS fibre) and direct injection by desorption of the fibre in the GC injection port. The lowest limit of detection (LLOD) of THC was 2 ng/mL in UHPLC-MS/MS and 0.5 ng/mL in SPME-GC/MS. In addition, cannabidiol (CBD) and cannabinol (CBN) could be detected in GC/MS equipment at 2 ng/mL, whilst in UHPLC-MS/MS the LLOD was 20 ng/mL. Both methods were applied to 70 samples coming from roadside tests. By SPME-GC/MS analysis, THC was confirmed in 42 samples, whilst CBD was detected in 21 of them, along with CBN in 14 samples. THC concentrations ranged from traces below the lowest limit of quantification or LLOQ (2 ng/mL) up to 690 ng/mL. Copyright © 2014 Forensic Science Society. Published by Elsevier Ireland Ltd. All rights reserved.

  20. Software ion scan functions in analysis of glycomic and lipidomic MS/MS datasets.

    Science.gov (United States)

    Haramija, Marko

    2018-03-01

    Hardware ion scan functions unique to tandem mass spectrometry (MS/MS) mode of data acquisition, such as precursor ion scan (PIS) and neutral loss scan (NLS), are important for selective extraction of key structural data from complex MS/MS spectra. However, their software counterparts, software ion scan (SIS) functions, are still not regularly available. Software ion scan functions can be easily coded for additional functionalities, such as software multiple precursor ion scan, software no ion scan, and software variable ion scan functions. These are often necessary, since they allow more efficient analysis of complex MS/MS datasets, often encountered in glycomics and lipidomics. Software ion scan functions can be easily coded by using modern script languages and can be independent of instrument manufacturer. Here we demonstrate the utility of SIS functions on a medium-size glycomic MS/MS dataset. Knowledge of sample properties, as well as of diagnostic and conditional diagnostic ions crucial for data analysis, was needed. Based on the tables constructed with the output data from the SIS functions performed, a detailed analysis of a complex MS/MS glycomic dataset could be carried out in a quick, accurate, and efficient manner. Glycomic research is progressing slowly, and with respect to the MS experiments, one of the key obstacles for moving forward is the lack of appropriate bioinformatic tools necessary for fast analysis of glycomic MS/MS datasets. Adding novel SIS functionalities to the glycomic MS/MS toolbox has a potential to significantly speed up the glycomic data analysis process. Similar tools are useful for analysis of lipidomic MS/MS datasets as well, as will be discussed briefly. Copyright © 2017 John Wiley & Sons, Ltd.

  1. 75 FR 57846 - Airworthiness Directives; Robert E. Rust, Jr. Model DeHavilland DH.C1 Chipmunk 21, DH.C1 Chipmunk...

    Science.gov (United States)

    2010-09-23

    ... Aircraft Certification Office (ACO), 1701 Columbia Avenue, College Park, Georgia 30337; telephone: (404... Airworthiness Directives; Robert E. Rust, Jr. Model DeHavilland DH.C1 Chipmunk 21, DH.C1 Chipmunk 22, and DH.C1... the Docket Office (phone: 800-647-5527) is Document Management Facility, U.S. Department of...

  2. Analytical Method Details (MS): SE52_MS01 [Metabolonote[Archive

    Lifescience Database Archive (English)

    Full Text Available stem and Waters Q-Tof Premier UPLC-QTOF-MS ESI Negative The eluates (3 μl) were subsequently subjected to metabolome...DS column (LC-ESI-Q-Tof/MS, HPLC: Waters Acquity UPLC system; MS: Waters Q-Tof Premier). The metabolome...d (Matsuda et al., 2009c, 2010a). Briefly, the metabolome data were obtained in the negative ion mode (m/z 1... the complex nature of the metabolome data. To construct MS2T libraries, the extracts of five ecotypes were

  3. Information-dependent acquisition-mediated LC-MS/MS screening procedure with semiquantitative potential.

    Science.gov (United States)

    Decaestecker, Tineke N; Vande Casteele, Sofie R; Wallemacq, Pierre E; Van Peteghem, Carlos H; Defore, Dieter L; Van Bocxlaer, Jan F

    2004-11-01

    The development of a LC-MS/MS general unknown screening procedure for toxicologically relevant substances in blood samples by means of information-dependent acquisition on a Q-TOF is reported. IDA is an artificial intelligence-based product ion scan mode providing automatic "on-the-fly" MS to MS/MS switching. By performing information-dependent scanning at two different fragmentation energies, two collision-induced dissociation product ion spectra for each of the detected compounds are generated. As such, information-rich MS/MS spectra are obtained from precursor ions not known beforehand. In addition, limitation of the MS/MS acquisition time to an acceptable minimum resulted in an almost instantaneous switch back to the MS mode. As such, this approach provided MS chromatograms that still could be of use for semiquantitative purposes. Since the switching intensity threshold, unequivocally related to the background noise, proved a critical parameter, the solid-phase extraction procedure, the liquid chromatographic conditions, and the mass spectrometric parameters all were optimized to the advantage of information-dependent acquisition. Finally, the screening procedure we developed was benchmarked, on one hand, qualitatively against the results obtained from traditional GUS approaches in a number of routine toxicological laboratories (20 samples) and, on the other hand, quantitatively with respect to its potential against established LC-MS/MS methods (7 samples). The procedure performed very well from a qualitative point of view; almost all of the drugs detected by the conventional techniques were identified, as well as additional drugs that were not previously reported. The procedure proved well-suited for an initial semiquantitative assessment, as is customary in, for example, forensic toxicology before accurate intoxication levels are determined using targeted analytical analyses.

  4. East Weddell Sea echinoids from the JR275 expedition

    Directory of Open Access Journals (Sweden)

    Thomas Saucède

    2015-05-01

    Full Text Available Information regarding the echinoids in this dataset is based on the Agassiz Trawl (AGT and epibenthic sledge (EBS samples collected during the British Antarctic Survey cruise JR275 on the RRS James Clark Ross in the austral summer 2012. A total of 56 (1 at the South Orkneys and 55 in the Eastern Weddell Sea Agassiz Trawl and 18 (2 at the South Orkneys and 16 in the Eastern Weddell Sea epibenthic sledge deployments were performed at depths ranging from ~280 to ~2060 m. This presents a unique collection for the Antarctic benthic biodiversity assessment of an important group of benthic invertebrates. In total 487 specimens belonging to six families, 15 genera, and 22 morphospecies were collected. The species richness per station varied between one and six. Total species richness represents 27% of the 82 echinoid species ever recorded in the Southern Ocean (David et al. 2005b, Pierrat et al. 2012, Saucède et al. 2014. The Cidaridae (sub-family Ctenocidarinae and Schizasteridae are the two most speciose families in the dataset. They comprise seven and nine species respectively. This is illustrative of the overall pattern of echinoid diversity in the Southern Ocean where 65% of Antarctic species belong to the families Schizasteridae and Cidaridae (Pierrat et al. 2012.

  5. Study of T L LiF: Mg,Ti (Model JR1152C) material for its use in the environmental monitoring; Estudio del material TL LiF: Mg, Ti (JR1152C) para su empleo en el monitoreo ambiental

    Energy Technology Data Exchange (ETDEWEB)

    Molina P, D.; Diaz B, E.; Prendes A, M. [Centro de Proteccion e Higiene de las Radiaciones, CPHR, Apdo. postal 6195, Habana 6, CP 10600, Ciudad Habana (Cuba)

    1999-07-01

    In order to evaluate the possibility to use the T L material of LiF: Mg,Ti (Model JR1152C) as environmental dosemeter it was realized its characterization of it according to the established criterion in the standard IEC-1066. The properties studied were: homogeneity of the lot, reproducibility, response linearity, detection threshold, auto irradiation, residual signal, response pride (fading) and angular dependence. The results prove the compliment of the IEC requirements and therefore the applicability of this dosemeter in the environmental monitoring. (Author)

  6. Automated protein identification by the combination of MALDI MS and MS/MS spectra from different instruments.

    Science.gov (United States)

    Levander, Fredrik; James, Peter

    2005-01-01

    The identification of proteins separated on two-dimensional gels is most commonly performed by trypsin digestion and subsequent matrix-assisted laser desorption ionization (MALDI) with time-of-flight (TOF). Recently, atmospheric pressure (AP) MALDI coupled to an ion trap (IT) has emerged as a convenient method to obtain tandem mass spectra (MS/MS) from samples on MALDI target plates. In the present work, we investigated the feasibility of using the two methodologies in line as a standard method for protein identification. In this setup, the high mass accuracy MALDI-TOF spectra are used to calibrate the peptide precursor masses in the lower mass accuracy AP-MALDI-IT MS/MS spectra. Several software tools were developed to automate the analysis process. Two sets of MALDI samples, consisting of 142 and 421 gel spots, respectively, were analyzed in a highly automated manner. In the first set, the protein identification rate increased from 61% for MALDI-TOF only to 85% for MALDI-TOF combined with AP-MALDI-IT. In the second data set the increase in protein identification rate was from 44% to 58%. AP-MALDI-IT MS/MS spectra were in general less effective than the MALDI-TOF spectra for protein identification, but the combination of the two methods clearly enhanced the confidence in protein identification.

  7. Experimental Gonococcal Infection in Male Volunteers: Cumulative Experience with Neisseria Gonorrhoeae Strains FA1090 and MS11mkC

    Science.gov (United States)

    2011-05-31

    variation and pathogenic- ity during 35 months in vitro. J. Bacteriol. 96, 596–605. Kellogg,D. S. Jr., Peacock ,W. L. Jr., Dea- con, W. E., Brown, L., and...and Frontiers Media SA, which permits use, distribution and reproduction in other forums, provided the original authors and source are credited and

  8. Molecular analysis of intact preen waxes of Calidris Canutus (Aves: Scolopacidae) by GC/MS and GC/MS/MS

    NARCIS (Netherlands)

    Sinninghe Damsté, J.S.; Dekker, M.H.A.; Piersma, T.

    2000-01-01

    The intact preen wax esters of the red knot Calidris canutus were studied with gas chromatography/mass spectrometry (GC/MS) and GC/MS/MS. In this latter technique, transitions from the molecular ion to fragment ions representing the fatty acid moiety of the wax esters were measured, providing

  9. Obituary: Raymond Edwin White Jr., 1933-2004

    Science.gov (United States)

    Liebert, James William

    2004-12-01

    Raymond E. White, Jr., died unexpectedly at his home, in the early morning hours of October 12, 2004. Death appears to have been caused by severe diabetic shock. He retired from the Department of Astronomy/Steward Observatory in July 1999 with the title of University Distinguished Professor, after serving on the faculty of this institution for over 35 years. He was born in Freeport, Illinois, on 6 May 1933, to Beatrice and Raymond E, Sr. -the latter being a career soldier in the US Army. Ray's early schooling took place in Illinois, New Jersey, Germany and Switzerland, following his father's assignments. He obtained a bachelors degree from the University of Illinois in 1955. Next Ray enlisted in the US Army, but quickly was enrolled in Officer Candidate School. He then served as lst Lt. in the US Army Corps of Engineers. Although military affairs remained a lifelong interest, and he was a member of the Company of Military Historians, Ray decided after three years to return to academia. He entered the astronomy PhD program at the University of Illinois in 1958. His PhD dissertation was supervised by Ivan R. King. Ray accepted a faculty position at the University of Arizona in 1964. First and foremost, Ray White was known at Arizona as an excellent teacher, revered by a large number of former students. When the astronomy major program was begun in 1967, Ray was one of three, original, major advisors. Over the next three decades, he was a leader at the University level in reforming the undergraduate program and courses. He was selected Outstanding University Faculty Member in April 1989 and he served as one of a handful of professors who are Faculty Fellows. These Fellows devote untold hundreds of hours as part-time residents at student dormitories, to give students a friendly face to address their problems. In 1995, Ray was among the first group of faculty to be recognized as University Distinguished Professors. In the year of his retirement, 1999, University

  10. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... Definition of MS Myelin Immune-Mediated Disease T Cells d What Causes MS? Disproved Theories Viruses Clusters ... d Research News & Progress Research News MSPARIS2017 Stem Cells in MS Progressive MS Research Clinical Trials in ...

  11. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... MS Relapsing-remitting MS (RRMS) Share this page Facebook Twitter Email Relapsing-remitting MS (RRMS) Relapsing-remitting ... Here Start Here Colophon Stay Informed Join Us Facebook Twitter LinkedIn YouTube Pinterest MS Connection About the ...

  12. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... d Living Well with MS d Diet, Exercise & Healthy Behaviors Diet & Nutrition Exercise Heat & Temperature Sensitivity Sleep Vaccinations Women's Health Unhealthy Habits Managing MS and Another Condition Aging with MS Anesthesia and Surgery Managing Your MS ...

  13. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... to navigation Skip to content Menu Navigation National Multiple Sclerosis Society Sign In In Your Area Donate Donate ... of MS What Causes MS? Who Gets MS? Multiple Sclerosis FAQs Types of MS Related Conditions Symptoms & Diagnosis ...

  14. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... Relapsing-remitting MS (RRMS) Share this page Facebook Twitter Email Relapsing-remitting MS (RRMS) Relapsing-remitting MS ( ... Start Here Colophon Stay Informed Join Us Facebook Twitter LinkedIn YouTube Pinterest MS Connection About the Society ...

  15. Multivariable modeling of pressure vessel and piping J-R data

    International Nuclear Information System (INIS)

    Eason, E.D.; Wright, J.E.; Nelson, E.E.

    1991-05-01

    Multivariable models were developed for predicting J-R curves from available data, such as material chemistry, radiation exposure, temperature, and Charpy V-notch energy. The present work involved collection of public test data, application of advanced pattern recognition tools, and calibration of improved multivariable models. Separate models were fitted for different material groups, including RPV welds, Linde 80 welds, RPV base metals, piping welds, piping base metals, and the combined database. Three different types of models were developed, involving different combinations of variables that might be available for applications: a Charpy model, a preirradiation Charpy model, and a copper-fluence model. In general, the best results were obtained with the preirradiation Charpy model. The copper-fluence model is recommended only if Charpy data are unavailable, and then only for Linde 80 welds. Relatively good fits were obtained, capable of predicting the values of J for pressure vessel steels to with a standard deviation of 13--18% over the range of test data. The models were qualified for predictive purposes by demonstrating their ability to predict validation data not used for fitting. 20 refs., 45 figs., 16 tabs

  16. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... the Challenges of MS You CAN! Webcasts DVDs Books For Kids: Keep S'myelin Información en Español Brochures ... Managing MS and Another Condition Aging with MS Anesthesia and Surgery Managing Your MS d Emotional Well- ...

  17. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... the Challenges of MS You CAN! Webcasts DVDs Books For Kids: Keep S'myelin Información en Español Brochures ... MS Managing MS Resources for You and Your Practice Publications for Clinicians Publications for Your Patients MS ...

  18. pDeep: Predicting MS/MS Spectra of Peptides with Deep Learning.

    Science.gov (United States)

    Zhou, Xie-Xuan; Zeng, Wen-Feng; Chi, Hao; Luo, Chunjie; Liu, Chao; Zhan, Jianfeng; He, Si-Min; Zhang, Zhifei

    2017-12-05

    In tandem mass spectrometry (MS/MS)-based proteomics, search engines rely on comparison between an experimental MS/MS spectrum and the theoretical spectra of the candidate peptides. Hence, accurate prediction of the theoretical spectra of peptides appears to be particularly important. Here, we present pDeep, a deep neural network-based model for the spectrum prediction of peptides. Using the bidirectional long short-term memory (BiLSTM), pDeep can predict higher-energy collisional dissociation, electron-transfer dissociation, and electron-transfer and higher-energy collision dissociation MS/MS spectra of peptides with >0.9 median Pearson correlation coefficients. Further, we showed that intermediate layer of the neural network could reveal physicochemical properties of amino acids, for example the similarities of fragmentation behaviors between amino acids. We also showed the potential of pDeep to distinguish extremely similar peptides (peptides that contain isobaric amino acids, for example, GG = N, AG = Q, or even I = L), which were very difficult to distinguish using traditional search engines.

  19. Ferro-based derivatizing agents for LC/MS an LC/EC/MS

    NARCIS (Netherlands)

    Seiwert, Bettina

    2007-01-01

    Within this thesis, the development and application of ferrocene-based derivatizing agents for LC/MS and LC/EC/MS is presented. The advantages of derivatization by ferrocenes are the similtaneous introduction of a mass tag and an electroactive group, which make them ideally suited for LC/MS and

  20. Application of CE-ICP-MS and CE-ESI-MS/MS for identification of Zn-binding ligands in Goji berries extracts.

    Science.gov (United States)

    Ruzik, Lena; Kwiatkowski, Piotr

    2018-06-01

    The identification of groups of ligands binding metals is a crucial issue for the better understanding of their bioaccessibility. In the current study, we have intended an approach for identification of Zn-binding ligands based on using capillary electrophoresis combined with inductively coupled plasma mass spectrometry (CE-ICP-MS) and tandem electrospray ionization mass spectrometry (CE-ESI-MS/MS). The approach, which featured the use of the coupling of capillary electrophoresis with inductively coupled plasma mass spectrometry allows to separate and observe zinc ions present in complexes with respect to their size and charge and to identify nine compounds with zinc isotopic profile. CE-ICP-MS provides us with information about presence of zinc species and elemental information about zinc distribution. CE-ESI-MS/MS provide us with information about the most favorable Zn binding ligands: amino acids, flavonols, stilbenoids, fenolic acids and carotenoids. The presented work is the continuation of previous studies based on using LC-ESI-MS/MS, though, now we presented a new solutions with the possibility of changing detectors without changing the separation techniques, what is important without re-optimizing the method. The new presented method allows to identify the zinc-binding ligands in shorter time. Copyright © 2018 Elsevier B.V. All rights reserved.

  1. Analysis of pesticide residues in strawberries and soils by GC-MS/MS, LC-MS/MS and two-dimensional GC-time-of-flight MS comparing organic and integrated pest management farming.

    Science.gov (United States)

    Fernandes, Virgínia C; Lehotay, Steven J; Geis-Asteggiante, Lucía; Kwon, Hyeyoung; Mol, Hans G J; van der Kamp, Henk; Mateus, Nuno; Domingues, Valentina F; Delerue-Matos, Cristina

    2014-01-01

    This study analysed 22 strawberry and soil samples after their collection over the course of 2 years to compare the residue profiles from organic farming with integrated pest management practices in Portugal. For sample preparation, we used the citrate-buffered version of the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. We applied three different methods for analysis: (1) 27 pesticides were targeted using LC-MS/MS; (2) 143 were targeted using low pressure GC-tandem mass spectrometry (LP-GC-MS/MS); and (3) more than 600 pesticides were screened in a targeted and untargeted approach using comprehensive, two-dimensional gas chromatography time-of-flight mass spectrometry (GC × GC-TOF-MS). Comparison was made of the analyses using the different methods for the shared samples. The results were similar, thereby providing satisfactory confirmation of both similarly positive and negative findings. No pesticides were found in the organic-farmed samples. In samples from integrated pest management practices, nine pesticides were determined and confirmed to be present, ranging from 2 µg kg(-1) for fluazifop-p-butyl to 50 µg kg(-1) for fenpropathrin. Concentrations of residues in strawberries were less than European maximum residue limits.

  2. Quantitative Determination of Perfluorochemicals and Fluorotelomer Alcohols in Plants from Biosolid-Amended Fields using LC/MS/MS and GC/MS

    Science.gov (United States)

    Analytical methods for determining perfluorochemicals (PFCs) and fluorotelomer alcohols (FTOHs) in plants using liquid chromatography/tandem mass spectrometry (LC/MS/MS) and gas chromatography/mass spectrometry (GC/MS) were developed, and applied to quantify a suite of analytes i...

  3. In Vivo Metabolism Study of Xiamenmycin A in Mouse Plasma by UPLC-QTOF-MS and LC-MS/MS

    Directory of Open Access Journals (Sweden)

    Feng Lei

    2015-01-01

    Full Text Available Xiamenmycin A is an antifibrotic leading compound with a benzopyran skeleton that is isolated from mangrove-derived Streptomyces xiamenensis. As a promising small molecule for fibrotic diseases, less information is known about its metabolic characteristics in vivo. In this study, the time-course of xiamenmycin A in mouse plasma was investigated by relative quantification. After two types of administration of xiamenmycin A at a single dose of 10 mg/kg, the plasma concentrations were measured quantitatively by LC-MS/MS. The dynamic changes in the xiamenmycin A concentration showed rapid absorption and quick elimination in plasma post-administration. Four metabolites (M1–M4 were identified in blood by UPLC-QTOF-MS, and xiamenmycin B (M3 is the principal metabolite in vivo, as verified by comparison of the authentic standard sample. The structures of other metabolites were identified based on the characteristics of their MS and MS/MS data. The newly identified metabolites are useful for understanding the metabolism of xiamenmycin A in vivo, aiming at the development of an anti-fibrotic drug candidate for the therapeutic treatment of excessive fibrotic diseases.

  4. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... Become an MS Activist Take Action Current Advocacy Issues Advocacy Results Advocacy News d Raise Awareness d ... MS are more likely to experience gradually worsening problems with walking and mobility, along with whatever other symptoms they may have. Diagnosing relapsing-remitting MS (RRMS) Learn More Learn More ... Room MS Prevalence ...

  5. Survey of diagnostic and treatment practices for multiple sclerosis (MS) in Europe. Part 2: Progressive MS, paediatric MS, pregnancy and general management.

    Science.gov (United States)

    Fernández, O; Delvecchio, M; Edan, G; Fredrikson, S; Giovannoni, G; Hartung, H-P; Havrdova, E; Kappos, L; Pozzilli, C; Soerensen, P S; Tackenberg, B; Vermersch, P; Comi, G

    2018-05-01

    The European Charcot Foundation supported the development of a set of surveys to understand current practice patterns for the diagnosis and management of multiple sclerosis (MS) in Europe. Part 2 of the report summarizes survey results related to secondary progressive MS (SPMS), primary progressive MS (PPMS), pregnancy, paediatric MS and overall patient management. A steering committee of MS neurologists developed case- and practice-based questions for two sequential surveys distributed to MS neurologists throughout Europe. Respondents generally favoured changing rather than stopping disease-modifying treatment (DMT) in patients transitioning from relapsing-remitting MS to SPMS, particularly with active disease. Respondents would not initiate DMT in patients with typical PPMS symptoms, although the presence of ≥1 spinal cord or brain gadolinium-enhancing lesion might affect that decision. For patients considering pregnancy, respondents were equally divided on whether to stop treatment before or after conception. Respondents strongly favoured starting DMT in paediatric MS with active disease; recommended treatments included interferon, glatiramer acetate and, in John Cunningham virus negative patients, natalizumab. Additional results regarding practice-based questions and management are summarized. Results of part 2 of the survey of diagnostic and treatment practices for MS in Europe largely mirror results for part 1, with neurologists in general agreement about the treatment and management of SPMS, PPMS, pregnancy and paediatric MS as well as the general management of MS. However, there are also many areas of disagreement, indicating the need for evidence-based recommendations and/or guidelines. © 2018 EAN.

  6. Sulphur fertilization influences the sulphur species composition in Allium sativum: sulphomics using HPLC-ICPMS/MS-ESI-MS/MS.

    Science.gov (United States)

    Raab, Andrea; Ronzan, Marilena; Feldmann, Joerg

    2017-10-18

    Garlic (A. sativum) contains a large number of small sulphur (S)-containing metabolites, which are important for its taste and smell and vary with A. sativum variety and growth conditions. This study was designed to investigate the influence of different sulphur-fertilization regimes on low molecular weight S-species by attempting the first sulphur mass balance in A. sativum roots and bulbs using HPLC-ICPMS/MS-ESI-MS/MS. Species unspecific quantification of acid soluble S-containing metabolites was achieved using HPLC-ICP-MS/MS. For identification of the compounds, high resolution ESI-MS (Orbitrap LTQ and q-TOF) was used. The plants contained up to 54 separated sulphur-containing compounds, which constitute about 80% of the total sulphur present in A. sativum. The roots and bulbs of A. sativum contained the same compounds, but not necessarily the same amounts and proportions. The S-containing metabolites in the roots reacted more sensitively to manipulations of sulphur fertilization than those compounds in the bulbs. In addition to known compounds (e.g. γ-glutamyl-S-1-propenylcysteine) we were able to identify and partially quantify 31 compounds. Three as yet undescribed S-containing compounds were also identified and quantified for the first time. Putative structures were assigned to the oxidised forms of S-1-propenylmercaptoglutathione, S-2-propenylmercaptoglutathione, S-allyl/propenyl-containing PC-2 and 2-amino-3-[(2-carboxypropyl)sulfanyl]propanoic acid. The parallel use of ICP-MS/MS as a sulphur-specific detector and ESI-MS as a molecular detector simplifies the identification and quantification of sulphur containing metabolites without species specific standards. This non-target analysis approach enables a mass balance approach and identifies the occurrence of the so far unidentified organosulphur compounds. The experiments showed that the sulphur-fertilization regime does not influence sulphur-speciation, but the concentration of some S

  7. Characterization, stoichiometry, and stability of salivary protein-tannin complexes by ESI-MS and ESI-MS/MS.

    Science.gov (United States)

    Canon, Francis; Paté, Franck; Meudec, Emmanuelle; Marlin, Thérèse; Cheynier, Véronique; Giuliani, Alexandre; Sarni-Manchado, Pascale

    2009-12-01

    Numerous protein-polyphenol interactions occur in biological and food domains particularly involving proline-rich proteins, which are representative of the intrinsically unstructured protein group (IUP). Noncovalent protein-ligand complexes are readily detected by electrospray ionization mass spectrometry (ESI-MS), which also gives access to ligand binding stoichiometry. Surprisingly, the study of interactions between polyphenolic molecules and proteins is still an area where ESI-MS has poorly benefited, whereas it has been extensively applied to the detection of noncovalent complexes. Electrospray ionization mass spectrometry has been applied to the detection and the characterization of the complexes formed between tannins and a human salivary proline-rich protein (PRP), namely IB5. The study of the complex stability was achieved by low-energy collision-induced dissociation (CID) measurements, which are commonly implemented using triple quadrupole, hybrid quadrupole time-of-flight, or ion trap instruments. Complexes composed of IB5 bound to a model polyphenol EgCG have been detected by ESI-MS and further analyzed by MS/MS. Mild ESI interface conditions allowed us to observe intact noncovalent PRP-tannin complexes with stoichiometries ranging from 1:1 to 1:5. Thus, ESI-MS shows its efficiency for (1) the study of PRP-tannin interactions, (2) the determination of stoichiometry, and (3) the study of complex stability. We were able to establish unambiguously both their stoichiometries and their overall subunit architecture via tandem mass spectrometry and solution disruption experiments. Our results prove that IB5.EgCG complexes are maintained intact in the gas phase.

  8. An improved method of sample preparation on AnchorChip targets for MALDI-MS and MS/MS and its application in the liver proteome project

    DEFF Research Database (Denmark)

    Zhang, Xumin; Shi, Liang; Shu, Shaokung

    2007-01-01

    An improved method for sample preparation for MALDI-MS and MS/MS using AnchorChip targets is presented. The method, termed the SMW method (sample, matrix wash), results in better sensitivity for peptide mass fingerprinting as well as for sequencing by MS/MS than previously published methods. The ...

  9. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... for You and Your Practice Publications for Clinicians Publications for Your Patients MS Navigator Program Programs and Services for Your Patients ... Relapsing-remitting MS (RRMS) Relapsing-remitting MS ( ...

  10. An in silico MS/MS library for automatic annotation of novel FAHFA lipids.

    Science.gov (United States)

    Ma, Yan; Kind, Tobias; Vaniya, Arpana; Gennity, Ingrid; Fahrmann, Johannes F; Fiehn, Oliver

    2015-01-01

    A new lipid class named 'fatty acid esters of hydroxyl fatty acids' (FAHFA) was recently discovered in mammalian adipose tissue and in blood plasma and some FAHFAs were found to be associated with type 2 diabetes. To facilitate the automatic annotation of FAHFAs in biological specimens, a tandem mass spectra (MS/MS) library is needed. Due to the limitation of the commercial available standard compounds, we proposed building an in silico MS/MS library to extend the coverage of molecules. We developed a computer-generated library with 3267 tandem mass spectra (MS/MS) for 1089 FAHFA species. FAHFA spectra were generated based on authentic standards with negative mode electrospray ionization and 10, 20, and 40 V collision induced dissociation at 4 spectra/s as used in in ultra-high performance liquid chromatography-QTOF mass spectrometry studies. However, positional information of the hydroxyl group is only obtained either at lower QTOF spectra acquisition rates of 1 spectrum/s or at the MS(3) level in ion trap instruments. Therefore, an additional set of 4290 fragment-rich MS/MS spectra was created to enable distinguishing positional FAHFA isomers. The library was generated based on ion fragmentations and ion intensities of FAHFA external reference standards, developing a heuristic model for fragmentation rules and extending these rules to large swaths of computer-generated structures of FAHFAs with varying chain lengths, degrees of unsaturation and hydroxyl group positions. Subsequently, we validated the new in silico library by discovering several new FAHFA species in egg yolk, showing that this library enables high-throughput screening of FAHFA lipids in various biological matrices. The developed library and templates are freely available for commercial or noncommercial use at http://fiehnlab.ucdavis.edu/staff/yanma/fahfa-lipid-library. This in silico MS/MS library allows users to annotate FAHFAs from accurate mass tandem mass spectra in an easy and fast manner

  11. Basil A. Pruitt Jr. MD and the US Army Institute for Surgical Research: Five Decades of Science, Clinical Care, Mentorship, and Leadership.

    Science.gov (United States)

    Stewart, Ronald M

    2017-08-24

    Over the past half century Dr. Basil A. Pruitt, Jr., a great citizen, surgeon, innovator, mentor and leader, transformed our world through his dogged commitment to science and service to humanity. Dr. Pruitt's contribution lives on in the work of the US Army Institute of Surgical Research and the surgeons, physicians and scientists he shaped and inspired.

  12. Peer-Reviewed Research and the IEP: Implications of "Ridley School District v. M.R. and J.R. ex rel. E.R." (2012)

    Science.gov (United States)

    Yell, Mitchell L.; Katsiyannis, Antonis; Losinski, Mickey; Marshall, Kelsey

    2016-01-01

    This article examines a case out of the U.S. Court of Appeals for the Third Circuit: "Ridley School District v. M.R and J.R. ex rel. E.R." (2012). The case is the first circuit court case in which the Individuals with Disabilities Education Improvement Act requirement that special education services be based on peer-reviewed research…

  13. Structure Elucidation of Unknown Metabolites in Metabolomics by Combined NMR and MS/MS Prediction.

    Science.gov (United States)

    Boiteau, Rene M; Hoyt, David W; Nicora, Carrie D; Kinmonth-Schultz, Hannah A; Ward, Joy K; Bingol, Kerem

    2018-01-17

    We introduce a cheminformatics approach that combines highly selective and orthogonal structure elucidation parameters; accurate mass, MS/MS (MS²), and NMR into a single analysis platform to accurately identify unknown metabolites in untargeted studies. The approach starts with an unknown LC-MS feature, and then combines the experimental MS/MS and NMR information of the unknown to effectively filter out the false positive candidate structures based on their predicted MS/MS and NMR spectra. We demonstrate the approach on a model mixture, and then we identify an uncatalogued secondary metabolite in Arabidopsis thaliana . The NMR/MS² approach is well suited to the discovery of new metabolites in plant extracts, microbes, soils, dissolved organic matter, food extracts, biofuels, and biomedical samples, facilitating the identification of metabolites that are not present in experimental NMR and MS metabolomics databases.

  14. Analytical Method Details (MS): SE53_MS03 [Metabolonote[Archive

    Lifescience Database Archive (English)

    Full Text Available SE53_MS03 CE-TOF/MS Agilent CE capillary electrophoresis system,Agilent G3250AA LC/...s were performed using an Agilent CE capillary electrophoresis system (Agilent Technologies, Waldbronn, Germ

  15. Quality evaluation of LC-MS/MS-based E. coli H antigen typing (MS-H) through label-free quantitative data analysis in a clinical sample setup.

    Science.gov (United States)

    Cheng, Keding; Sloan, Angela; McCorrister, Stuart; Peterson, Lorea; Chui, Huixia; Drebot, Mike; Nadon, Celine; Knox, J David; Wang, Gehua

    2014-12-01

    The need for rapid and accurate H typing is evident during Escherichia coli outbreak situations. This study explores the transition of MS-H, a method originally developed for rapid H antigen typing of E. coli using LC-MS/MS of flagella digest of reference strains and some clinical strains, to E. coli isolates in clinical scenario through quantitative analysis and method validation. Motile and nonmotile strains were examined in batches to simulate clinical sample scenario. Various LC-MS/MS batch run procedures and MS-H typing rules were compared and summarized through quantitative analysis of MS-H data output for a standard method development. Label-free quantitative data analysis of MS-H typing was proven very useful for examining the quality of MS-H result and the effects of some sample carryovers from motile E. coli isolates. Based on this, a refined procedure and protein identification rule specific for clinical MS-H typing was established and validated. With LC-MS/MS batch run procedure and database search parameter unique for E. coli MS-H typing, the standard procedure maintained high accuracy and specificity in clinical situations, and its potential to be used in a clinical setting was clearly established. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Multi-Segment Direct Inject nano-ESI-LTQ-FT-ICR-MS/MS For Protein Identification

    Directory of Open Access Journals (Sweden)

    Neal Rachel E

    2011-07-01

    Full Text Available Abstract Reversed phase high performance liquid chromatography (HPLC interfaced to electrospray tandem mass spectrometry (MS/MS is commonly used for the identification of peptides from proteolytically cleaved proteins embedded in a polyacrylamide gel matrix as well as for metabolomics screening. HPLC separations are time consuming (30-60 min average, costly (columns and mobile phase reagents, and carry the risk of column carry over between samples. The use of a chip-based nano-ESI platform (Advion NanoMate based on replaceable nano-tips for sample introduction eliminates sample cross-contamination, provides unchanging sample matrix, and enhances spray stability with attendant increases in reproducibility. Recent papers have established direct infusion nano-ESI-MS/MS utilizing the NanoMate for protein identification of gel spots based on full range MS scans with data dependent MS/MS. In a full range scan, discontinuous ion suppression due to sample matrix can impair identification of putative mass features of interest in both the proteomic and metabolomic workflows. In the current study, an extension of an established direct inject nano-ESI-MS/MS method is described that utilizes the mass filtering capability of an ion-trap for ion packet separation into four narrow mass ranges (50 amu overlap with segment specific dynamic data dependent peak inclusion for MS/MS fragmentation (total acquisition time of 3 minutes. Comparison of this method with a more traditional nanoLC-MS/MS based protocol utilizing solvent/sample stream splitting to achieve nanoflow demonstrated comparable results for protein identification from polyacrylamide gel matrices. The advantages of this method include full automation, lack of cross-contamination, low cost, and high throughput.

  17. 75 FR 17158 - Chesapeake and Ohio Canal National Historical Park Advisory Commission; Notice of Public Meeting

    Science.gov (United States)

    2010-04-05

    ... members of the Commission are as follows: Mrs. Sheila Rabb Weidenfeld, Chairperson. Mr. Charles J. Weir... Kirkpatrick. Dr. George E. Lewis, Jr. Mr. Charles D. McElrath. Ms. Patricia Schooley. Mr. Jack Reeder. Ms. Merrily Pierce. Topics that will be presented during the meeting include: 1. Update on park operations. 2...

  18. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... Disease T Cells d What Causes MS? Disproved Theories Viruses Clusters d Who Gets MS? Pediatric MS ... times as often as men; in PPMS, the number of women and men are approximately equal. RRMS ...

  19. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... Living Well with MS Diet, Exercise & Healthy Behaviors Emotional Well-Being Spiritual Well-Being Cognitive Health Work, ... MS Anesthesia and Surgery Managing Your MS d Emotional Well-Being Mood Changes d Spiritual Well-Being ...

  20. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... Disease T Cells d What Causes MS? Disproved Theories Viruses Clusters d Who Gets MS? Pediatric MS ... of Distinction Lawry Circle Circle of Influence d Planned Giving d Other Ways to Give Donate by ...

  1. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... Trials in MS Wellness and Lifestyle Research Diet Vitamin D How and Why Do Scientists Share Results ... The National MS Society is Here to Help Need More Information? We Are Here Our MS Navigators ...

  2. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... Disease T Cells d What Causes MS? Disproved Theories Viruses Clusters d Who Gets MS? Pediatric MS ... Community at MSconnection.org Join a Local Support Group Peer Connections: One-on-One Edward M. Dowd ...

  3. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... Disease T Cells d What Causes MS? Disproved Theories Viruses Clusters d Who Gets MS? Pediatric MS ... Review of Society's Research Programs d Careers d Leadership Board of Directors Senior Leadership Team Founder Sylvia ...

  4. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... working effectively. How does RRMS differ from progressive types of MS? While RRMS is defined by attacks ... Pinterest MS Connection About the Society Vision Careers Leadership Cultural Values Financials News Press Room MS Prevalence ...

  5. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... Room Events at a Glance MS the Disease Public Service Announcements In the News Archives d MS ... For Professionals Researchers Physicians Nurses Rehabilitation Professionals Mental Health Professionals Health and Wellness Professionals What Is MS? ...

  6. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... Disproved Theories Viruses Clusters d Who Gets MS? Pediatric MS African Americans Hispanics & Latino/as d Multiple ... Questions to Ask d Resources for Specific Populations Pediatric MS Support Veterans with Multiple Sclerosis d Find ...

  7. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... Conditions to Rule Out For Clinicians Treating MS Comprehensive Care Find an MS Care Provider Medications Managing ... ADEM) d For Clinicians d Treating MS d Comprehensive Care Developing a Healthcare Team Make the Most ...

  8. Simultaneous analysis of 17 diuretics in dietary supplements by HPLC and LC-MS/MS.

    Science.gov (United States)

    Woo, H; Kim, J W; Han, K M; Lee, J H; Hwang, I S; Lee, J H; Kim, J; Kweon, S J; Cho, S; Chae, K R; Han, S Y; Kim, J

    2013-01-01

    In order to test health foods for illegally added diuretics for weight loss, we developed simple, rapid, selective, and sensitive methods using HPLC and LC-MS/MS for the simultaneous analysis of 17 diuretics in dietary supplements. HPLC conditions were set with a Capcell-pak C18, using a mobile phase consisting of gradient conditions, UV detection at 254 nm and validated for linearity (r(2)> 0.999), precision (CV ≤ 3%), recoveries (90.4-102.8%) and reproducibility. Identification and quantification of 17 diuretics were accomplished by ion-spray LC-MS/MS using multiple reaction monitoring (MRM). The chromatographic separation was carried out under the reversed-phase mechanism on an HSS-T3 column. The LC-MS/MS method was validated for linearity (r(2)> 0.99) and precision (CV Diuretics were not detected in all samples. Extraction recovery was also investigated and the extraction recoveries in different formulations were from 88% to 110% and from 81% to 116% using HPLC and LC-MS/MS, respectively. There was no significant difference in recoveries in the type of dietary supplements. Based on this result, the developed methods to monitor illegal drug adulterations in dietary supplements using HPLC and LC-MS/MS are simple, fast and reliable. Therefore, it is applicable to routine drug-adulteration screening.

  9. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... Viruses Clusters d Who Gets MS? Pediatric MS African Americans Hispanics & Latino/as d Multiple Sclerosis FAQs d ... Diet & Nutrition Exercise Heat & Temperature Sensitivity Sleep Vaccinations Women's Health Unhealthy Habits Managing MS and Another Condition ...

  10. MS-SQL data base programming

    Energy Technology Data Exchange (ETDEWEB)

    Noh, Chang Bae; Kim, Nam Jung; Lee, Hyeong Gyo

    2002-07-15

    This is about MS-SQL data base programming which is divided into thirteen chapters. The contents of this book are to understand MS-SQL 2000 DBMS with its composition, new function and history of MS-SQL, to learn conception of data base, install, run and closing of MS-SQL 2000 DBMS, to deal with the basic of MS-SQL DBMS, to handle the intermediate level of MS-SQL DBMS, to deal with MS-SQL DBMS in advanced level, to practice query like changing data base and checking of data lists, function on its use and data diff, get date, date add, char, upper and system function, set-up of MS-SQL ODBC, constructing of web server of windows 2000, web programming using visual studio.net.making board and making reference room.

  11. MS-SQL data base programming

    International Nuclear Information System (INIS)

    Noh, Chang Bae; Kim, Nam Jung; Lee, Hyeong Gyo

    2002-07-01

    This is about MS-SQL data base programming which is divided into thirteen chapters. The contents of this book are to understand MS-SQL 2000 DBMS with its composition, new function and history of MS-SQL, to learn conception of data base, install, run and closing of MS-SQL 2000 DBMS, to deal with the basic of MS-SQL DBMS, to handle the intermediate level of MS-SQL DBMS, to deal with MS-SQL DBMS in advanced level, to practice query like changing data base and checking of data lists, function on its use and data diff, get date, date add, char, upper and system function, set-up of MS-SQL ODBC, constructing of web server of windows 2000, web programming using visual studio.net.making board and making reference room.

  12. Analytical Method Details (MS): SE2_MS3 [Metabolonote[Archive

    Lifescience Database Archive (English)

    Full Text Available 00.0-1500.0); 2: ITMS + c norm !corona !pi Dep MS/MS Most intense ion from (1)., Rejected mass=284.2000;300.2000;328.2000;344.2000;372.2000;388.2000;416.3000;432.3000;460.0000. ...

  13. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... Treating MS d Comprehensive Care Developing a Healthcare Team Make the Most of Your Doctor Visits Advance Medical Directives d Find an MS Care Provider Partners in MS Care d Managing Relapses Plasmapheresis d Rehabilitation Functional Electrical Stimulation (FES) ...

  14. MS Based Metabonomics

    Energy Technology Data Exchange (ETDEWEB)

    Want, Elizabeth J.; Metz, Thomas O.

    2010-03-01

    Metabonomics is the latest and least mature of the systems biology triad, which also includes genomics and proteomics, and has its origins in the early orthomolecular medicine work pioneered by Linus Pauling and Arthur Robinson. It was defined by Nicholson and colleagues in 1999 as the quantitative measurement of perturbations in the metabolite complement of an integrated biological system in response to internal or external stimuli, and is often used today to describe many non-global types of metabolite analyses. Applications of metabonomics are extensive and include toxicology, nutrition, pharmaceutical research and development, physiological monitoring and disease diagnosis. For example, blood samples from millions of neonates are tested routinely by mass spectrometry (MS) as a diagnostic tool for inborn errors of metabolism. The metabonome encompasses a wide range of structurally diverse metabolites; therefore, no single analytical platform will be sufficient. Specialized sample preparation and detection techniques are required, and advances in NMR and MS technologies have led to enhanced metabonome coverage, which in turn demands improved data analysis approaches. The role of MS in metabonomics is still evolving as instrumentation and software becomes more sophisticated and as researchers realize the strengths and limitations of current technology. MS offers a wide dynamic range, high sensitivity, and reproducible, quantitative analysis. These attributes are essential for addressing the challenges of metabonomics, as the range of metabolite concentrations easily exceeds nine orders of magnitude in biofluids, and the diversity of molecular species ranges from simple amino and organic acids to lipids and complex carbohydrates. Additional challenges arise in generating a comprehensive metabolite profile, downstream data processing and analysis, and structural characterization of important metabolites. A typical workflow of MS-based metabonomics is shown in Figure

  15. LC-MS-MS identification of drug metabolites obtained by metalloporphyrin mediated oxidation

    Directory of Open Access Journals (Sweden)

    Maurin Andrea J. M.

    2003-01-01

    Full Text Available In this paper we report the application of liquid chromatography-mass spectrometry (LC-MS-MS to the identification of the products formed by oxidation of albendazole and disopyramide with metalloporphyrins in dichloroethane, using iodosylbenzene as an oxygen donor. Our results show that LC-MS-MS is a powerful tool to study the in vitro metabolism of drugs, allowing the identification of known and unknown metabolites. In addition, it was observed that the catalyst system used resulted in the formation of the same metabolites as obtained in vivo, although for disopyramide other products were also observed.

  16. DBS-LC-MS/MS assay for caffeine: validation and neonatal application.

    Science.gov (United States)

    Bruschettini, Matteo; Barco, Sebastiano; Romantsik, Olga; Risso, Francesco; Gennai, Iulian; Chinea, Benito; Ramenghi, Luca A; Tripodi, Gino; Cangemi, Giuliana

    2016-09-01

    DBS might be an appropriate microsampling technique for therapeutic drug monitoring of caffeine in infants. Nevertheless, its application presents several issues that still limit its use. This paper describes a validated DBS-LC-MS/MS method for caffeine. The results of the method validation showed an hematocrit dependence. In the analysis of 96 paired plasma and DBS clinical samples, caffeine levels measured in DBS were statistically significantly lower than in plasma but the observed differences were independent from hematocrit. These results clearly showed the need for extensive validation with real-life samples for DBS-based methods. DBS-LC-MS/MS can be considered to be a good alternative to traditional methods for therapeutic drug monitoring or PK studies in preterm infants.

  17. Two-year follow-up results for Hip-Hop to Health Jr.: a randomized controlled trial for overweight prevention in preschool minority children.

    Science.gov (United States)

    Fitzgibbon, Marian L; Stolley, Melinda R; Schiffer, Linda; Van Horn, Linda; KauferChristoffel, Katherine; Dyer, Alan

    2005-05-01

    To assess the impact of a culturally proficient dietary/physical activity intervention on changes in body mass index (BMI) (kg/m 2 ). Randomized controlled trial (Hip-Hop to Health Jr.) conducted between September 1999 and June 2002 in 12 Head Start preschool programs in Chicago, Illinois. Intervention children had significantly smaller increases in BMI compared with control children at 1-year follow-up, 0.06 vs 0.59 kg/m 2 ; difference -0.53 kg/m 2 (95% CI -0.91 to -0.14), P = .01; and at 2-year follow-up, 0.54 vs 1.08 kg/m 2 ; difference -0.54 kg/m 2 (95% CI -0.98 to -0.10), P = .02, with adjustment for baseline age and BMI. The only significant difference between intervention and control children in food intake/physical activity was the Year 1 difference in percent of calories from saturated fat, 11.6% vs 12.8% ( P = .002). Hip-Hop to Health Jr. was effective in reducing subsequent increases in BMI in preschool children. This represents a promising approach to prevention of overweight among minority children in the preschool years.

  18. Effects of hydrogen-charging on the properties of S235JR steel

    Science.gov (United States)

    Pietkun-Greber, Izabela

    2017-10-01

    The paper presents the test results of the S235JR steel susceptibility to damage under the influence of hydrogen. The test of mechanical properties was performed on the basis of a static stretch test of non-hydrogenated samples and after cathodic polarization. Electrochemical measurements for the assessment of corrosion resistance of non-hydrogenated and hydrogenated steels were carried out using open circuit potential measurement and registering of potentiodynamic polarization curves in a three-electrode measuring system. Hydrogenation was carried out for between 3 and 24 hours in a solution of 0.1 N sulfuric acid (VI) with the addition of 2 mg/dm 3 of arsenic oxide (III) at an electric current density of 10 mA/cm2. The hydrogen content in the steel before and after saturation with hydrogen was determined using the analyzer. Fracture samples after tensile test were observed using scanning electron microscope. The results of the research showed that as the hydrogen concentration in the examined steel increased (the lengthening of the saturation time), the deterioration of its mechanical and electrochemical properties occurred.

  19. MsLDR-creator: a web service to design msLDR assays.

    Science.gov (United States)

    Bormann, Felix; Dahl, Andreas; Sers, Christine

    2012-03-01

    MsLDR-creator is a free web service to design assays for the new DNA methylation detection method msLDR. The service provides the user with all necessary information about the oligonucleotides required for the measurement of a given CpG within a sequence of interest. The parameters are calculated by the nearest neighbour approach to achieve optimal behaviour during the experimental procedure. In addition, to guarantee a good start using msLDR, further information, like protocols and hints and tricks, are provided.

  20. 75 FR 4844 - Chesapeake and Ohio Canal National Historical Park Advisory Commission; Notice of Public Meeting

    Science.gov (United States)

    2010-01-29

    .... Mr. Charles J. Weir. Mr. Barry A. Passett. Mr. James G. McCleaf, II. Mr. John A. Ziegler. Mrs. Mary E.... Gilford. Brother James Kirkpatrick. Dr. George E. Lewis, Jr. Mr. Charles D. McElrath. Ms. Patricia Schooley. Mr. Jack Reeder. Ms. Merrily Pierce. Topics that will be presented during the meeting include: 1...

  1. 75 FR 41520 - Chesapeake and Ohio Canal National Historical Park Advisory Commission; Notice of Public Meeting

    Science.gov (United States)

    2010-07-16

    ... Rabb Weidenfeld, Chairperson Mr. Charles J. Weir Mr. Barry A. Passett Mr. James G. McCleaf II Mr. John... Reynolds Dr. James H. Gilford Brother James Kirkpatrick Dr. George E. Lewis, Jr. Mr. Charles D. McElrath Ms. Patricia Schooley Mr. Jack Reeder Ms. Merrily Pierce Topics that will be presented during the meeting...

  2. Analytical Method Details (MS): SE29_MS1 [Metabolonote[Archive

    Lifescience Database Archive (English)

    Full Text Available SE29_MS1 LC-FT-ICR-MS ESI positive method 1 Agilent1100 HPLC (Agilent), LTQ-FT (The... (100mg) are solved in 300uL 80% methanol solution. 20uL sample is injected into HPLC after 0.2um membrane filter treatment. HPLC

  3. ~ i t i d e r m a t o ~ h ~ t i c Activities of Nine (9) Essential Oils J.R. ...

    African Journals Online (AJOL)

    i t i d e r m a t o ~ h ~ t i c Activities of Nine (9) Essential Oils. J.R. KUIATE", S.P. KUATE'.~, N.E. KEMADJOU~, S. DJOKOUA~, F. ZIFACK~ AND J. ~. 0. ~. 0. ~. I Department of Biochemistry, FS, University of Dschang, P.O. Box 67 Dschang, Cameroon. 2~epartment of Biochemistry, FS, University of Yaoundt!, P.O. Box 812 ...

  4. contemporary christian spirituality: an “encompassing field”

    African Journals Online (AJOL)

    The spirit of the disciplines: Understanding how God changes lives. San Fran cisco: Harper. 1993. In search of guidance: Developing a conversational relationship with God. San Francisco: Harper. 1998. The divine conspiracy: Rediscovering our hidden life in God. London: Harper. Collins. Keywords. Trefwoorde. Spirituality.

  5. A comparison between DART-MS and DSA-MS in the forensic analysis of writing inks.

    Science.gov (United States)

    Drury, Nicholas; Ramotowski, Robert; Moini, Mehdi

    2018-05-23

    Ambient ionization mass spectrometry is gaining momentum in forensic science laboratories because of its high speed of analysis, minimal sample preparation, and information-rich results. One such application of ambient ionization methodology includes the analysis of writing inks from questioned documents where colorants of interest may not be soluble in common solvents, rendering thin layer chromatography (TLC) and separation-mass spectrometry methods such as LC/MS (-MS) impractical. Ambient ionization mass spectrometry uses a variety of ionization techniques such as penning ionization in Direct Analysis in Real Time (DART), and atmospheric pressure chemical ionization in Direct Sample Analysis (DSA), and electrospray ionization in Desorption Electrospray Ionization (DESI). In this manuscript, two of the commonly used ambient ionization techniques are compared: Perkin Elmer DSA-MS and IonSense DART in conjunction with a JEOL AccuTOF MS. Both technologies were equally successful in analyzing writing inks and produced similar spectra. DSA-MS produced less background signal likely because of its closed source configuration; however, the open source configuration of DART-MS provided more flexibility for sample positioning for optimum sensitivity and thereby allowing smaller piece of paper containing writing ink to be analyzed. Under these conditions, the minimum sample required for DART-MS was 1mm strokes of ink on paper, whereas DSA-MS required a minimum of 3mm. Moreover, both techniques showed comparable repeatability. Evaluation of the analytical figures of merit, including sensitivity, linear dynamic range, and repeatability, for DSA-MS and DART-MS analysis is provided. To the forensic context of the technique, DART-MS was applied to the analysis of United States Secret Service ink samples directly on a sampling mesh, and the results were compared with DSA-MS of the same inks on paper. Unlike analysis using separation mass spectrometry, which requires sample

  6. Natural isotope correction of MS/MS measurements for metabolomics and (13)C fluxomics.

    Science.gov (United States)

    Niedenführ, Sebastian; ten Pierick, Angela; van Dam, Patricia T N; Suarez-Mendez, Camilo A; Nöh, Katharina; Wahl, S Aljoscha

    2016-05-01

    Fluxomics and metabolomics are crucial tools for metabolic engineering and biomedical analysis to determine the in vivo cellular state. Especially, the application of (13)C isotopes allows comprehensive insights into the functional operation of cellular metabolism. Compared to single MS, tandem mass spectrometry (MS/MS) provides more detailed and accurate measurements of the metabolite enrichment patterns (tandem mass isotopomers), increasing the accuracy of metabolite concentration measurements and metabolic flux estimation. MS-type data from isotope labeling experiments is biased by naturally occurring stable isotopes (C, H, N, O, etc.). In particular, GC-MS(/MS) requires derivatization for the usually non-volatile intracellular metabolites introducing additional natural isotopes leading to measurements that do not directly represent the carbon labeling distribution. To make full use of LC- and GC-MS/MS mass isotopomer measurements, the influence of natural isotopes has to be eliminated (corrected). Our correction approach is analyzed for the two most common applications; (13)C fluxomics and isotope dilution mass spectrometry (IDMS) based metabolomics. Natural isotopes can have an impact on the calculated flux distribution which strongly depends on the substrate labeling and the actual flux distribution. Second, we show that in IDMS based metabolomics natural isotopes lead to underestimated concentrations that can and should be corrected with a nonlinear calibration. Our simulations indicate that the correction for natural abundance in isotope based fluxomics and quantitative metabolomics is essential for correct data interpretation. © 2015 Wiley Periodicals, Inc.

  7. Development and Validation of an LC-MS/MS Method and Comparison with a GC-MS Method to Measure Phenytoin in Human Brain Dialysate, Blood, and Saliva

    Directory of Open Access Journals (Sweden)

    Raphael Hösli

    2018-01-01

    Full Text Available Phenytoin (PHT is one of the most often used critical dose drugs, where insufficient or excessive dosing can have severe consequences such as seizures or toxicity. Thus, the monitoring and precise measuring of PHT concentrations in patients is crucial. This study develops and validates an LC-MS/MS method for the measurement of phenytoin concentrations in different body compartments (i.e., human brain dialysate, blood, and saliva and compares it with a formerly developed GC-MS method that measures PHT in the same biological matrices. The two methods are evaluated and compared based on their analytical performance, appropriateness to analyze human biological samples, including corresponding extraction and cleanup procedures, and their validation according to ISO 17025/FDA Guidance for Industry. The LC-MS/MS method showed a higher performance compared with the GC-MS method. The LC-MS/MS was more sensitive, needed a smaller sample volume (25 µL and less chemicals, was less time consuming (cleaning up, sample preparation, and analysis, and resulted in a better LOD ( 0.995 for all tested matrices (blood, saliva, and dialysate. For larger sample numbers as in pharmacokinetic/pharmacodynamic studies and for bedside as well as routine analyses, the LC-MS/MS method offers significant advantages over the GC-MS method.

  8. Structure Annotation and Quantification of Wheat Seed Oxidized Lipids by High-Resolution LC-MS/MS.

    Science.gov (United States)

    Riewe, David; Wiebach, Janine; Altmann, Thomas

    2017-10-01

    Lipid oxidation is a process ubiquitous in life, but the direct and comprehensive analysis of oxidized lipids has been limited by available analytical methods. We applied high-resolution liquid chromatography-mass spectrometry (LC-MS) and tandem mass spectrometry (MS/MS) to quantify oxidized lipids (glycerides, fatty acids, phospholipids, lysophospholipids, and galactolipids) and implemented a platform-independent high-throughput-amenable analysis pipeline for the high-confidence annotation and acyl composition analysis of oxidized lipids. Lipid contents of 90 different naturally aged wheat ( Triticum aestivum ) seed stocks were quantified in an untargeted high-resolution LC-MS experiment, resulting in 18,556 quantitative mass-to-charge ratio features. In a posthoc liquid chromatography-tandem mass spectrometry experiment, high-resolution MS/MS spectra (5 mD accuracy) were recorded for 8,957 out of 12,080 putatively monoisotopic features of the LC-MS data set. A total of 353 nonoxidized and 559 oxidized lipids with up to four additional oxygen atoms were annotated based on the accurate mass recordings (1.5 ppm tolerance) of the LC-MS data set and filtering procedures. MS/MS spectra available for 828 of these annotations were analyzed by translating experimentally known fragmentation rules of lipids into the fragmentation of oxidized lipids. This led to the identification of 259 nonoxidized and 365 oxidized lipids by both accurate mass and MS/MS spectra and to the determination of acyl compositions for 221 nonoxidized and 295 oxidized lipids. Analysis of 15-year aged wheat seeds revealed increased lipid oxidation and hydrolysis in seeds stored in ambient versus cold conditions. © 2017 The author(s). All Rights Reserved.

  9. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... and problems with cognition (learning and memory or information processing). People with progressive forms of MS are more likely to experience gradually worsening problems with walking and mobility, along with whatever other symptoms they may have. Diagnosing ... MS Society is Here to Help Need More Information? We Are Here Our MS Navigators help identify ...

  10. Hawaii Energy and Environmental Technologies (HEET) Initiative

    Science.gov (United States)

    2010-08-01

    Cell. Ind. Eng. Chem. Res. Vol. 46, 2007, pp. 734-744. Antal, Jr., M.J., Bourke , J., Manley-Harris, M., Fushimi, C, Dowaki, K., and Nunoura, T. "A...G., Jakab, E.; Bourke , J., Manley-Harris, M.; and Nunoura, T. "Do all carbonized charcoals have the same chemical structure? Implications of TG-MS...Antal, Jr., M.J., Varhegyi, G., Meszaros, E., Bourke , J., and Jakab, E. "Combustion Kinetics of Corncob Charcoal and Partially Demineralized Corncob

  11. 75 FR 65376 - Chesapeake and Ohio Canal National Historical Park Advisory Commission; Notice of Public Meeting

    Science.gov (United States)

    2010-10-22

    .... Charles J. Weir Mr. Barry A. Passett Mr. James G. McCleaf II Mr. John A. Ziegler Mrs. Mary E. Woodward Mrs... Kirkpatrick Dr. George E. Lewis, Jr. Mr. Charles D. McElrath Ms. Patricia Schooley Mr. Jack Reeder Ms. Merrily Pierce Topics that will be presented during the meeting include: 1. Update on park operations. 2. Update...

  12. Lynn White Jr. and the greening-of-religion hypothesis.

    Science.gov (United States)

    Taylor, Bron; Van Wieren, Gretel; Zaleha, Bernard Daley

    2016-10-01

    Lynn White Jr.'s "The Historical Roots of Our Ecologic Crisis," which was published in Science in 1967, has played a critical role in precipitating interdisciplinary environmental studies. Although White advances a multifaceted argument, most respondents focus on his claim that the Judeo-Christian tradition, especially Christianity, has promoted anthropocentric attitudes and environmentally destructive behaviors. Decades later, some scholars argue contrarily that Christianity in particular and the world's predominant religions in general are becoming more environmentally friendly, known as the greening-of-religion hypothesis. To test these claims, we conducted a comprehensive review of over 700 articles-historical, qualitative, and quantitative-that are pertinent to them. Although definitive conclusions are difficult, we identified many themes and dynamics that hinder environmental understanding and mobilization, including conservative theological orientations and beliefs about the role of divine agency in preventing or promoting natural events, whether the religion is an Abrahamic tradition or originated in Asia. On balance, we found the thrust of White's thesis is supported, whereas the greening-of-religion hypothesis is not. We also found that indigenous traditions often foster proenvironmental perceptions. This finding suggests that indigenous traditions may be more likely to be proenvironmental than other religious systems and that some nature-based cosmologies and value systems function similarly. Although we conclude White's thesis and subsequent claims are largely born out, additional research is needed to better understand under what circumstances and communication strategies religious or other individuals and groups may be more effectively mobilized to respond to contemporary environmental challenges. © 2016 Society for Conservation Biology.

  13. Determination of drug residues by CLAR-MS/MS in animal tissues

    International Nuclear Information System (INIS)

    Brenes Jimenez, Jose Eduardo

    2009-01-01

    Produced food of animal origin, present the possibility of occurrence of any contact with substances that have negative effects on the health of people who consume them. The use of drugs in veterinary medicine is one of the possible sources of such waste; so, the conditions for the analysis of some classes of antibiotics in animal tissues are based on the study. Costa Rica and the countries that are export destination, have regulation and programs for control before to be distributed in local markets, or post if it is received any complaint of pollution. The high resolution liquid chromatography coupled to mass spectrometers (CLAR-MS/MS) allows the analysis of analytes monitored, according to the specifications required by the legislation. The cases of two laboratories in Costa Rica are presented as the only ones who have the ability to perform the analysis of drug residues CLAR-MS/MS. (author) [es

  14. The Son's Fault: Martin Luther King, Jr.'s Search for and Recovery of Sonship.

    Science.gov (United States)

    Hinds, Jay-Paul

    2018-04-01

    This article examines the role of sonship in the psychological and spiritual development of men. In using the methodology of psychobiography, I explore the life history of Martin Luther King, Jr. to analyze his search for and recovery of sonship. I propose that sonship helps men rebel against and, in the end, overcome the feelings of inadequacy that are experienced in their struggles to achieve manhood, particularly within the father-son dyad. The scholarship of pastoral theologian Donald Capps is instructive in this regard, in that he suggests that sons should be allowed to search for a male figure, a father-substitute, who can affirm, not disdain or reject, this state of sonship. In the end, what is often viewed as a negative act of regression-i.e., the recovery of and return to sonship-is recognized instead as a positive one that assists a man in his journey toward wholeness.

  15. Metabolomic and elemental analysis of camel and bovine urine by GC-MS and ICP-MS.

    Science.gov (United States)

    Ahamad, Syed Rizwan; Alhaider, Abdul Qader; Raish, Mohammad; Shakeel, Faiyaz

    2017-01-01

    Recent studies from the author's laboratory indicated that camel urine possesses antiplatelet activity and anti-cancer activity which is not present in bovine urine. The objective of this study is to compare the volatile and elemental components of bovine and camel urine using GC-MS and ICP-MS analysis. We are interested to know the component that performs these biological activities. The freeze dried urine was dissolved in dichloromethane and then derivatization process followed by using BSTFA for GC-MS analysis. Thirty different compounds were analyzed by the derivatization process in full scan mode. For ICP-MS analysis twenty eight important elements were analyzed in both bovine and camel urine. The results of GC-MS and ICP-MS analysis showed marked difference in the urinary metabolites. GC-MS evaluation of camel urine finds a lot of products of metabolism like benzene propanoic acid derivatives, fatty acid derivatives, amino acid derivatives, sugars, prostaglandins and canavanine. Several research reports reveal the metabolomics studies on camel urine but none of them completely reported the pharmacology related metabolomics. The present data of GC-MS suggest and support the previous studies and activities related to camel urine.

  16. Application of LC–MS/MS for quantitative analysis of glucocorticoids and stimulants in biological fluids

    OpenAIRE

    Haneef, Jamshed; Shaharyar, Mohammad; Husain, Asif; Rashid, Mohd; Mishra, Ravinesh; Parveen, Shama; Ahmed, Niyaz; Pal, Manoj; Kumar, Deepak

    2013-01-01

    Liquid chromatography tandem mass chromatography (LCâMS/MS) is an important hyphenated technique for quantitative analysis of drugs in biological fluids. Because of high sensitivity and selectivity, LCâMS/MS has been used for pharmacokinetic studies, metabolites identification in the plasma and urine. This manuscript gives comprehensive analytical review, focusing on chromatographic separation approaches (column packing materials, column length and mobile phase) as well as different acquisiti...

  17. Application of LC–MS/MS for quantitative analysis of glucocorticoids and stimulants in biological fluids

    OpenAIRE

    Haneef, Jamshed; Shaharyar, Mohammad; Husain, Asif; Rashid, Mohd; Mishra, Ravinesh; Parveen, Shama; Ahmed, Niyaz; Pal, Manoj; Kumar, Deepak

    2013-01-01

    Liquid chromatography tandem mass chromatography (LC–MS/MS) is an important hyphenated technique for quantitative analysis of drugs in biological fluids. Because of high sensitivity and selectivity, LC–MS/MS has been used for pharmacokinetic studies, metabolites identification in the plasma and urine. This manuscript gives comprehensive analytical review, focusing on chromatographic separation approaches (column packing materials, column length and mobile phase) as well as different acquisiti...

  18. Study of T L LiF: Mg,Ti (Model JR1152C) material for its use in the environmental monitoring

    International Nuclear Information System (INIS)

    Molina P, D.; Diaz B, E.; Prendes A, M.

    1999-01-01

    In order to evaluate the possibility to use the T L material of LiF: Mg,Ti (Model JR1152C) as environmental dosemeter it was realized its characterization of it according to the established criterion in the standard IEC-1066. The properties studied were: homogeneity of the lot, reproducibility, response linearity, detection threshold, auto irradiation, residual signal, response pride (fading) and angular dependence. The results prove the compliment of the IEC requirements and therefore the applicability of this dosemeter in the environmental monitoring. (Author)

  19. Improved LC-MS/MS method for the quantification of hepcidin-25 in clinical samples.

    Science.gov (United States)

    Abbas, Ioana M; Hoffmann, Holger; Montes-Bayón, María; Weller, Michael G

    2018-06-01

    Mass spectrometry-based methods play a crucial role in the quantification of the main iron metabolism regulator hepcidin by singling out the bioactive 25-residue peptide from the other naturally occurring N-truncated isoforms (hepcidin-20, -22, -24), which seem to be inactive in iron homeostasis. However, several difficulties arise in the MS analysis of hepcidin due to the "sticky" character of the peptide and the lack of suitable standards. Here, we propose the use of amino- and fluoro-silanized autosampler vials to reduce hepcidin interaction to laboratory glassware surfaces after testing several types of vials for the preparation of stock solutions and serum samples for isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS). Furthermore, we have investigated two sample preparation strategies and two chromatographic separation conditions with the aim of developing a LC-MS/MS method for the sensitive and reliable quantification of hepcidin-25 in serum samples. A chromatographic separation based on usual acidic mobile phases was compared with a novel approach involving the separation of hepcidin-25 with solvents at high pH containing 0.1% of ammonia. Both methods were applied to clinical samples in an intra-laboratory comparison of two LC-MS/MS methods using the same hepcidin-25 calibrators with good correlation of the results. Finally, we recommend a LC-MS/MS-based quantification method with a dynamic range of 0.5-40 μg/L for the assessment of hepcidin-25 in human serum that uses TFA-based mobile phases and silanized glass vials. Graphical abstract Structure of hepcidin-25 (Protein Data Bank, PDB ID 2KEF).

  20. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... Clinicians Publications for Your Patients MS Navigator Program Programs and Services for Your Patients Contact Us Clinical Fellows ... Relapsing-remitting MS (RRMS) Relapsing-remitting ...

  1. The EIPeptiDi tool: enhancing peptide discovery in ICAT-based LC MS/MS experiments

    Directory of Open Access Journals (Sweden)

    Tradigo Giuseppe

    2007-07-01

    Full Text Available Abstract Background Isotope-coded affinity tags (ICAT is a method for quantitative proteomics based on differential isotopic labeling, sample digestion and mass spectrometry (MS. The method allows the identification and relative quantification of proteins present in two samples and consists of the following phases. First, cysteine residues are either labeled using the ICAT Light or ICAT Heavy reagent (having identical chemical properties but different masses. Then, after whole sample digestion, the labeled peptides are captured selectively using the biotin tag contained in both ICAT reagents. Finally, the simplified peptide mixture is analyzed by nanoscale liquid chromatography-tandem mass spectrometry (LC-MS/MS. Nevertheless, the ICAT LC-MS/MS method still suffers from insufficient sample-to-sample reproducibility on peptide identification. In particular, the number and the type of peptides identified in different experiments can vary considerably and, thus, the statistical (comparative analysis of sample sets is very challenging. Low information overlap at the peptide and, consequently, at the protein level, is very detrimental in situations where the number of samples to be analyzed is high. Results We designed a method for improving the data processing and peptide identification in sample sets subjected to ICAT labeling and LC-MS/MS analysis, based on cross validating MS/MS results. Such a method has been implemented in a tool, called EIPeptiDi, which boosts the ICAT data analysis software improving peptide identification throughout the input data set. Heavy/Light (H/L pairs quantified but not identified by the MS/MS routine, are assigned to peptide sequences identified in other samples, by using similarity criteria based on chromatographic retention time and Heavy/Light mass attributes. EIPeptiDi significantly improves the number of identified peptides per sample, proving that the proposed method has a considerable impact on the protein

  2. Isotope ratio monitoring LC/MS (IRM-LC/MS): new applications

    International Nuclear Information System (INIS)

    Juchelka, D; Hilkert, A.; Krummen, M.

    2005-01-01

    With the introduction of compound specific isotope analysis by isotope ratio monitoring GC/ MS (IRM-GC/MS) the immediate demand for similar applications using HPLC was created. Many compounds of biological, medical, pharmaceutical and environmental interest are not volatile or too polar. Consequently, they cannot be directly analyzed by gas chromatography. In IRM-GC/MS the carrier is helium, which does not interfere with the essential combust ion step prior to isotope ratio mass spectrometry (IRMS). In opposite the LC mobile phase has inhibited a similar direct conversion up to now. All earlier IRM-LC/MS approaches were based on the removal of the liquid phase prior to combustion risking fractionation of the isotope ratios of the eluted compounds. To avoid such restrictions we developed a new continuous flow concept for the coupling of an HPLC system to the isotope ratio MS for 13 C/ 12C isotope ratio analysis. In the Finnigan LC IsoLink, the liquid phase is not removed from the sample prior to oxidation. The sample is oxidized still in the mobile phase followed by on-line separation of the CO 2 from the liquid phase and transfer into the isotope ratio MS. Therefore, this strategy is based on water and inorganic buffers as mobile phase. The new approach opens up a whole new world in the application of gas isotope ratio mass spectrometry. The 13 C/ 12 C ratio s of organic acids, amino acids, carbohydrates and nucleotides can now be measured. These components typically within a complex matrix are separated by liquid chromatography followed by on-line determination of the isotope ratios. The draw backs of using derivatization and off-line preparation procedures can now be over come. This new technique allow s studying biochemical cycles, running tracer experiments and determining the origin of components. Applications from different scientific areas such as biogeochemistry, molecular biology, and pharmacy as well as authenticity control o f foods will be presented

  3. Ms. Mentor Unmasked

    Science.gov (United States)

    Krebs, Paula

    2008-01-01

    This article presents an interview with Emily Toth, who writes the monthly "Ms. Mentor" academic advice column in the "Chronicle of Higher Education" and teaches in the English department at Louisiana State University, in Baton Rouge. She is the author of "Ms. Mentor's Impeccable Advice for Women in Academia" (1997), "Inside Peyton Place: The Life…

  4. Relapsing-Remitting MS (RRMS)

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  5. Lung Cancer Serum Biomarker Discovery Using Label Free LC-MS/MS

    Science.gov (United States)

    Zeng, Xuemei; Hood, Brian L.; Zhao, Ting; Conrads, Thomas P.; Sun, Mai; Gopalakrishnan, Vanathi; Grover, Himanshu; Day, Roger S.; Weissfeld, Joel L.; Wilson, David O.; Siegfried, Jill M.; Bigbee, William L.

    2011-01-01

    Introduction Lung cancer remains the leading cause of cancer-related death with poor survival due to the late stage at which lung cancer is typically diagnosed. Given the clinical burden from lung cancer, and the relatively favorable survival associated with early stage lung cancer, biomarkers for early detection of lung cancer are of important potential clinical benefit. Methods We performed a global lung cancer serum biomarker discovery study using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in a set of pooled non-small cell lung cancer (NSCLC) case sera and matched controls. Immunoaffinity subtraction was used to deplete the top most abundant serum proteins; the remaining serum proteins were subjected to trypsin digestion and analyzed in triplicate by LC-MS/MS. The tandem mass spectrum data were searched against the human proteome database and the resultant spectral counting data were used to estimate the relative abundance of proteins across the case/control serum pools. The spectral counting derived abundances of some candidate biomarker proteins were confirmed with multiple reaction monitoring MS assays. Results A list of 49 differentially abundant candidate proteins was compiled by applying a negative binomial regression model to the spectral counting data (pbiomarkers with statistically significant differential abundance across the lung cancer case/control pools which, when validated, could improve lung cancer early detection. PMID:21304412

  6. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... Treating MS Comprehensive Care Find an MS Care Provider Medications Managing Relapses Rehabilitation Complementary & Alternative Medicines For Clinicians Resources & Support Library & Education Programs Find Support Advanced Care ...

  7. Progressive-Relapsing MS (PRMS)

    Science.gov (United States)

    ... Is MS? Types of MS Share this page Facebook Twitter Email ... multiple sclerosis (PRMS) was described in the 1996 disease-course definitions as — steadily worsening neurologic function from the beginning ...

  8. EPA CRL MS014: Analysis of Aldicarb, Bromadiolone, Carbofuran, Oxamyl and Methomyl in Water by Multiple Reaction Monitoring Liquid Chromatography / Tandem Mass Spectrometry (LC/MS/MS)

    Science.gov (United States)

    Method MS014 describes procedures for solvent extraction of aldicarb, bromadiolone, carbofuran, oxamyl and methomyl from water samples, followed by analysis using liquid chromatography tandem mass spectrometry (LC-MS-MS).

  9. General Charles F. Bolden, Jr. and Professor Claude Nicollier reunite during visit to CERN

    CERN Multimedia

    Jordan Juras

    2011-01-01

    Thursday 23 June, CERN saw an unlikely and much savoured meeting between two old colleagues and friends: General Charles F. Bolden, Jr. and Professor Claude Nicollier.   Bolden and Nicollier were separately invited to CERN for different reasons - Charles Bolden had been invited by Professor Samuel Ting to visit the newly built and now fully operational Payload Operation and Control Centre of the AMS collaboration and Claude Nicollier had been invited by the Theory Department to give a colloquium. They were delightfully surprised when they met at the entrance of the main building. Bolden and Nicollier served together in the Space Shuttle Program and were trained by NASA during the 1980’s where they became close friends. On 24 April, 1990, Bolden piloted the Space Shuttle Discovery into orbit with the Hubble telescope in the payload bay. Though Nicollier did not accompany Bolden during the Hubble launch, he did return to the telescope 3 years later on board the Space Shuttle Ende...

  10. Application of LC–MS/MS for quantitative analysis of glucocorticoids and stimulants in biological fluids

    Directory of Open Access Journals (Sweden)

    Jamshed Haneef

    2013-10-01

    Full Text Available Liquid chromatography tandem mass chromatography (LC–MS/MS is an important hyphenated technique for quantitative analysis of drugs in biological fluids. Because of high sensitivity and selectivity, LC–MS/MS has been used for pharmacokinetic studies, metabolites identification in the plasma and urine. This manuscript gives comprehensive analytical review, focusing on chromatographic separation approaches (column packing materials, column length and mobile phase as well as different acquisition modes (SIM, MRM for quantitative analysis of glucocorticoids and stimulants. This review is not meant to be exhaustive but rather to provide a general overview for detection and confirmation of target drugs using LC–MS/MS and thus useful in the doping analysis, toxicological studies as well as in pharmaceutical analysis. Keywords: LC–MS/MS, Ionization techniques, Glucocorticoids, Stimulants, Hyphenated techniques, Biological fluid

  11. Periodization of the urban interventions: a review of ratings from “Vargas & Castilho”, “Boyer” and “Simões Jr.”

    Directory of Open Access Journals (Sweden)

    Geise Brizotti Pasquotto

    2010-09-01

    Full Text Available The present paper aims to compare the periods proposed by three authors “Vargas e Castilho” (2006, “Boyer” (1998 and “Simões Jr.” (1994. They did it to identify four significant moments of intervention in urban space from the period of modernity. It is noteworthy that, in this comparison, the most important thing is not to define a concept, but understanding the process and the paradigms that underpin each of these interventions.

  12. MS Windows domēna darbstacijas migrācijas iespējas no MS Windows XP uz MS Windows 7.

    OpenAIRE

    Zariņš, Valdis

    2009-01-01

    Kvalifikācijas darbā tiek aprakstītas MS Windows domēna darbstacijas migrācijas iespējas no MS Windows XP uz MS Windows 7, kā servera operētājsistēmas izmantojot tādus Microsoft produktus, kā Microsoft Windows Server 2003 un Microsoft Windows Server 2008. Kvalifikācijas darba teorētiskaja daļā tiek apskatīti Microsoft Windows 7 priekšrocības un uzlabojumus gan no darbstacijas lietotāja , gan no darbstacijas administratora puses. Ir aprakstītas Microsoft Windows Server 2008 jauninājumu ie...

  13. Os dilemas do marxismo latino-americano nas obras de Caio Prado Jr. e José Carlos Mariátegui

    OpenAIRE

    Kaysel, André

    2012-01-01

    O objetivo deste artigo é comparar a relação entre o marxismo e a questão nacional nas obras do historiador brasileiro Caio Prado Jr. e do jornalista e militante peruano José Carlos Mariátegui. Parto da hipótese de que ambos compartilham uma leitura análoga da questão nacional, entendida como formação inconclusa da nação, obstaculizada pela persistência do legado colonial. Para tanto, discuto as proximidades e as discrepâncias entre os dois autores por meio de um cotejo de suas obras em torno...

  14. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... Contact Us Newly Diagnosed If you or somone close to you has recently been diagnosed, access our MS information and resources. Start ... Room MS Prevalence Charitable Ratings Corporate Support Helpful Links ...

  15. MS in Your Relationships

    Science.gov (United States)

    ... MS Relationships Share this page Facebook Twitter Email Relationships MS poses additional challenges, but it also enriches ... when it is not. Keeping balance in your relationship When one person in a couple is affected ...

  16. Single-cell analysis by ICP-MS/MS as a fast tool for cellular bioavailability studies of arsenite.

    Science.gov (United States)

    Meyer, S; López-Serrano, A; Mitze, H; Jakubowski, N; Schwerdtle, T

    2018-01-24

    Single-cell inductively coupled plasma mass spectrometry (SC-ICP-MS) has become a powerful and fast tool to evaluate the elemental composition at a single-cell level. In this study, the cellular bioavailability of arsenite (incubation of 25 and 50 μM for 0-48 h) has been successfully assessed by SC-ICP-MS/MS for the first time directly after re-suspending the cells in water. This procedure avoids the normally arising cell membrane permeabilization caused by cell fixation methods (e.g. methanol fixation). The reliability and feasibility of this SC-ICP-MS/MS approach with a limit of detection of 0.35 fg per cell was validated by conventional bulk ICP-MS/MS analysis after cell digestion and parallel measurement of sulfur and phosphorus.

  17. An impulse-driven liquid-droplet deposition interface for combining LC with MALDI MS and MS/MS.

    Science.gov (United States)

    Young, J Bryce; Li, Liang

    2006-03-01

    A simple and robust impulse-driven droplet deposition system was developed for off-line liquid chromatography matrix-assisted laser desorption ionization mass spectrometry (LC-MALDI MS). The system uses a solenoid operated with a pulsed voltage power supply to generate impulses that dislodge the hanging droplets from the LC outlet directly to a MALDI plate via a momentum transfer process. There is no contact between the LC outlet and the collection surface. The system is compatible with solvents of varying polarity and viscosity, and accommodates the use of hydrophobic and hydrophilic MALDI matrices. MALDI spots are produced on-line with the separation, and do not require further processing before MS analysis. It is shown that high quality MALDI spectra from 5 fmol of pyro-Glu-fibrinopeptide deposition after LC separation could be obtained using the device, indicating that there was no sample loss in the interface. To demonstrate the analytical performance of the system as a proteome analysis tool, a range of BSA digest concentrations covering about 3 orders of magnitude, from 5 fmol to 1 pmol, were analyzed by LC-MALDI quadrupole time-of-flight MS, yielding 6 and 57% amino acid sequence coverage, respectively. In addition, a complex protein mixture of an E. coli cell extract was tryptically digested and analyzed by LC-MALDI MS, resulting in the detection of a total of 409 unique peptides from 100 fractions of 15-s intervals.

  18. SWATH Mass Spectrometry Performance Using Extended Peptide MS/MS Assay Libraries*

    Science.gov (United States)

    Wu, Jemma X.; Song, Xiaomin; Pascovici, Dana; Zaw, Thiri; Care, Natasha; Krisp, Christoph; Molloy, Mark P.

    2016-01-01

    The use of data-independent acquisition methods such as SWATH for mass spectrometry based proteomics is usually performed with peptide MS/MS assay libraries which enable identification and quantitation of peptide peak areas. Reference assay libraries can be generated locally through information dependent acquisition, or obtained from community data repositories for commonly studied organisms. However, there have been no studies performed to systematically evaluate how locally generated or repository-based assay libraries affect SWATH performance for proteomic studies. To undertake this analysis, we developed a software workflow, SwathXtend, which generates extended peptide assay libraries by integration with a local seed library and delivers statistical analysis of SWATH-quantitative comparisons. We designed test samples using peptides from a yeast extract spiked into peptides from human K562 cell lysates at three different ratios to simulate protein abundance change comparisons. SWATH-MS performance was assessed using local and external assay libraries of varying complexities and proteome compositions. These experiments demonstrated that local seed libraries integrated with external assay libraries achieve better performance than local assay libraries alone, in terms of the number of identified peptides and proteins and the specificity to detect differentially abundant proteins. Our findings show that the performance of extended assay libraries is influenced by the MS/MS feature similarity of the seed and external libraries, while statistical analysis using multiple testing corrections increases the statistical rigor needed when searching against large extended assay libraries. PMID:27161445

  19. LC-MS/MS Peptide Mapping with Automated Data Processing for Routine Profiling of N-Glycans in Immunoglobulins

    Science.gov (United States)

    Shah, Bhavana; Jiang, Xinzhao Grace; Chen, Louise; Zhang, Zhongqi

    2014-06-01

    Protein N-Glycan analysis is traditionally performed by high pH anion exchange chromatography (HPAEC), reversed phase liquid chromatography (RPLC), or hydrophilic interaction liquid chromatography (HILIC) on fluorescence-labeled glycans enzymatically released from the glycoprotein. These methods require time-consuming sample preparations and do not provide site-specific glycosylation information. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) peptide mapping is frequently used for protein structural characterization and, as a bonus, can potentially provide glycan profile on each individual glycosylation site. In this work, a recently developed glycopeptide fragmentation model was used for automated identification, based on their MS/MS, of N-glycopeptides from proteolytic digestion of monoclonal antibodies (mAbs). Experimental conditions were optimized to achieve accurate profiling of glycoforms. Glycan profiles obtained from LC-MS/MS peptide mapping were compared with those obtained from HPAEC, RPLC, and HILIC analyses of released glycans for several mAb molecules. Accuracy, reproducibility, and linearity of the LC-MS/MS peptide mapping method for glycan profiling were evaluated. The LC-MS/MS peptide mapping method with fully automated data analysis requires less sample preparation, provides site-specific information, and may serve as an alternative method for routine profiling of N-glycans on immunoglobulins as well as other glycoproteins with simple N-glycans.

  20. Investigation of enrofloxacin residues in broiler tissues using ELISA and LC-MS/MS.

    Science.gov (United States)

    Panzenhagen, Pedro Henrique N; Aguiar, Waldemir S; Gouvêa, Raquel; de Oliveira, Andréa M G; Barreto, Fabiano; Pereira, Virgínia L A; Aquino, Maria Helena C

    2016-01-01

    This study investigated the efficiency of an enrofloxacin ELISA test kit to detect the presence of enrofloxacin residues in broiler tissues compared with LC-MS/MS. Broiler tissues from 72 samples consisting of 60 breast muscle, six pools of livers (500 g each) and six pools of kidneys (500 g each) were obtained from six different slaughterhouses. Breast muscle from 10 carcasses and pools of livers and kidneys from approximately 200 carcasses of the same flock were collected from each slaughterhouse. ELISA and HPLC were used to identify and quantify the contamination of the samples with enrofloxacin. A total of 72% of the analysed samples contained enrofloxacin residues detected by the ELISA and 22.2% were detected by LC-MS/MS. The mean values of enrofloxacin contamination found in chicken breast by ELISA and HPLC were 8.63 and 12.25 μg kg(-1), respectively. None of the samples exceeded the maximum limit of 100 μg kg(-1) by both methods set by the European Union as well as the Brazilian Agriculture Ministry. All positive samples for enrofloxacin residues detected by LC-MS/MS were also positive by ELISA. These data confirm the efficiency of the ELISA test, and suggest its use as a screening method for enrofloxacin residues in poultry tissues due to its quick results, low price and ease of applicability.

  1. Relationship between plasma and salivary melatonin and cortisol investigated by LC-MS/MS.

    Science.gov (United States)

    van Faassen, Martijn; Bischoff, Rainer; Kema, Ido P

    2017-08-28

    Disturbance of the circadian rhythm has been associated with disease states, such as metabolic disorders, depression and cancer. Quantification of the circadian markers such as melatonin and cortisol critically depend on reliable and reproducible analytical methods. Previously, melatonin and cortisol were primarily analyzed separately, mainly using immunoassays. Here we describe the validation and application of a high-throughput liquid chromatography in combination with mass spectrometry (LC-MS/MS) method for the combined analysis of melatonin and cortisol in plasma and saliva. The LC-MS/MS method was validated according to international validation guidelines. We used this method to analyze total plasma, free plasma (as obtained by equilibrium dialysis) and saliva melatonin and cortisol in healthy adults. Validation results for plasma and saliva melatonin and cortisol were well within the international validation criteria. We observed no difference between saliva collected by passive drooling or Salivette. Moreover, we noted a significant difference in saliva vs. free plasma melatonin. We observed on average 36% (95% CI: 4%-60%) higher salivary melatonin levels in comparison to free plasma melatonin, suggestive of local production of melatonin in the salivary glands. The novel outcome of this study is probably due to the high precision of our LC-MS/MS assay. These outcomes illustrate the added value of accurate and sensitive mass spectrometry based methods for the quantification of neuroendocrine biomarkers.

  2. Analytical methods for multiresidue determination of sulfonamides and trimethoprim in meat and ground water samples by CE-MS and CE-MS/MS.

    Science.gov (United States)

    Soto-Chinchilla, Jorge J; García-Campaña, Ana M; Gámiz-Gracia, Laura

    2007-11-01

    This paper presents two methods based on CZE-MS detection and CZE-MS/MS detection developed for the multiresidue determination of ten sulfonamides (sulfapyridine, sulfadoxin, sulfamethazine, sulfadimethoxine, sulfameter, sulfamerazine, sulfachlorpyridazine, sulfadiazine, sulfamethoxazole, and sulfamethizole) and a potentiator, trimethoprim (TMP), whose contents are regulated by the EU Council Regulation no. 2377/90 in animal edible tissues. Experimental designs were employed to optimize the electrospray conditions. MS/MS experiments using an IT as analyzer operating in multiple reaction monitoring (MRM) mode were carried out to achieve the minimum number of points according to the 2002/657/EC European Decision for unambiguous identification. The proposed procedures have been compared in terms of the performance characteristics and trueness. The limits of detection and quantification were in all cases lower than the maximum residue limits legislated for these compounds and the recoveries were satisfactory, being possible the application for their monitoring in foodstuff of animal origin and in environmental samples, allowing the determination of sulfonamides and TMP residues in meat and in superficial water in the low microg/L range.

  3. Cross-validated stable-isotope dilution GC-MS and LC-MS/MS assays for monoacylglycerol lipase (MAGL) activity by measuring arachidonic acid released from the endocannabinoid 2-arachidonoyl glycerol.

    Science.gov (United States)

    Kayacelebi, Arslan Arinc; Schauerte, Celina; Kling, Katharina; Herbers, Jan; Beckmann, Bibiana; Engeli, Stefan; Jordan, Jens; Zoerner, Alexander A; Tsikas, Dimitrios

    2017-03-15

    2-Arachidonoyl glycerol (2AG) is an endocannabinoid that activates cannabinoid (CB) receptors CB1 and CB2. Monoacylglycerol lipase (MAGL) inactivates 2AG through hydrolysis to arachidonic acid (AA) and glycerol, thus modulating the activity at CB receptors. In the brain, AA released from 2AG by the action of MAGL serves as a substrate for cyclooxygenases which produce pro-inflammatory prostaglandins. Here we report stable-isotope GC-MS and LC-MS/MS assays for the reliable measurement of MAGL activity. The assays utilize deuterium-labeled 2AG (d 8 -2AG; 10μM) as the MAGL substrate and measure deuterium-labeled AA (d 8 -AA; range 0-1μM) as the MAGL product. Unlabelled AA (d 0 -AA, 1μM) serves as the internal standard. d 8 -AA and d 0 -AA are extracted from the aqueous buffered incubation mixtures by ethyl acetate. Upon solvent evaporation the residue is reconstituted in the mobile phase prior to LC-MS/MS analysis or in anhydrous acetonitrile for GC-MS analysis. LC-MS/MS analysis is performed in the negative electrospray ionization mode by selected-reaction monitoring the mass transitions [M-H] - →[M-H - CO 2 ] - , i.e., m/z 311→m/z 267 for d 8 -AA and m/z 303→m/z 259 for d 0 -AA. Prior to GC-MS analysis d 8 -AA and d 0 -AA were converted to their pentafluorobenzyl (PFB) esters by means of PFB-Br. GC-MS analysis is performed in the electron-capture negative-ion chemical ionization mode by selected-ion monitoring the ions [M-PFB] - , i.e., m/z 311 for d 8 -AA and m/z 303 for d 0 -AA. The GC-MS and LC-MS/MS assays were cross-validated. Linear regression analysis between the concentration (range, 0-1μM) of d 8 -AA measured by LC-MS/MS (y) and that by GC-MS (x) revealed a straight line (r 2 =0.9848) with the regression equation y=0.003+0.898x, indicating a good agreement. In dog liver, we detected MAGL activity that was inhibitable by the MAGL inhibitor JZL-184. Exogenous eicosatetraynoic acid is suitable as internal standard for the quantitative determination

  4. The potential use of complex derivatization procedures in comprehensive HPLC-MS/MS detection of anabolic steroids.

    Science.gov (United States)

    Baranov, Pavel A; Appolonova, Svetlana A; Rodchenkov, Grigory M

    2010-10-01

    The use of two separate derivatization procedures with the formation of oxime (hydroxyl ammonium pretreatment) and picolinoyl (mixed anhydride method) derivates of anabolic steroids following HPLC-MS/MS analysis was proposed. The main product ions of obtained derivatives for 21 anabolic steroids were evaluated and fragmentation pathways were compared.The analysis of MS/MS spectra for underivatized steroids versus oxime or picolinoyl derivatives showed that in case of analytes containing conjugated double bonds in sterane core all of the observed MS/MS spectra contained abundant product ions of diagnostic value. The implementation of derivatization procedures to such compounds is useful for upgrading sensitivity or selectivity of the evaluated method. On the other hand, MS/MS spectra of underivatized and oxime analytes without conjugated double bonds in sterane core produce spectra with large amounts of low abundant product ions. Picolinoyl derivatives formation leads to highly specific spectra with product ions of diagnostic value coupled with sensitive and selective analysis at the same time. The intra- and inter-group comparison analysis revealed that fragmentation pathways for underivatized steroids and correspondent oxime derivatives are similar.The obtained oxime and picolinoyl derivatives provided 10-15 times higher ESI response in the HPLC-ESI-MS-selected reaction monitoring (SRM) when compared to those of underivatized molecules in positive HPLC-ESI-MS mode.Due to the laborious sample preparation we suggest to use the performed strategy for confirmation analysis purposes, metabolic studies or while the identification of new steroids or steroid-like substances. Copyright © 2010 John Wiley & Sons, Ltd.

  5. ESI MS/MS Study of Calix[4]arene Derivatives and their Metal Complexes

    OpenAIRE

    Benković, Tomislav; Tomišić, Vladislav; Frkanec, Leo; Galić, Nives

    2012-01-01

    The peptidocalixarenes 1–3 bearing tryptophan, phenylglycine and leucil units at the lower rim and their complexes with alkali-metal (Li+, Na+, K+, Rb+, Cs+) and selected lanthanide cations (La3+, Ce3+, Eu3+, Yb3+) were analyzed by ESI MS. The influences of the solvent (acetonitrile, methanol, addition of formic acid or sodium acetate) and the calixarene:cation molar ratio on signal intensities were investigated. Comprehensive MS/MS analyses were performed of all singly and doubly charged ion...

  6. Relapsing-Remitting MS (RRMS)

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  7. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... Events Living Well with MS Diet, Exercise & Healthy Behaviors Emotional Well-Being Spiritual Well-Being Cognitive Health ... Living Well with MS d Diet, Exercise & Healthy Behaviors Diet & Nutrition Exercise Heat & Temperature Sensitivity Sleep Vaccinations ...

  8. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... Rule Out For Clinicians Treating MS Comprehensive Care Find an MS Care Provider Medications Managing Relapses Rehabilitation ... Medicines For Clinicians Resources & Support Library & Education Programs Find Support Advanced Care Needs Resources for Specific Populations ...

  9. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... bowel and bladder problems, and problems with cognition (learning and memory or information processing). People with progressive ... More The National MS Society is Here to Help Need More Information? We Are Here Our MS ...

  10. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... of Programs and Events Living Well with MS Diet, Exercise & Healthy Behaviors Emotional Well-Being Spiritual Well- ... and Events d Living Well with MS d Diet, Exercise & Healthy Behaviors Diet & Nutrition Exercise Heat & Temperature ...

  11. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... d Spiritual Well-Being Building Spirituality into Your Life d Cognitive Health d Work, Home & Leisure Employment ... Partnership Opportunities d Personal Stories Ambassadors & Familiar Faces Life with MS Givers Shakers Families with MS Seekers ...

  12. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... Brochure Working with MS (.pdf) Download Brochure Taming Stress (.pdf) Download Brochure Multiple Sclerosis and Your Emotions (. ... For Professionals Researchers Physicians Nurses Rehabilitation Professionals Mental Health Professionals Health and Wellness Professionals What Is MS? ...

  13. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... Online d Give in Honor or Memory d Workplace Giving d Employer Matching Gifts d Gifts of ... Living with MS (.pdf) Download Brochure Focus on Employment (.pdf) Download Brochure Working with MS (.pdf) Download ...

  14. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... Life d Cognitive Health d Work, Home & Leisure Employment Insurance & Financial Information Staying Mobile Reclaiming Control Accessibility ... Living with MS (.pdf) Download Brochure Focus on Employment (.pdf) Download Brochure Working with MS (.pdf) Download ...

  15. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... working effectively. How does RRMS differ from progressive types of MS? While RRMS is defined by attacks ... forms of MS involve much less of this type of inflammation. People with RRMS tend to have ...

  16. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... attacks of inflammation (relapses) in the CNS, progressive forms of MS involve much less of this type ... and memory or information processing). People with progressive forms of MS are more likely to experience gradually ...

  17. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... Associated Myelopathy (HAM) Neuromyelitis Optica (NMO) Schilder's Disease Transverse Myelitis d Symptoms & Diagnosis d Diagnosing MS d ... Overview (.pdf) Download Document Pediatric MS Learn More Transverse Myelitis Learn More Neuromyelitis Optica (NMO) Learn More ...

  18. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... Directors Senior Leadership Team Founder Sylvia Lawry d Cultural Values d Financials Annual Reports Sources of Support ... MS Connection About the Society Vision Careers Leadership Cultural Values Financials News Press Room MS Prevalence Charitable ...

  19. Hip-Hop to Health Jr. Randomized Effectiveness Trial

    Science.gov (United States)

    Kong, Angela; Buscemi, Joanna; Stolley, Melinda R.; Schiffer, Linda A.; Kim, Yoonsang; Braunschweig, Carol L.; Gomez-Perez, Sandra L.; Blumstein, Lara B.; Van Horn, Linda; Dyer, Alan R.; Fitzgibbon, Marian L.

    2015-01-01

    Introduction The preschool years provide a unique window of opportunity to intervene on obesity-related lifestyle risk factors during the formative years of a child’s life. The purpose of this study was to assess the impact of a preschool-based obesity prevention effectiveness trial at 1-year follow-up. Design RCT. Settings/participants Primarily African American children (aged 3–5 years, N=618) attending Head Start preschool programs administered by Chicago Public Schools. Methods Eighteen preschools were randomly assigned in 2007–2008 to receive either: (1) a 14-week teacher-delivered intervention focused on healthy lifestyle behaviors; or (2) a 14-week teacher-delivered general health curriculum (control group). Main outcome measures The primary outcome, BMI, was measured at baseline, post-intervention, and 1-year follow-up. Diet and screen time behaviors were also assessed at these time points. Multilevel mixed effects models were used to test for between-group differences. Data were analyzed in 2014. Results Significant between-group differences were observed in diet, but not in BMI z-score or screen time at 1-year follow-up. Diet differences favored the intervention arm over controls in overall diet quality (p=0.02) and in subcomponents of diet quality, as measured by the Healthy Eating Index-2005, and in fruit intake (servings/day, excludes juice) (p=0.02). Diet quality worsened more among controls than the intervention group at 1-year follow-up. Conclusions The adaptation of Hip-Hop to Health Jr. produced modest benefits in diet quality, but did not significantly impact weight gain trajectory. Not unlike other effectiveness trials, this real-world version delivered by Head Start teachers produced fewer benefits than the more rigorous efficacy trial. It is important to understand and build upon the lessons learned from these types of trials so that we can design, implement, and disseminate successful evidence-based programs more widely and effectively

  20. A novel study of screening and confirmation of modafinil, adrafinil and their metabolite modafinilic acid under EI-GC-MS and ESI-LC-MS-MS ionization.

    Science.gov (United States)

    Dubey, S; Ahi, S; Reddy, I M; Kaur, T; Beotra, A; Jain, S

    2009-12-01

    Adrafinil and modafinil have received wide publicity and have become controversial in the sporting world when several athletes were discovered allegedly using these drugs as doping agents. By acknowledging the facts, the World Anti-Doping Agency (WADA) banned these drugs in sports since 2004. The present study explores the possibility of differentiating adrafinil and modafinil and their major metabolites under electron impact ionization in gas chromatograph-mass spectrometer (GC-MSD) and electrospray ionization in liquid chromatograph-mass spectrometer (LC-MS/MS) by studying the fragmentation pattern of these drugs. Adrafinil, modafinil and their major metabolite, modafinilic acid were analyzed on EI-GC-MSD and ESI-LC-MS/MS using various individual parameters on both the instruments. The analytical technique and equipment used in the analysis were an Agilent 6890N GC with 5973 mass selective detector for the GC-MSD analysis and an Agilent 1100 HPLC with API-3200 Triple quadrupole mass spectrometer for the LC-MS/MS analysis. Validation of both methods was performed using six replicates at different concentrations. The results show that adrafinil, modafinil and their major metabolite modafinilic acid could be detected as a single artifact without differentiation under EI-GC-MSD analysis. However, all drugs could be detected and differentiated under ESI-LCMS/MS analysis without any artifaction. The GC-MSD analysis gives a single artifact for both the drugs without differentiation and thus can be used as a marker for screening purposes. Further, the Multiple Reaction Monitoring (MRM) method developed under LC-MS/MS is fit for the purpose for confirmation of suspicious samples in routine sports testing and in forensic and clinical analysis.

  1. The APEX Quantitative Proteomics Tool: Generating protein quantitation estimates from LC-MS/MS proteomics results

    Directory of Open Access Journals (Sweden)

    Saeed Alexander I

    2008-12-01

    Full Text Available Abstract Background Mass spectrometry (MS based label-free protein quantitation has mainly focused on analysis of ion peak heights and peptide spectral counts. Most analyses of tandem mass spectrometry (MS/MS data begin with an enzymatic digestion of a complex protein mixture to generate smaller peptides that can be separated and identified by an MS/MS instrument. Peptide spectral counting techniques attempt to quantify protein abundance by counting the number of detected tryptic peptides and their corresponding MS spectra. However, spectral counting is confounded by the fact that peptide physicochemical properties severely affect MS detection resulting in each peptide having a different detection probability. Lu et al. (2007 described a modified spectral counting technique, Absolute Protein Expression (APEX, which improves on basic spectral counting methods by including a correction factor for each protein (called Oi value that accounts for variable peptide detection by MS techniques. The technique uses machine learning classification to derive peptide detection probabilities that are used to predict the number of tryptic peptides expected to be detected for one molecule of a particular protein (Oi. This predicted spectral count is compared to the protein's observed MS total spectral count during APEX computation of protein abundances. Results The APEX Quantitative Proteomics Tool, introduced here, is a free open source Java application that supports the APEX protein quantitation technique. The APEX tool uses data from standard tandem mass spectrometry proteomics experiments and provides computational support for APEX protein abundance quantitation through a set of graphical user interfaces that partition thparameter controls for the various processing tasks. The tool also provides a Z-score analysis for identification of significant differential protein expression, a utility to assess APEX classifier performance via cross validation, and a

  2. Human herpesviruses and MS

    DEFF Research Database (Denmark)

    Christensen, Tove

    2007-01-01

    and they are capable of reactivation. Epstein Barr virus (EBV), HHV-6A and varicella zoster virus (VZV) are consistently linked with MS, particularly with respect to epidemiology, antibody responses in serum (EBV) and cerebrospinal fluid (EBV and HHV-6A), and with MS exacerbations that are associated with viral...... reactivation (VZV, HHV-6A and EBV). HHV have the potential for a causal role in MS--they may be key players in the disease process--and this role could be mediated through several direct or indirect mechanisms....

  3. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... working effectively. How does RRMS differ from progressive types of MS? While RRMS is defined by attacks of ... forms of MS involve much less of this type of inflammation. People with RRMS tend to have more ...

  4. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... More Schilder's Disease Learn More The National MS Society is Here to Help Need More Information? We ... Twitter LinkedIn YouTube Pinterest MS Connection About the Society Vision Careers Leadership Cultural Values Financials News Press ...

  5. Quantification of free and total sialic acid excretion by LC-MS/MS

    NARCIS (Netherlands)

    van der Ham, Maria; Prinsen, Berthil H. C. M. T.; Huijmans, Jan G. M.; Abeling, Nicolaas G. G. M.; Dorland, Bert; Berger, Ruud; de Koning, Tom J.; de Sain-van der Velden, Monique G. M.

    2007-01-01

    The main purpose for measuring urinary free sialic acid (FSA) is to diagnose sialic acid (SA) storage diseases. Elevated amounts of conjugated sialic acid (CSA) are observed in several diseases indicating the need to quantify CSA as well. A LC-MS/MS method for quantification of FSA and total sialic

  6. ms_lims, a simple yet powerful open source laboratory information management system for MS-driven proteomics.

    Science.gov (United States)

    Helsens, Kenny; Colaert, Niklaas; Barsnes, Harald; Muth, Thilo; Flikka, Kristian; Staes, An; Timmerman, Evy; Wortelkamp, Steffi; Sickmann, Albert; Vandekerckhove, Joël; Gevaert, Kris; Martens, Lennart

    2010-03-01

    MS-based proteomics produces large amounts of mass spectra that require processing, identification and possibly quantification before interpretation can be undertaken. High-throughput studies require automation of these various steps, and management of the data in association with the results obtained. We here present ms_lims (http://genesis.UGent.be/ms_lims), a freely available, open-source system based on a central database to automate data management and processing in MS-driven proteomics analyses.

  7. Proceedings of the Annual Meeting (14th) Aquatic Plant Control Research Planning and Operations Review, Held at Lake Eufaula, Oklahoma on 26-29 November 1979.

    Science.gov (United States)

    1980-10-01

    Jr ... 76 ’- CHEMICAL CONTROL TECHNOLOGY DEVELOPMENT An Overview by Howard E. Westerdahl ..........--.-. 78 Development of Controlled-Release Herbicide...Experiment Station P. 0. Box 631 Vicksburg, MS 39180 Howard Westerdahl USAE Waterways Experiment Station P. 0. Box 631 Vicksburg, MS 39180 Kin Whittington...Ballroom 8:00 a.m. Chemical Control Technology Development - H. E. Westerdahl , WES, presiding 8:10 a.m. The Development of Controlled-Release

  8. Novel Approaches to Preventing Urinary Tract Infection in Women

    Science.gov (United States)

    2001-09-01

    vaccines . In: Mobley HLT. 54. Johnson JR. Steil A. Delavari P. Canine feces as a reservoir ofextraintestinal Warren 1W, eds. Urinary tract infections...the material was subjected to analysis by Triple quadrupole ESI-MS/CID-MS experiments were electrospray ionization mass spectrometry in the positive ion...prophylaxis. Characteristic of prophylactic regimens development of vaccines against these infections, containing nitrofurantoin is the frequency of side

  9. Diet-induced perturbation of the rat liver mitochondrial acetylome studied by quantitative (iTRAQ) LC-MS/MS

    DEFF Research Database (Denmark)

    León, Ileana R.; Schwämmle, Veit; Williamson, James

    described3. Quantitation by MS/MS was achieved by using iTRAQ 8-Plex reagents (Life Technologies). LC-MS/MS analyses were performed using an Easy-nLC (Proxeon/ThermoFisher) fitted with an in-house made 17 cm C18 column that was interfaced to an LTQ-OrbiTrap XL instrument (ThermoFisher). Data analysis...

  10. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... Review of Society's Research Programs d Careers d Leadership Board of Directors Senior Leadership Team Founder Sylvia Lawry d Cultural Values d ... Pinterest MS Connection About the Society Vision Careers Leadership Cultural Values Financials News Press Room MS Prevalence ...

  11. Relapsing-Remitting MS (RRMS)

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    Full Text Available ... Another Condition Aging with MS Anesthesia and Surgery Managing Your MS d Emotional Well-Being Mood Changes d Spiritual Well-Being Building Spirituality into Your Life d Cognitive Health d Work, Home & Leisure Employment Insurance & Financial Information Staying Mobile ...

  12. Comprehensive analysis of proteins of pH fractionated samples using monolithic LC/MS/MS, intact MW measurement and MALDI-QIT-TOF MS

    Science.gov (United States)

    Yoo, Chul; Patwa, Tasneem H.; Kreunin, Paweena; Miller, Fred R.; Huber, Christian G.; Nesvizhskii, Alexey I.; Lubman, David M.

    2012-01-01

    A comprehensive platform that integrates information from the protein and peptide levels by combining various MS techniques has been employed for the analysis of proteins in fully malignant human breast cancer cells. The cell lysates were subjected to chromatofocusing fractionation, followed by tryptic digestion of pH fractions for on-line monolithic RP-HPLC interfaced with linear ion trap MS analysis for rapid protein identification. This unique approach of direct analysis of pH fractions resulted in the identification of large numbers of proteins from several selected pH fractions, in which approximately 1.5 μg of each of the pH fraction digests was consumed for an analysis time of ca 50 min. In order to combine valuable information retained at the protein level with the protein identifications obtained from the peptide level information, the same pH fraction was analyzed using nonporous (NPS)-RP-HPLC/ESI-TOF MS to obtain intact protein MW measurements. In order to further validate the protein identification procedures from the fraction digest analysis, NPS-RP-HPLC separation was performed for off-line protein collection to closely examine each protein using MALDI-TOF MS and MALDI-quadrupole ion trap (QIT)-TOF MS, and excellent agreement of protein identifications was consistently observed. It was also observed that the comparison to intact MW and other MS information was particularly useful for analyzing proteins whose identifications were suggested by one sequenced peptide from fraction digest analysis. PMID:17206599

  13. Quantification of acetaminophen (paracetamol) in human plasma and urine by stable isotope-dilution GC-MS and GC-MS/MS as pentafluorobenzyl ether derivative.

    Science.gov (United States)

    Trettin, Arne; Zoerner, Alexander A; Böhmer, Anke; Gutzki, Frank-Mathias; Stichtenoth, Dirk O; Jordan, Jens; Tsikas, Dimitrios

    2011-08-01

    We report on the quantitative determination of acetaminophen (paracetamol; NAPAP-d(0)) in human plasma and urine by GC-MS and GC-MS/MS in the electron-capture negative-ion chemical ionization (ECNICI) mode after derivatization with pentafluorobenzyl (PFB) bromide (PFB-Br). Commercially available tetradeuterated acetaminophen (NAPAP-d(4)) was used as the internal standard. NAPAP-d(0) and NAPAP-d(4) were extracted from 100-μL aliquots of plasma and urine with 300 μL ethyl acetate (EA) by vortexing (60s). After centrifugation the EA phase was collected, the solvent was removed under a stream of nitrogen gas, and the residue was reconstituted in acetonitrile (MeCN, 100 μL). PFB-Br (10 μL, 30 vol% in MeCN) and N,N-diisopropylethylamine (10 μL) were added and the mixture was incubated for 60 min at 30 °C. Then, solvents and reagents were removed under nitrogen and the residue was taken up with 1000 μL of toluene, from which 1-μL aliquots were injected in the splitless mode. GC-MS quantification was performed by selected-ion monitoring ions due to [M-PFB](-) and [M-PFB-H](-), m/z 150 and m/z 149 for NAPAP-d(0) and m/z 154 and m/z 153 for NAPAP-d(4), respectively. GC-MS/MS quantification was performed by selected-reaction monitoring the transition m/z 150 → m/z 107 and m/z 149 → m/z 134 for NAPAP-d(0) and m/z 154 → m/z 111 and m/z 153 → m/z 138 for NAPAP-d(4). The method was validated for human plasma (range, 0-130 μM NAPAP-d(0)) and urine (range, 0-1300 μM NAPAP-d(0)). Accuracy (recovery, %) ranged between 89 and 119%, and imprecision (RSD, %) was below 19% in these matrices and ranges. A close correlation (r>0.999) was found between the concentrations measured by GC-MS and GC-MS/MS. By this method, acetaminophen can be reliably quantified in small plasma and urine sample volumes (e.g., 10 μL). The analytical performance of the method makes it especially useful in pediatrics. Copyright © 2011 Elsevier B.V. All rights reserved.

  14. VOC identification and inter-comparison from laboratory biomass burning using PTR-MS and PIT-MS

    Science.gov (United States)

    C. Warneke; J. M. Roberts; P. Veres; J. Gilman; W. C. Kuster; I. Burling; R. Yokelson; J. A. de Gouw

    2011-01-01

    Volatile organic compounds (VOCs) emitted from fires of biomass commonly found in the southeast and southwest U.S. were investigated with PTR-MS and PIT-MS, which are capable of fast measurements of a large number of VOCs. Both instruments were calibrated with gas standards and mass dependent calibration curves are determined. The sensitivity of the PIT-MS linearly...

  15. The LVIS Jr. microstent to assist coil embolization of wide-neck intracranial aneurysms: clinical study to assess safety and efficacy

    International Nuclear Information System (INIS)

    Moehlenbruch, M.; Herweh, C.; Behrens, L.; Jestaedt, L.; Bendszus, M.; Pham, M.; Amiri, H.; Ringleb, P.A.

    2014-01-01

    This study was aimed to assess clinical safety and efficacy of the LVIS Jr. microstent in stent-assisted coil embolization of wide-neck intracranial aneurysms. IRB approved single-center interventional clinical study in 22 patients (10 females, 12 males, mean age 55, age range 33-74 years) for the endovascular treatment of wide-neck aneurysms. After obtaining informed consent, patients were included according to the following criteria: aneurysm fundus-to-neck ratio 4 mm, and a parent vessel diameter of ≤3.5 mm. Primary end point for clinical safety was absence of death, absence of major or minor stroke, and absence of transient ischemic attack. Primary end point for treatment efficacy was complete angiographic occlusion according to the Raymond-Roy Occlusion Classification (RROC) immediately after the procedure and at follow-up after 3 and 6 months on magnetic resonance imaging (MRI). In 20/22 (91 %) of patients, the primary end point of safety was reached; in the two remaining patients, transient ischemic attack, but no permanent deficit was observed; in 16/22 (73 %), efficient occlusion (RROC1) was reached, and in 6/22 (27 %), a residual neck remained (RROC2). Single [seven with antegrade, two in crossover configuration, and four with ''first-balloon-then-stent'' (FBTS) technique] or double-stent (eight patients with Y configuration and one patient with X configuration) deployment was technically successful in all cases. Deployment of the LVIS Jr. microstent in various single- or double-stent configurations is safe and effective to assist the treatment of intracranial wide-neck aneurysms. (orig.)

  16. HPLC-UV, MALDI-TOF-MS and ESI-MS/MS analysis of the mechlorethamine DNA crosslink at a cytosine-cytosine mismatch pair.

    Directory of Open Access Journals (Sweden)

    Pornchai Rojsitthisak

    Full Text Available Mechlorethamine [ClCH(2CH(2N(CH(3CH(2CH(2Cl], a nitrogen mustard alkylating agent, has been proven to form a DNA interstrand crosslink at a cytosine-cytosine (C-C mismatch pair using gel electrophoresis. However, the atomic connectivity of this unusual crosslink is unknown.HPLC-UV, MALDI-TOF-MS, and ESI-MS/MS were used to determine the atomic connectivity of the DNA C-C crosslink formed by mechlorethamine, MALDI-TOF-MS of the HPLC-purified reaction product of mechlorethamine with the DNA duplex d[CTCACACCGTGGTTC]•d[GAACCACCGTGTGAG] (underlined bases are a C-C mismatch pair indicated formation of an interstrand crosslink at m/z 9222.088 [M-2H+Na](+. Following enzymatic digestion of the crosslinked duplex by snake venom phosphodiesterase and calf intestinal phosphatase, ESI-MS/MS indicated the presence of dC-mech-dC [mech = CH(2CH(2N(CH(3CH(2CH(2] at m/z 269.2 [M](2+ (expected m/z 269.6, exact mass 539.27 and its hydrolytic product dC-mech-OH at m/z 329.6 [M](+ (expected m/z 329.2. Fragmentation of dC-mech-dC gave product ions at m/z 294.3 and 236.9 [M](+, which are both due to loss of the 4-amino group of cytosine (as ammonia, in addition to dC and dC+HN(CH(3CH = CH(2, respectively. The presence of m/z 269.2 [M](2+ and loss of ammonia exclude crosslink formation at cytosine N(4 or O(2 and indicate crosslinking through cytosine N(3 with formation of two quaternary ammonium ions.Our results provide an important addition to the literature, as the first example of the use of HPLC and MS for analysis of a DNA adduct at the N(3 position of cytosine.

  17. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... Text Print Discover More Here are a few related topics that may interest you Living with MS (.pdf) Download Brochure Focus on Employment (.pdf) Download Brochure Working with MS (.pdf) Download Brochure Taming Stress (.pdf) Download Brochure Multiple Sclerosis and Your Emotions (. ...

  18. Distinctive and Complementary MS2 Fragmentation Characteristics for Identification of Sulfated Sialylated N-Glycopeptides by nanoLC-MS/MS Workflow

    Science.gov (United States)

    Kuo, Chu-Wei; Guu, Shih-Yun; Khoo, Kay-Hooi

    2018-04-01

    High sensitivity identification of sulfated glycans carried on specific sites of glycoproteins is an important requisite for investigation of molecular recognition events involved in diverse biological processes. However, aiming for resolving site-specific glycosylation of sulfated glycopeptides by direct LC-MS2 sequencing is technically most challenging. Other than the usual limiting factors such as lower abundance and ionization efficiency compared to analysis of non-glycosylated peptides, confident identification of sulfated glycopeptides among the more abundant non-sulfated glycopeptides requires additional considerations in the selective enrichment and detection strategies. Metal oxide has been applied to enrich phosphopeptides and sialylated glycopeptides, but its use to capture sulfated glycopeptides has not been investigated. Likewise, various complementary MS2 fragmentation modes have yet to be tested against sialylated and non-sialylated sulfoglycopeptides due to limited appropriate sample availability. In this study, we have investigated the feasibility of sequencing tryptic sulfated N-glycopeptide and its MS2 fragmentation characteristics by first optimizing the enrichment methods to allow efficient LC-MS detection and MS2 analysis by a combination of CID, HCD, ETD, and EThcD on hybrid and tribrid Orbitrap instruments. Characteristic sulfated glyco-oxonium ions and direct loss of sulfite from precursors were detected as evidences of sulfate modification. It is anticipated that the technical advances demonstrated in this study would allow a feasible extension of our sulfoglycomic analysis to sulfoglycoproteomics. [Figure not available: see fulltext.

  19. How much separation for LC-MS/MS quantitative bioanalysis of drugs and metabolites?

    Science.gov (United States)

    Tan, Aimin; Fanaras, John C

    2018-05-01

    LC-MS/MS has been the dominant analytical technology for quantitative bioanalysis of drugs and metabolites for more than two decades. Despite this, a very fundamental question like how much separation is required for LC-MS/MS quantitative bioanalysis of drugs and metabolites has not been adequately addressed. Some think that no or only very limited separation is necessary thanks to the unparalleled selectivity offered by tandem mass spectrometry. Others think that the more separation, the better, because of the potential detrimental impact of matrix effect (ion suppression or enhancement). Still others just use a rule-of-thumb approach by keeping the adjusted retention/capacity factor always between 2 and 5. The purpose of this article is to address this fundamental question through rational thinking together with various real case examples drawn from regulated bioanalytical laboratories. Copyright © 2018 Elsevier B.V. All rights reserved.

  20. COMPARISON OF COMMERCIAL LC MS/MS COMPATIBLE DETERGENTS WITH SODIUM DEOXYCHOLATE FOR SHOTGUN PROTEOMICS

    Directory of Open Access Journals (Sweden)

    Caleb J. Porter

    2014-12-01

    Full Text Available In this study, we compared the performance of sodium deoxycholate (SDC with several commercially available LC MS/MS compatible detergents for digestion of complex proteomic mixtures. First, the parameters affecting in-solution digestion using SDC were investigated with a full factorial experimental design. Metrics explored were trypsin ratio, digestion time, and concentration of SDC. These parameters were not found to be statistically associated with total peptide identifications in the experimental space investigated. However, in terms of digestion efficiency, digestion time was highly significant (p = 0.0095 as determined by the percent of peptides identified with missed cleavages. The optimized protocol for peptide identification and throughput was used to compare the performance of SDC with various commercially available LC MS/MS compatible surfactants namely Invitrosol, RapiGest, and PPS Silent Surfactant. The detergents were found to be similar through comparisons of the total identified peptides and the hydrophobicity of recovered peptides. We found suitable recovery across a large range of SDC concentrations determined from a bicinchoninic acid (BCA assay. In a spike down experiment, no distinct differences in total number of peptide identifications were discovered when comparing PPS (Silent Surfactant and SDC for preparation of peptide samples derived from low protein amounts (< 20 µg. Combined, these results indicate that SDC is a cost effective alternative to other commonly used LC MS/MS compatible surfactants

  1. pyOpenMS: a Python-based interface to the OpenMS mass-spectrometry algorithm library.

    Science.gov (United States)

    Röst, Hannes L; Schmitt, Uwe; Aebersold, Ruedi; Malmström, Lars

    2014-01-01

    pyOpenMS is an open-source, Python-based interface to the C++ OpenMS library, providing facile access to a feature-rich, open-source algorithm library for MS-based proteomics analysis. It contains Python bindings that allow raw access to the data structures and algorithms implemented in OpenMS, specifically those for file access (mzXML, mzML, TraML, mzIdentML among others), basic signal processing (smoothing, filtering, de-isotoping, and peak-picking) and complex data analysis (including label-free, SILAC, iTRAQ, and SWATH analysis tools). pyOpenMS thus allows fast prototyping and efficient workflow development in a fully interactive manner (using the interactive Python interpreter) and is also ideally suited for researchers not proficient in C++. In addition, our code to wrap a complex C++ library is completely open-source, allowing other projects to create similar bindings with ease. The pyOpenMS framework is freely available at https://pypi.python.org/pypi/pyopenms while the autowrap tool to create Cython code automatically is available at https://pypi.python.org/pypi/autowrap (both released under the 3-clause BSD licence). © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Extending the Technological, Discursive, and Rhetorical Horizons of Academic Research Libraries' Information Architectures: An Analysis of North Carolina State University's James B. Hunt Jr. Library

    Science.gov (United States)

    Carr, Patrick L.

    2017-01-01

    This dissertation analyzes how North Carolina State University's (NCSU) James B. Hunt Jr. Library extends the ways in which the information architectures of academic research libraries can function as a technology, as discourse, and as rhetoric. The starting point for the analysis is the libraries of antiquity, which functioned technologically as…

  3. 75 FR 2853 - False Killer Whale Take Reduction Team Meeting

    Science.gov (United States)

    2010-01-19

    ... interactions in Hawaiian waters. Pacific Science 59:593-601. Carretta J.V., K.A. Forney, M.S. Lowry, J. Barlow....S. Lowry, J. Barlow, J. Baker, D. Johnston, B. Hanson, R.L. Brownell Jr., J. Robbins, D.K. Mattila...

  4. Disease: H00875 [KEGG MEDICUS

    Lifescience Database Archive (English)

    Full Text Available H00875 Megalencephalic leukoencephalopathy with subcortical cysts (MLC) Megalencephaiic leukoencephalopathy...tion, gene) ... AUTHORS ... Singhal BS, Gorospe JR, Naidu S ... TITLE ... Megalencephalic leukoencephalopathy with...naap MS ... TITLE ... Mutant GlialCAM causes megalencephalic leukoencephalopathy with subcortical cysts, benig

  5. The neurophysiologist perspective into MS plasticity

    Directory of Open Access Journals (Sweden)

    Elise eHoudayer

    2015-09-01

    Full Text Available Multiple sclerosis (MS is a frequent, highly debilitating inflammatory demyelinating disease, starting to manifest in early adulthood and presenting a wide variety of symptoms which are often resistant to pharmacological treatments. Cortical dysfunctions have been demonstrated to be key components of MS condition, and plasticity of the corticospinal motor system is highly involved in major MS symptoms, such as fatigue, spasticity or pain. Cortical dysfunction in MS can be studied with neurophysiological tools such as electroencephalography (EEG and related techniques (evoked potentials – EPs or transcranial magnetic stimulation (TMS. These techniques are now widely used to provide essential elements of MS diagnosis and can also be used to modulate plasticity. Indeed the recent development of non-invasive brain stimulation (NIBS techniques able to induce cortical plasticity, such as repetitive TMS or transcranial direct current stimulation (tDCS, has brought promising results as add-on treatments.In this review we will focus on the use of these tools (EEG, TMS to study plasticity in MS and on the major techniques used to modulate plasticity in MS.

  6. The Neurophysiologist Perspective into MS Plasticity.

    Science.gov (United States)

    Houdayer, Elise; Comi, Giancarlo; Leocani, Letizia

    2015-01-01

    Multiple sclerosis (MS) is a frequent, highly debilitating inflammatory demyelinating disease, starting to manifest in early adulthood and presenting a wide variety of symptoms, which are often resistant to pharmacological treatments. Cortical dysfunctions have been demonstrated to be key components of MS condition, and plasticity of the corticospinal motor system is highly involved in major MS symptoms, such as fatigue, spasticity, or pain. Cortical dysfunction in MS can be studied with neurophysiological tools, such as electroencephalography (EEG) and related techniques (evoked potentials) or transcranial magnetic stimulation (TMS). These techniques are now widely used to provide essential elements of MS diagnosis and can also be used to modulate plasticity. Indeed, the recent development of non-invasive brain stimulation techniques able to induce cortical plasticity, such as repetitive TMS or transcranial direct current stimulation, has brought promising results as add-on treatments. In this review, we will focus on the use of these tools (EEG and TMS) to study plasticity in MS and on the major techniques used to modulate plasticity in MS.

  7. The Microcosm within: An interview with William B. Miller, Jr., on the Extended Hologenome theory of evolution.

    Science.gov (United States)

    Hunt, Tam

    2015-01-01

    There is a singular unifying reality underlying every biologic interaction on our planet. In immunology, that which does not kill you makes you different. -William B. Miller, Jr. We are experiencing a revolution in our understanding of inner space on a par with our exponentially increasing understanding of outer space. In biology, we are learning that the genetic and epigenetic complexity within organisms is far deeper than suspected. This is a key theme in William B. Miller Jr.'s book, The Microcosm Within: Evolution and Extinction in the Hologenome. We are learning also that a focus on the human genome alone is misleading when it comes to who we really are as biological entities, and in terms of how we and other creatures have evolved. Rather than being defined by the human genome alone, we are instead defined by the "hologenome," the sum of the human genome and the far larger genetic endowment of the microbiome and symbiotic communities that reside within and around us. Miller is a medical doctor previously in private practice in Pennsylvania and Phoenix, Arizona. This book is his first foray into evolutionary theory. His book could have been titled "The Origin of Variation" because this is his primary focus. He accepts that natural selection plays a role in evolution, but he demotes this mechanism to a less important role than the Modern Synthesis suggests. His main gripe, however, concerns random variation. He argues that random variation is unable to explain the origin and evolution of biological forms that we see in the world around us and in the historical record. Miller suggests that, rather than random variation as the engine of novelty, there is a creative impulse at the heart of cellular life, and even at the level of the genetic aggregate, that generates novelty on a regular basis. I probe this assertion in the interview below. He also highlights the strong role of "exogenous genetic assault" in variation and in his immunological model of evolution.

  8. Simultaneous determination of creatinine and creatine in human serum by double-spike isotope dilution liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-mass spectrometry (GC-MS).

    Science.gov (United States)

    Fernández-Fernández, Mario; Rodríguez-González, Pablo; Añón Álvarez, M Elena; Rodríguez, Felix; Menéndez, Francisco V Álvarez; García Alonso, J Ignacio

    2015-04-07

    This work describes the first multiple spiking isotope dilution procedure for organic compounds using (13)C labeling. A double-spiking isotope dilution method capable of correcting and quantifying the creatine-creatinine interconversion occurring during the analytical determination of both compounds in human serum is presented. The determination of serum creatinine may be affected by the interconversion between creatine and creatinine during sample preparation or by inefficient chemical separation of those compounds by solid phase extraction (SPE). The methodology is based on the use differently labeled (13)C analogues ((13)C1-creatinine and (13)C2-creatine), the measurement of the isotopic distribution of creatine and creatinine by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and the application of multiple linear regression. Five different lyophilized serum-based controls and two certified human serum reference materials (ERM-DA252a and ERM-DA253a) were analyzed to evaluate the accuracy and precision of the proposed double-spike LC-MS/MS method. The methodology was applied to study the creatine-creatinine interconversion during LC-MS/MS and gas chromatography-mass spectrometry (GC-MS) analyses and the separation efficiency of the SPE step required in the traditional gas chromatography-isotope dilution mass spectrometry (GC-IDMS) reference methods employed for the determination of serum creatinine. The analysis of real serum samples by GC-MS showed that creatine-creatinine separation by SPE can be a nonquantitative step that may induce creatinine overestimations up to 28% in samples containing high amounts of creatine. Also, a detectable conversion of creatine into creatinine was observed during sample preparation for LC-MS/MS. The developed double-spike LC-MS/MS improves the current state of the art for the determination of creatinine in human serum by isotope dilution mass spectrometry (IDMS), because corrections are made for all the possible errors

  9. United Kingdom Shadow Secretary of State for Universities and Skills David Willetts MP (centre) in front of the CMS detector with (from left to right) A. Barr, Partner and Founder, Matterhorn Investment Management LLP P. Bate, S. Harper, M. Willetts, T. Virdee, J. Ellis, CMS Spokesperson G. Tonelli, CMS Technical Coordinator A. Ball and (front) Partner, Caravel Capital H. Hsueh and P. Wells. Monday 4th January 2010

    CERN Multimedia

    Maximilien Brice; Point 5

    2010-01-01

    United Kingdom Shadow Secretary of State for Universities and Skills David Willetts MP (centre) in front of the CMS detector with (from left to right) A. Barr, Partner and Founder, Matterhorn Investment Management LLP P. Bate, S. Harper, M. Willetts, T. Virdee, J. Ellis, CMS Spokesperson G. Tonelli, CMS Technical Coordinator A. Ball and (front) Partner, Caravel Capital H. Hsueh and P. Wells. Monday 4th January 2010

  10. Chemical characterization of Azadirachta indica grafted on Melia azedarach and analyses of azadirachtin by HPLC-MS-MS (SRM) and meliatoxins by MALDI-MS.

    Science.gov (United States)

    Forim, Moacir Rossi; Cornélio, Vivian Estevam; da Silva, M Fátima das G F; Rodrigues-Filho, Edson; Fernandes, João B; Vieira, Paulo C; Matinez, Sueli Souza; Napolitano, Michael P; Yost, Richard A

    2010-01-01

    Melia azedarach adapted to cool climates was selected as rootstocks for vegetative propagation of Azadirachta indica. Cleft grafting of A. indica on M. azedarach rootstock showed excellent survival. Little is known about the chemistry of grafting. The roots, stems, leaves and seeds of this graft were examined in order to verify if grafted A. indica would produce limonoids different from those found in non-grafted plants. Intact matured fruits were also studied to verify if they were free of meliatoxins. After successive chromatographic separations the extracts afforded several limonoids. HPLC-MS/MS and MALDI-MS were used to develop sensitive methods for detecting azadirachtin on all aerial parts of this graft and meliatoxins in fruits, respectively. The stem afforded the limonoid salannin, which was previously found in the oil seeds of A. indica. Salannin is also found in the root bark of M. azedarach. Thus, the finding of salannin in this study suggests that it could have been translocated from the M. azedarach rootstock to the A. indica graft. HPLC-MS/MS analyses showed that azadirachtin was present in all parts of the fruits, stem, flowers and root, but absent in the leaves. The results of MALDI-MS analyses confirmed the absence of meliatoxins in graft fruits. This study showed that A. indica grafted onto M. azedarach rootstock produces azadirachtin, and also that its fruits are free of meliatoxins from rootstocks, confirming that this graft forms an excellent basis for breeding vigorous Neem trees in cooler regions.

  11. The utility of ultra-high performance supercritical fluid chromatography-tandem mass spectrometry (UHPSFC-MS/MS) for clinically relevant steroid analysis.

    Science.gov (United States)

    Storbeck, Karl-Heinz; Gilligan, Lorna; Jenkinson, Carl; Baranowski, Elizabeth S; Quanson, Jonathan L; Arlt, Wiebke; Taylor, Angela E

    2018-05-15

    Liquid chromatography tandem mass spectrometry (LC-MS/MS) assays are considered the reference standard for serum steroid hormone analyses, while full urinary steroid profiles are only achievable by gas chromatography (GC-MS). Both LC-MS/MS and GC-MS have well documented strengths and limitations. Recently, commercial ultra-high performance supercritical fluid chromatography-tandem mass spectrometry (UHPSFC-MS/MS) systems have been developed. These systems combine the resolution of GC with the high-throughput capabilities of UHPLC. Uptake of this new technology into research and clinical labs has been slow, possibly due to the perceived increase in complexity. Here we therefore present fundamental principles of UHPSFC-MS/MS and the likely applications for this technology in the clinical research setting, while commenting on potential hurdles based on our experience to date. Copyright © 2018 The Authors. Published by Elsevier B.V. All rights reserved.

  12. Simultaneous Determination of Cyclosporine A, Tacrolimus, Sirolimus, and Everolimus in Whole-Blood Samples by LC-MS/MS

    Directory of Open Access Journals (Sweden)

    Mustafa Karapirli

    2012-01-01

    Full Text Available Objectives. Cyclosporine A (CyA, tacrolimus (TRL, sirolimus (SIR, and everolimus (RAD are immunosuppressive drugs frequently used in organ transplantation. Our aim was to confirm a robust sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS method for determination of CyA, TRL, SIR, and RAD in whole-blood samples. Materials and Methods. We used an integrated online solid-phase extraction-LC-MS/MS system and atmospheric pressure ionization tandem mass spectrometry (API-MS/MS in the multiple reaction monitoring (MRM detection mode. CyA, TRL, SIR, and RAD were simultaneously analyzed in whole blood treated with precipitation reagent taken from transplant patients. Results. System performance parameters were suitable for using this method as a high-throughput technique in clinical practice. The high concentration of one analyte in the sample did not affect the concentration of other analytes. Total analytical time was 2.5 min, and retention times of all analytes were shorter than 2 minutes. Conclusion. This LC-MS/MS method can be preferable for therapeutic drug monitoring of these immunosuppressive drugs (CyA, TRL, SRL, and RAD in whole blood. Sample preparation was too short and simple in this method, and it permits robust, rapid, sensitive, selective, and simultaneous determination of these drugs.

  13. A UPLC-MS/MS method for analysis of vancomycin in human cerebrospinal fluid and comparison with the chemiluminescence immunoassay.

    Science.gov (United States)

    Mei, Shenghui; Wang, Jiaqing; Zhu, Leting; Chen, Ruiling; Li, Xingang; Chen, Kai; Chen, Guangqiang; Zhou, Jianxin; Wang, Qiang; Zhao, Zhigang

    2017-08-01

    Vancomycin (VCM) is clinically used in treating patients with postoperative intracranial infections. The cerebrospinal fluid (CSF) concentration of VCM varies greatly among patients. To guide the dosage regimens, monitoring of VCM in CSF is needed. However a method for analysis of VCM in human CSF is lacking. An ultraperformance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was developed and validated for analysis of VCM in human CSF, and the agreement of UPLC-MS/MS and chemiluminescence immunoassay (CLIA) in the analysis of CSF VCM was evaluated. The ion transitions were m/z 725.5 > 144.1 for VCM and m/z 455.2 > 308.2 for methotrexate (internal standard). The agreement between UPLC-MS/MS and CLIA was evaluated by Bland-Altman plot in 179 samples. The calibration range of the UPLC-MS/MS method was 1-400 mg/L. The inaccuracy and imprecision were -0.69-10.80% and  0.98). The 95% limit of agreement of the ratio of CLIA to UPLC-MS/MS was 61.66-107.40%. Further studies are warranted to confirm the results. Copyright © 2017 John Wiley & Sons, Ltd.

  14. STS-33 crewmembers on KSC LC Pad 39B 195 ft level with OV-103 in background

    Science.gov (United States)

    1990-01-01

    STS-33 crewmembers, wearing launch and entry suit (LES), take a break from training activities to pose for group portrait in front of Discovery, Orbiter Vehicle (OV) 103, at the 195 ft level elevator entrance at Kennedy Space Center (KSC) Launch Complex (LC) Pad 39B. Left to right are Pilot John E. Blaha, Mission Specialist (MS) Kathryn C. Thornton, MS Manley L. Carter, Jr, Commander Frederick D. Gregory, and MS F. Story Musgrave. Visible in the background is the catwalk to OV-103's side hatch.

  15. Development and validation of analytical method for Naftopidil in human plasma by LC–MS/MS

    Directory of Open Access Journals (Sweden)

    Pritam S. Jain

    2015-09-01

    Full Text Available A highly sensitive and simple high-performance liquid chromatographic–tandem mass spectrometric (LC–MS-MS assay is developed and validated for the quantification of Naftopidil in human plasma. Naftopidil is extracted from human plasma by methyl tertiary butyl ether and analyzed using a reversed-phase gradient elution on a discovery C 18 5 μ (50 × 4.6 column. A methanol: 2 mM ammonium formate (90:10 as mobile phase, is used and detection was performed by MS using electrospray ionization in positive mode. Propranolol is used as the internal standard. The lower limits of quantification are 0.495 ng/mL. The calibration curves are linear over the concentration range of 0.495–200.577 ng/mL of plasma for each analyte. This novel LC–MS-MS method shows satisfactory accuracy and precision and is sufficiently sensitive for the performance of pharmacokinetic studies in humans.

  16. Determination of chlormequat in pig serum and sow milk by LC-MS/MS

    DEFF Research Database (Denmark)

    Poulsen, Mette Erecius; Christensen, Hanne Bjerre; Sørensen, M.T.

    2007-01-01

    reproduction. Validation of the method was based on recovery tests at three spiking levels, determined as double determinations and repeated at least four times. Samples were extracted with methanol-water-acetic acid, centrifuged, filtrated and determined by LC-MS/MS. The mean recoveries were in the range 80...

  17. Metabolomics data normalization with EigenMS.

    Directory of Open Access Journals (Sweden)

    Yuliya V Karpievitch

    Full Text Available Liquid chromatography mass spectrometry has become one of the analytical platforms of choice for metabolomics studies. However, LC-MS metabolomics data can suffer from the effects of various systematic biases. These include batch effects, day-to-day variations in instrument performance, signal intensity loss due to time-dependent effects of the LC column performance, accumulation of contaminants in the MS ion source and MS sensitivity among others. In this study we aimed to test a singular value decomposition-based method, called EigenMS, for normalization of metabolomics data. We analyzed a clinical human dataset where LC-MS serum metabolomics data and physiological measurements were collected from thirty nine healthy subjects and forty with type 2 diabetes and applied EigenMS to detect and correct for any systematic bias. EigenMS works in several stages. First, EigenMS preserves the treatment group differences in the metabolomics data by estimating treatment effects with an ANOVA model (multiple fixed effects can be estimated. Singular value decomposition of the residuals matrix is then used to determine bias trends in the data. The number of bias trends is then estimated via a permutation test and the effects of the bias trends are eliminated. EigenMS removed bias of unknown complexity from the LC-MS metabolomics data, allowing for increased sensitivity in differential analysis. Moreover, normalized samples better correlated with both other normalized samples and corresponding physiological data, such as blood glucose level, glycated haemoglobin, exercise central augmentation pressure normalized to heart rate of 75, and total cholesterol. We were able to report 2578 discriminatory metabolite peaks in the normalized data (p<0.05 as compared to only 1840 metabolite signals in the raw data. Our results support the use of singular value decomposition-based normalization for metabolomics data.

  18. Analysis of benzodiazepines and their metabolites using DBS cards and LC-MS/MS.

    Science.gov (United States)

    Lee, Heesang; Park, Yujin; Jo, Jiyeong; In, Sangwhan; Park, Yonghoon; Kim, Eunmi; Pyo, Jaesung; Choe, Sanggil

    2015-10-01

    Dried Blood Spot (DBS) has been used a blood extraction method for inherited metabolic disorder screening since 1960s. With introduction of LC-MS/MS, not only DBS could be used to analysis drugs in small blood volume, but in various fields, such as toxicology, drug therapeutic monitoring, drug diagnostic screening, and illicit drugs. In toxicology field, many drugs (e.g. benzodiazepines, acetaminophen, small molecule drugs) have been tested with DBS. Compared with earlier blood extraction methods (SPE and LLE), DBS has lots of advantages; lower blood volume (less than 50μL), shorter analysis time caused by a more concise analysis procedure and lower cost. We optimized the DBS procedure and LC-MS/MS conditions for 18 benzodiazepines, seven benzodiazepine metabolites, and one z-drug (zolpidem) analysis in blood. 30μL of whole blood was spotted on FTA DMPK card C and dried for 2h in a desiccator. A 6-mm disk was punched and vortexed for 1min in a centrifuge tube with 300μL methanol/acetonitrile mixture (1:1, v/v). After evaporation, redissolved in 100μL mobile phase of LC-MS/MS and 5μL was injected. In the analysis for 26 target compounds in blood, all of the method validation parameters - LLOD, LLOQ, accuracy (intra- and inter-assay), and precision (intra- and inter-assay) - were satisfied with method validation criteria, within 15%. The results of matrix effect, recovery, and process efficiency were good. We developed a fast and reliable sample preparation method using DBS for 26 benzodiazepines, benzodiazepine metabolites, and z-drug (zolpidem). Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.

  19. Hip-Hop to Health Jr. Obesity Prevention Effectiveness Trial: postintervention results.

    Science.gov (United States)

    Fitzgibbon, Marian L; Stolley, Melinda R; Schiffer, Linda A; Braunschweig, Carol L; Gomez, Sandra L; Van Horn, Linda; Dyer, Alan R

    2011-05-01

    The preschool years offer an opportunity to interrupt the trajectory toward obesity in black children. The Hip-Hop to Health Jr. Obesity Prevention Effectiveness Trial was a group-randomized controlled trial assessing the feasibility and effectiveness of a teacher-delivered weight control intervention for black preschool children. The 618 participating children were enrolled in 18 schools administered by the Chicago Public Schools. Children enrolled in the nine schools randomized to the intervention group received a 14-week weight control intervention delivered by their classroom teachers. Children in the nine control schools received a general health intervention. Height and weight, physical activity, screen time, and diet data were collected at baseline and postintervention. At postintervention, children in the intervention schools engaged in more moderate-to-vigorous physical activity (MVPA) than children in the control schools (difference between adjusted group means = 7.46 min/day, P = 0.02). Also, children in the intervention group had less total screen time (-27.8 min/day, P = 0.05). There were no significant differences in BMI, BMI Z score, or dietary intake. It is feasible to adapt an obesity prevention program to be taught by classroom teachers. The intervention showed positive influences on physical activity and screen time, but not on diet. Measuring diet and physical activity in preschool children remains a challenge, and interventions delivered by classroom teachers require both intensive initial training and ongoing individualized supervision.

  20. Data-independent MS/MS quantification of neuropeptides for determination of putative feeding-related neurohormones in microdialysate.

    Science.gov (United States)

    Schmerberg, Claire M; Liang, Zhidan; Li, Lingjun

    2015-01-21

    Food consumption is an important behavior that is regulated by an intricate array of neuropeptides (NPs). Although many feeding-related NPs have been identified in mammals, precise mechanisms are unclear and difficult to study in mammals, as current methods are not highly multiplexed and require extensive a priori knowledge about analytes. New advances in data-independent acquisition (DIA) MS/MS and the open-source quantification software Skyline have opened up the possibility to identify hundreds of compounds and quantify them from a single DIA MS/MS run. An untargeted DIA MS(E) quantification method using Skyline software for multiplexed, discovery-driven quantification was developed and found to produce linear calibration curves for peptides at physiologically relevant concentrations using a protein digest as internal standard. By using this method, preliminary relative quantification of the crab Cancer borealis neuropeptidome (winnowing candidate NPs related to a behavior of interest in a functionally relevant manner, and demonstrates the success of such a UPLC-MS(E) quantification method using the open source software Skyline.

  1. Identification of alkyl dimethylbenzylammonium surfactants in water samples by solid-phase extraction followed by ion trap LC/MS and LC/MS/MS

    Science.gov (United States)

    Ferrer, I.; Furlong, E.T.

    2001-01-01

    A novel methodology was developed for the determination of alkyl (C12, C14, and C16) dimethylbenzylammonium chloride (benzalkonium chloride or BAC, Chemical Abstract Service number: 8001-54-5) in water samples. This method is based on solid-phase extraction (SPE) using polymeric cartridges, followed by high-performance liquid chromatography/ion trap mass spectrometry (LC/MS) and tandem mass spectrometry(MS/MS) detection, equipped with an electrospray interface in positive ion mode. Chromatographic separation was achieved for three BAC homologues by using a C18 column and a gradient of acetonitrile/10 millimolar aqueous ammonium formate. Total method recoveries were higher than 71% in different water matrices. The main ions observed by LC/MS were at mass-to-charge ratios (m/z) of 304, 332, and 360, which correspond to the molecular ions of the C12, C14, and C16 alkyl BAC, respectively. The unequivocal structural identification of these compounds in water samples was performed by LC/MS/MS after isolation and subsequent fragmentation of each molecular ion. The main fragmentation observed for the three different homologues corresponded to the loss of the toluyl group in the chemical structure, which leads to the fragment ions at m/z 212, 240, and 268 and a tropylium ion, characteristic of all homologues, at m/z 91. Detection limits for the methodology developed in this work were in the low nanogram-per-liter range. Concentration levels of BAC - ranging from 1.2 to 36.6 micrograms per liter - were found in surface-water samples collected downstream from different wastewater-treatment discharges, thus indicating its input and persistence through the wastewater-treatment process.

  2. US Army Institute of Surgical Research Annual Research Progress Report for Fiscal Year 1987.

    Science.gov (United States)

    1987-10-01

    212 Takeshi Shimazu, MD; Hisashi Ikeuchi, MD; LTC Gene B. Hubbard, DIA, MS; Avery A. Johnson, BS; Arthur D. Mason, Jr., MD; and COL...levels. Analytical Biochemistry 107:451-455, 1980. 12. Kimura M, Fujita T, and Itokawa Y: Liquid-chromatographic determination of the total thiamine...78234-5012 1 October 1986 - 30 September 1987 INVESTIGATORS Takeshi Shimazu, MD Hisashi Ikeuchi, MD Gene B. Hubbard, DVM, MS, Lieutenant Col iel, VC

  3. A Group Theoretic Approach to Metaheuristic Local Search for Partitioning Problems

    Science.gov (United States)

    2005-05-01

    Tabu Search. Mathematical and Computer Modeling 39: 599-616. 107 Daskin , M.S., E. Stern. 1981. A Hierarchical Objective Set Covering Model for EMS... A Group Theoretic Approach to Metaheuristic Local Search for Partitioning Problems by Gary W. Kinney Jr., B.G.S., M.S. Dissertation Presented to the...DISTRIBUTION STATEMENT A Approved for Public Release Distribution Unlimited The University of Texas at Austin May, 2005 20050504 002 REPORT

  4. Improved liquid chromatography-MS/MS of heparan sulfate oligosaccharides via chip-based pulsed makeup flow.

    Science.gov (United States)

    Huang, Yu; Shi, Xiaofeng; Yu, Xiang; Leymarie, Nancy; Staples, Gregory O; Yin, Hongfeng; Killeen, Kevin; Zaia, Joseph

    2011-11-01

    Microfluidic chip-based hydrophilic interaction chromatography (HILIC) is a useful separation system for liquid chromatography-mass spectrometry (LC-MS) in compositional profiling of heparan sulfate (HS) oligosaccharides; however, ions observed using HILIC LC-MS are low in charge. Tandem MS of HS oligosaccharide ions with low charge results in undesirable losses of SO(3) from precursor ions during collision induced dissociation. One solution is to add metal cations to stabilize sulfate groups. Another is to add a nonvolatile, polar compound such as sulfolane, a molecule known to supercharge proteins, to produce a similar effect for oligosaccharides. We demonstrate use of a novel pulsed makeup flow (MUF) HPLC-chip. The chip enables controlled application of additives during specified chromatographic time windows and thus minimizes the extent to which nonvolatile additives build up in the ion source. The pulsed MUF system was applied to LC-MS/MS of HS oligosaccharides. Metal cations and sulfolane were tested as additives. The most promising results were obtained for sulfolane, for which supercharging of the oligosaccharide ions increased their signal strengths relative to controls. Tandem MS of these supercharged precursor ions showed decreased abundances of product ions from sulfate losses yet more abundant product ions from backbone cleavages.

  5. Determination of Dextromethorphan in Oral Fluid by LC-MS-MS.

    Science.gov (United States)

    Amaratunga, Piyadarsha; Clothier, Morgan; Lorenz Lemberg, Bridget; Lemberg, Dave

    2016-06-01

    Dextromethorphan (DXM) is an antitussive drug found in commonly used nonprescription cold and cough medications. At low doses, DXM is a safe drug that does not produce adverse reactions. However, abuse of DXM has been reported among adolescents and young adults using the drug at higher doses. DXM is not a scheduled drug in the USA, and the primary reason for its abuse is the ease of availability. DXM is available to purchase in the form of over-the-counter cough medications, such as Robitussin(®) and Coricidin(®), or it can be purchased over the Internet in the form of a powder. In this research work, we developed an LC-MS-MS method that can quantify DXM and dextrorphan (DXO) in oral fluid in a high-throughput toxicology laboratory setting. The developed method was validated according to the Scientific Working Group for Forensic Toxicology guidelines. The linear dynamic range was 5-100 ng/mL with a lowest limit of quantitation (LLOQ) of 5.0 ng/mL for DXM and DXO. Overall, the results of the accuracy and the precision values were within the acceptance criteria for both drugs. In addition, selectivity, matrix effect and recovery were calculated for the LC-MS-MS method. Authentic samples (n = 59) were tested to evaluate the applicability of the method. Thirty samples were found to be positive for DXM and DXO and two samples were found to be positive for DXM only. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  6. Analysis of banned veterinary drugs and herbicide residues in shellfish by liquid chromatography-tandem mass spectrometry (LC/MS/MS) and gas chromatography-tandem mass spectrometry (GC/MS/MS)

    International Nuclear Information System (INIS)

    Chang, Geng-Ruei; Chen, Hui-Shan; Lin, Feng-Yi

    2016-01-01

    Seafood safety is a crucial public health concern for consumers. In this study, we applied a validated method to analyze the residue of banned veterinary drugs in shellfish, namely chloramphenicol, malachite green, leucomalachite green, and nitrofuran metabolites; additionally, the QuEChERS method was employed to detect 76 herbicides by LC/MS/MS and GC/MS/MS. In total, 42 shellfish samples, which included hard clams, freshwater clams, and oysters, were collected from aquafarms and production areas in Taiwan during 2012. Our results revealed 3.8 ng/g of chloramphenicol in one hard clam, 19.9–32.1 ng/g of ametryn in two hard clams, 16.1–60.1 ng/g of pendimethalin in four hard clams, and 17.0 ng/g of mefenacet in one oyster, indicating that 19.1% of the samples contained residues from banned veterinary drugs and pesticides. These data can be used to monitor the residue of veterinary drugs and pesticides in aquatic organisms and as a reference for food safety. - Highlights: • A certified method was employed for analyzing residues of banned veterinary drugs and herbicides in shellfish samples. • The trace levels of chloramphenicol, ametryn, pendimethalin were detected in hard clam samples. • For ensuring food safety, continual monitoring of aquatic products is necessary.

  7. Structural Feature Ions for Distinguishing N- and O-Linked Glycan Isomers by LC-ESI-IT MS/MS

    Science.gov (United States)

    Everest-Dass, Arun V.; Abrahams, Jodie L.; Kolarich, Daniel; Packer, Nicolle H.; Campbell, Matthew P.

    2013-06-01

    Glycomics is the comprehensive study of glycan expression in an organism, cell, or tissue that relies on effective analytical technologies to understand glycan structure-function relationships. Owing to the macro- and micro-heterogeneity of oligosaccharides, detailed structure characterization has required an orthogonal approach, such as a combination of specific exoglycosidase digestions, LC-MS/MS, and the development of bioinformatic resources to comprehensively profile a complex biological sample. Liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS/MS) has emerged as a key tool in the structural analysis of oligosaccharides because of its high sensitivity, resolution, and robustness. Here, we present a strategy that uses LC-ESI-MS/MS to characterize over 200 N- and O-glycans from human saliva glycoproteins, complemented by sequential exoglycosidase treatment, to further verify the annotated glycan structures. Fragment-specific substructure diagnostic ions were collated from an extensive screen of the literature available on the detailed structural characterization of oligosaccharides and, together with other specific glycan structure feature ions derived from cross-ring and glycosidic-linkage fragmentation, were used to characterize the glycans and differentiate isomers. The availability of such annotated mass spectrometric fragmentation spectral libraries of glycan structures, together with such substructure diagnostic ions, will be key inputs for the future development of the automated elucidation of oligosaccharide structures from MS/MS data.

  8. Application of HRAM screening and LC-MS/MS confirmation of active pharmaceutical ingredient in "natural" herbal supplements.

    Science.gov (United States)

    Pascali, Jennifer P; Fais, Paolo; Vaiano, Fabio; Bertol, Elisabetta

    2018-05-01

    The growing market of herbal remedies worldwide could pose severe problems to consumers' health due to the possible presence of potentially harmful, undeclared synthetic substances or analogues of prescription drugs. The present work shows a simple but effective approach to unequivocally identify synthetic anorectic compounds in allegedly 'natural' herbal extracts, by exploiting liquid chromatography/time of flight (Q-TOF LC/MS) technology coupled to liquid chromatography/triple quadrupole (LC-MS/MS) confirmation and quantitation. The procedure was applied to five tea herbal extracts and pills sold as coadjutant for weigh loss. The method exploited liquid-liquid sample extraction (LLE) and separation in a C18 (2.1mm×150mm, 1.8μm) column. QTOF acquisitions were carried out both in scan mode and all ion MS/MS mode and results were obtained after search against ad hoc prepared library. Sibutramine, 4-hydroxyamphetamine, caffeine and theophylline were preliminary identified samples. Confirmation and quantitation of the preliminary identified compounds were obtained in LC-MS/MS after preparation of appropriated standards. Sibutramine, caffeine and theophylline were finally confirmed and quantitate. Copyright © 2018 Elsevier B.V. All rights reserved.

  9. Post-acquisition data mining techniques for LC-MS/MS-acquired data in drug metabolite identification.

    Science.gov (United States)

    Dhurjad, Pooja Sukhdev; Marothu, Vamsi Krishna; Rathod, Rajeshwari

    2017-08-01

    Metabolite identification is a crucial part of the drug discovery process. LC-MS/MS-based metabolite identification has gained widespread use, but the data acquired by the LC-MS/MS instrument is complex, and thus the interpretation of data becomes troublesome. Fortunately, advancements in data mining techniques have simplified the process of data interpretation with improved mass accuracy and provide a potentially selective, sensitive, accurate and comprehensive way for metabolite identification. In this review, we have discussed the targeted (extracted ion chromatogram, mass defect filter, product ion filter, neutral loss filter and isotope pattern filter) and untargeted (control sample comparison, background subtraction and metabolomic approaches) post-acquisition data mining techniques, which facilitate the drug metabolite identification. We have also discussed the importance of integrated data mining strategy.

  10. Sensitivity and proportionality assessment of metabolites from microdose to high dose in rats using LC-MS/MS.

    Science.gov (United States)

    Ni, Jinsong; Ouyang, Hui; Seto, Carmai; Sakuma, Takeo; Ellis, Robert; Rowe, Josh; Acheampong, Andrew; Welty, Devin; Szekely-Klepser, Gabriella

    2010-03-01

    The objective of this study was to evaluate the sensitivity requirement for LC-MS/MS as an analytical tool to characterize metabolites in plasma and urine at microdoses in rats and to investigate proportionality of metabolite exposure from a microdose of 1.67 µg/kg to a high dose of 5000 µg/kg for atorvastatin, ofloxacin, omeprazole and tamoxifen. Only the glucuronide metabolite of ofloxacin, the hydroxylation metabolite of omeprazole and the hydration metabolite of tamoxifen were characterized in rat plasma at microdose by LC-MS/MS. The exposure of detected metabolites of omeprazole and tamoxifen appeared to increase in a nonproportional manner with increasing doses. Exposure of ortho- and para-hydroxyatorvastatin, but not atorvastatin and lactone, increased proportionally with increasing doses. LC-MS/MS has demonstrated its usefulness for detecting and characterizing the major metabolites in plasma and urine at microdosing levels in rats. The exposure of metabolites at microdose could not simply be used to predict their exposure at higher doses.

  11. Multiclass determination and confirmation of antibiotic residues in honey using LC-MS/MS.

    Science.gov (United States)

    Lopez, Mayda I; Pettis, Jeffery S; Smith, I Barton; Chu, Pak-Sin

    2008-03-12

    A multiclass method has been developed for the determination and confirmation in honey of tetracyclines (chlortetracycline, doxycycline, oxytetracycline, and tetracycline), fluoroquinolones (ciprofloxacin, danofloxacin, difloxacin, enrofloxacin, and sarafloxacin), macrolides (tylosin), lincosamides (lincomycin), aminoglycosides (streptomycin), sulfonamides (sulfathiazole), phenicols (chloramphenicol), and fumagillin residues using liquid chromatography tandem mass spectrometry (LC-MS/MS). Erythromycin (a macrolide) and monensin (an ionophore) can be detected and confirmed but not quantitated. Honey samples (approximately 2 g) are dissolved in 10 mL of water and centrifuged. An aliquot of the supernatant is used to determine streptomycin. The remaining supernatant is filtered through a fine-mesh nylon fabric and cleaned up by solid phase extraction. After solvent evaporation and sample reconstitution, 15 antibiotics are assayed by LC-MS/MS using electrospray ionization (ESI) in positive ion mode. Afterward, chloramphenicol is assayed using ESI in negative ion mode. The method has been validated at the low part per billion levels for most of the drugs with accuracies between 65 and 104% and coefficients of variation less than 17%. The evaluation of matrix effects caused by honey of different floral origin is presented.

  12. Methods in endogenous steroid profiling - A comparison of gas chromatography mass spectrometry (GC-MS) with supercritical fluid chromatography tandem mass spectrometry (SFC-MS/MS).

    Science.gov (United States)

    Teubel, Juliane; Wüst, Bernhard; Schipke, Carola G; Peters, Oliver; Parr, Maria Kristina

    2018-06-15

    In various fields of endocrinology, the determination of steroid hormones synthesised by the human body plays an important role. Research on central neurosteroids has been intensified within the last years, as they are discussed as biomarkers for various cognitive disorders. Their concentrations in cerebrospinal fluid (CSF) are considered to be regulated independently from peripheral fluids. For that reason, the challenging matrix CSF becomes a very interesting specimen for analysis. Concentrations are expected to be very low and available amount of CSF is limited. Thus, a comprehensive method for very sensitive quantification of a set of analytes as large as possible in one analytical aliquot is desired. However, high structural similarities of the selected panel of 51 steroids and steroid sulfates, including numerous isomers, challenges achievement of chromatographic selectivity. Since decades the analysis of endogenous steroids in various body fluids is mainly performed by gas chromatography (GC) coupled to (tandem) mass spectrometry (MS(/MS)). Due to the structure of the steroids of interest, derivatisation is performed to meet the analytical requirements for GC-MS(/MS). Most of the laboratories use a two-step derivatisation in multi-analyte assays that was already published in the 1980s. However, for some steroids this elaborate procedure yields multiple isomeric derivatives. Thus, some laboratories utilize (ultra) high performance liquid chromatography ((U)HPLC)-MS/MS as alternative but, even UHPLC is not able to separate some of the isomeric pairs. Supercritical fluid chromatography (SFC) as an orthogonal separation technique to GC and (U)HPLC may help to overcome these issues. Within this project the two most promising methods for endogenous steroid profiling were investigated and compared: the "gold standard" GC-MS and the orthogonal separation technique SFC-MS/MS. Different derivatisation procedures for gas chromatographic detection were explored and the

  13. Characterization of Proteins Present in Isolated Senile Plaques from Alzheimer's Diseased Brains by MALDI-TOF MS with MS/MS.

    Science.gov (United States)

    Kelley, Andrea R; Perry, George; Bach, Stephan B H

    2018-04-18

    The increase of insoluble senile plaques in the brain is a primary hallmark of Alzheimer's disease. The usefulness of matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) with tandem MS for the characterization of senile plaques from AD brains and the relevance of the components identified to furthering AD research using MS is discussed. Thirty-three components were reproducibly observed within tryptic aliquots of senile plaques from two different AD brains after sample preparation optimization. Additionally, this is one of the first accounts of LIFT being utilized for the direct sequencing of peptides from isolated senile plaques. While many of the species observed coisolated within senile plaques have been linked to AD etiology, if only speculatively, this is the first instance that many of them have been demonstrated to be a part of the plaques themselves. This work is the first step in determining the potential roles that the species may have in the aggregation or proliferation of the plaques.

  14. Short Communication: Testosterone Measured with an Automatic Immunoassay Compares Reasonbly Well to Results Obtained by LC-MS/MS

    DEFF Research Database (Denmark)

    Knudsen, Cindy Søndersø; Højskov, Carsten Schriver; Møller, Holger Jon

    2016-01-01

    Background: Previous studies have reported problems measuring testosterone with immunological assays. Here we explore an automatic second generation immunoassay compared to a LC-MS/MS method. Methods: We collected blood samples from 76 women and measured testosterone, progesterone, gender...... hormonebinding globulin (SHBG), and albumin employing Cobas e601/c501. Testosterone, androstenedione (andro), dehydroepiandrosterone sulphate (DHEAS), and 17-hydroxyprogesterone (17-OHP) concentrations were measured employing LC-MS/MS. We evaluated the difference between testosterone measured by the two methods...... and examined the potential interference from the selected steroids and bindings proteins. Results: Testosterone concentrations measured by the two methods yielded: Cobas e601 = 1.240 x (LC-MS/MS) - 0.197, r = 0.84, for testosterone concentrations between 0.22 - 4.9 nmol/L. A positive correlation was observed...

  15. Contributions in the Preparation and Processing of Composite Material Type Silumin 3 - Reinforced Matrix with S235JR Steel Mesh

    Directory of Open Access Journals (Sweden)

    Remus Belu-Nica

    2015-07-01

    Full Text Available In the paper are presented concrete data on developing technological batches of metal composite material (MCM type Silumin 3-reinforced matrix with steel mesh S235JR, with the indicating of the parameter and of the distinct stages of work. The samples from prepared batches were cut along and across by water jet abrasive process and were subjected to a destructive testing program and microstructural examination, obtaining results in concordance with the desired quality. The abrasive material used for cut was GMA granite with the average mesh of 80, the particle size ranging between 150-300 µm, density 2300 kg/m3 and melting point 1240°C.

  16. Metabolism of the new psychoactive substances N,N-diallyltryptamine (DALT) and 5-methoxy-DALT and their detectability in urine by GC-MS, LC-MSn, and LC-HR-MS-MS.

    Science.gov (United States)

    Michely, Julian A; Helfer, Andreas G; Brandt, Simon D; Meyer, Markus R; Maurer, Hans H

    2015-10-01

    N,N-Diallyltryptamine (DALT) and 5-methoxy-DALT (5-MeO-DALT) are synthetic tryptamine derivatives commonly referred to as so-called new psychoactive substances (NPS). They have psychoactive effects that may be similar to those of other tryptamine derivatives. The objectives of this work were to study the metabolic fate and detectability, in urine, of DALT and 5-MeO-DALT. For metabolism studies, rat urine obtained after high-dose administration was prepared by precipitation and analyzed by liquid chromatography-high-resolution mass spectrometry (LC-HR-MS-MS). On the basis of the metabolites identified, several aromatic and aliphatic hydroxylations, N-dealkylation, N-oxidation, and combinations thereof are proposed as the main metabolic pathways for both compounds. O-Demethylation of 5-MeO-DALT was also observed, in addition to extensive glucuronidation or sulfation of both compounds after phase I transformation. The cytochrome P450 (CYP) isoenzymes predominantly involved in DALT metabolism were CYP2C19, CYP2D6, and CYP3A4; those mainly involved in 5-MeO-DALT metabolism were CYP1A2, CYP2C19, CYP2D6, and CYP3A4. For detectability studies, rat urine was screened by GC-MS, LC-MS(n), and LC-HR-MS-MS after administration of low doses. LC-MS(n) and LC-HR-MS-MS were deemed suitable for monitoring consumption of both compounds. The most abundant targets were a ring hydroxy metabolite of DALT, the N,O-bis-dealkyl metabolite of 5-MeO-DALT, and their glucuronides. GC-MS enabled screening of DALT by use of its main metabolites only.

  17. Screening of veterinary drug residues in food by LC-MS/MS. Background and challenges.

    Science.gov (United States)

    Delatour, Thierry; Racault, Lucie; Bessaire, Thomas; Desmarchelier, Aurélien

    2018-04-01

    Regulatory agencies and government authorities have established maximum residue limits (MRL) in various food matrices of animal origin for supporting governments and food operators in the monitoring of veterinary drug residues in the food chain, and ultimately in the consumer's plate. Today, about 200 veterinary drug residues from several families, mainly with antibiotic, antiparasitic or antiinflammatory activities, are regulated in a variety of food matrices such as milk, meat or egg. This article provides a review of the regulatory framework in milk and muscle including data from Codex Alimentarius, Europe, the U.S.A., Canada and China for about 220 veterinary drugs. The article also provides a comprehensive overview of the challenge for food control, and emphasizes the pivotal role of liquid chromatography-mass spectrometry (LC-MS), either in tandem with quadrupoles (LC-MS/MS) or high resolution MS (LC-HRMS), for ensuring an adequate consumer protection combined with an affordable cost. The capability of a streamlined LC-MS/MS platform for screening 152 veterinary drug residues in a broad range of raw materials and finished products is highlighted in a production line perspective. The rationale for a suite of four methods intended to achieve appropriate performance in terms of scope and sensitivity is presented. Overall, the platform encompasses one stream for the determination of 105 compounds in a run (based on acidic QuEChERS-like), plus two streams for 23 β-lactams (alkaline QuEChERS-like) and 10 tetracyclines (low-temperature partitioning), respectively, and a dedicated stream for 14 aminoglycosides (molecularly-imprinted polymer).

  18. The role of EBV in MS pathogenesis

    DEFF Research Database (Denmark)

    Christensen, Tove

    2006-01-01

    Environmental factors operate on a background of genetic susceptibility in the pathogenesis of MS. Human herpesviruses, notably Epstein-Barr virus (EBV), and human endogenous retroviruses are factors associated with MS. EBV association is found in epidemiological surveys where late EBV infection...... confers a higher risk of MS, and EBV reactivation also appears to be linked to disease activity in early MS. MS patients have elevated anti-EBV antibody responses, both in serum and cerebrospinal fluid. Molecular mimicry is found between certain EBV and myelin epitopes in the cell-mediated immune response....... EBV cannot stand alone as a causal factor of MS, but is likely to play an indirect role as an activator of the underlying disease process....

  19. Wide-scope screening of pesticides in fruits and vegetables using information-dependent acquisition employing UHPLC-QTOF-MS and automated MS/MS library searching.

    Science.gov (United States)

    Wang, Zhibin; Cao, Yanzhong; Ge, Na; Liu, Xiaomao; Chang, Qiaoying; Fan, Chunlin; Pang, Guo-Fang

    2016-11-01

    This paper presents an application of ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-QTOF-MS) for simultaneous screening and identification of 427 pesticides in fresh fruit and vegetable samples. Both full MS scan mode for quantification, and an artificial-intelligence-based product ion scan mode information-dependent acquisition (IDA) providing automatic MS to MS/MS switching of product ion spectra for identification, were conducted by one injection. A home-in collision-induced-dissociation all product ions accurate mass spectra library containing more than 1700 spectra was developed prior to actual application. Both qualitative and quantitative validations of the method were carried out. The result showed that 97.4 % of the pesticides had the screening detection limit (SDL) less than 50 μg kg -1 and more than 86.7 % could be confirmed by accurate MS/MS spectra embodied in the home-made library. Meanwhile, calibration curves covering two orders of magnitude were performed, and they were linear over the concentration range studied for the selected matrices (from 5 to 500 μg kg -1 for most of the pesticides). Recoveries between 80 and 110 % in four matrices (apple, orange, tomato, and spinach) at two spiked levels, 10 and 100 μg kg -1 , was 88.7 or 86.8 %. Furthermore, the overall relative standard deviation (RSD, n = 12) for 94.3 % of the pesticides in 10 μg kg -1 and 98.1 % of the pesticides in 100 μg kg -1 spiked levels was less than 20 %. In order to validate the suitability for routine analysis, the method was applied to 448 fruit and vegetable samples purchased in different local markets. The results show 83.3 % of the analyzed samples have positive findings (higher than the limits of identification and quantification), and 412 commodity-pesticide combinations are identified in our scope. The approach proved to be a cost-effective, time-saving and powerful strategy for routine large

  20. Determination of 48 fragrance allergens in toys using GC with ion trap MS/MS.

    Science.gov (United States)

    Lv, Qing; Zhang, Qing; Li, Wentao; Li, Haiyu; Li, Pi; Ma, Qiang; Meng, Xianshuang; Qi, Meiling; Bai, Hua

    2013-11-01

    This paper presents a method for the simultaneous determination of 48 fragrance allergens in four types of toys (plastic toys, play clays, plush toys, and paper toys) based on GC with ion trap MS/MS. Compared with single-stage MS, MS/MS is superior in terms of the qualification and quantification of a large range of compounds in complicated matrices. Procedures for extraction and purification were optimized for each toy type. The method proved to be linear over a wide range of concentrations for all analytes with correlation coefficients between 0.9768 and 0.9999. Validation parameters, namely, LODs and LOQs, ranged from 0.005-5.0 and from 0.02-20 mg/kg, respectively. Average recoveries of target compounds (spiked at three concentration levels) were in the range of 79.5-109.1%. Intraday and interday repeatabilities of the proposed method varied from 0.7-10.5% and from 3.1-13.4%, respectively. The proposed method was used to monitor fragrance allergens in commercial toy products. Our findings indicate that this method is an accurate and effective technique for analyzing fragrance allergens in materials composed of complex components. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Ellagitannin composition of blackberry as determined by HPLC-ESI-MS and MALDI-TOF-MS.

    Science.gov (United States)

    Hager, Tiffany J; Howard, Luke R; Liyanage, Rohana; Lay, Jackson O; Prior, Ronald L

    2008-02-13

    Blackberries ( Rubus sp.) were evaluated by high-performance liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS) and matrix-assisted laser desorption/ionization-time-of-flight mass spectrometry (MALDI-TOF-MS) to identify the ellagitannins present in flesh, torus (receptacle tissue), and seeds. Most ellagitannins were present (or detectable) only in seed tissues. Ellagitannins identified by HPLC-ESI-MS in the seeds included pedunculagin, casuarictin/potentillin, castalagin/vescalagin, lambertianin A/sanguiin H-6, lambertianin C, and lambertianin D. For several of the ellagitannins, isomeric separation was also obtained. The MALDI-TOF-MS analysis was primarily utilized to evaluate and identify high molecular mass (>1000 Da) ellagitannins. The MALDI analysis verified the presence of the ellagitannins identified by HPLC-ESI-MS including lambertianin A/sanguiin H-6, lambertianin C, and lambertianin D, but the analysis also indicated the presence of several other compounds that were most likely ellagitannins based on the patterns observed in the masses (i.e., loss or addition of a gallic acid moiety to a known ellagitannin). This study determined the presence of several possible isomeric forms of ellagitannins previously unidentified in fruit and presents a possible analytical HPLC method for the analysis of the major ellagitannins present in the fruit.

  2. Life history of the gall-maker Eugeniamyia dispar Maia, Mendonça-Jr. & Romanowski, 1996 (Diptera, Cecidomyiidae

    Directory of Open Access Journals (Sweden)

    M. de S.,Jr. MENDONÇA

    Full Text Available The development of the galls of the midge Eugeniamyia dispar Maia, Mendonça-Jr. & Romanowski, 1996 (Diptera: Cecidomyiidae was monitored weekly on its host plant, Eugenia uniflora (Myrtaceae. The work was carried out in the urban area of Porto Alegre, RS, Brazil, from October 1993 to September 1995. Galls were collected from the field and raised in the laboratory to obtain adults. The females oviposit on young leaves of the host plant, with the first instar larvae inducing the gall, which is unilocular. The last instar larvae drop to the soil to pupate and later emerge as adults. The galls occur from late August to early June, when young leaves of the host can be found, with populations peaking during the summer. So far this species is only known from the two southernmost states of Brazil (RS and SC.

  3. Life history of the gall-maker Eugeniamyia dispar Maia, Mendonça-Jr. & Romanowski, 1996 (Diptera, Cecidomyiidae).

    Science.gov (United States)

    Mendonça, M de S; Romanowski, H P

    2002-05-01

    The development of the galls of the midge Eugeniamyia dispar Maia, Mendonça-Jr. & Romanowski, 1996 (Diptera: Cecidomyiidae) was monitored weekly on its host plant, Eugenia uniflora (Myrtaceae). The work was carried out in the urban area of Porto Alegre, RS, Brazil, from October 1993 to September 1995. Galls were collected from the field and raised in the laboratory to obtain adults. The females oviposit on young leaves of the host plant, with the first instar larvae inducing the gall, which is unilocular. The last instar larvae drop to the soil to pupate and later emerge as adults. The galls occur from late August to early June, when young leaves of the host can be found, with populations peaking during the summer. So far this species is only known from the two southernmost states of Brazil (RS and SC).

  4. Matrix effects break the LC behavior rule for analytes in LC-MS/MS analysis of biological samples.

    Science.gov (United States)

    Fang, Nianbai; Yu, Shanggong; Ronis, Martin Jj; Badger, Thomas M

    2015-04-01

    High-performance liquid chromatography (HPLC) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) are generally accepted as the preferred techniques for detecting and quantitating analytes of interest in biological matrices on the basis of the rule that one chemical compound yields one LC-peak with reliable retention time (Rt.). However, in the current study, we have found that under the same LC-MS conditions, the Rt. and shape of LC-peaks of bile acids in urine samples from animals fed dissimilar diets differed significantly among each other. To verify this matrix effect, 17 authentic bile acid standards were dissolved in pure methanol or in methanol containing extracts of urine from pigs consuming either breast milk or infant formula and analyzed by LC-MS/MS. The matrix components in urine from piglets fed formula significantly reduced the LC-peak Rt. and areas of bile acids. This is the first characterization of this matrix effect on Rt. in the literature. Moreover, the matrix effect resulted in an unexpected LC behavior: one single compound yielded two LC-peaks, which broke the rule of one LC-peak for one compound. The three bile acid standards which exhibited this unconventional LC behavior were chenodeoxycholic acid, deoxycholic acid, and glycocholic acid. One possible explanation for this effect is that some matrix components may have loosely bonded to analytes, which changed the time analytes were retained on a chromatography column and interfered with the ionization of analytes in the MS ion source to alter the peak area. This study indicates that a comprehensive understanding of matrix effects is needed towards improving the use of HPLC and LC-MS/MS techniques for qualitative and quantitative analyses of analytes in pharmacokinetics, proteomics/metabolomics, drug development, and sports drug testing, especially when LC-MS/MS data are analyzed by automation software where identification of an analyte is based on its exact molecular weight and Rt

  5. IsoMS: automated processing of LC-MS data generated by a chemical isotope labeling metabolomics platform.

    Science.gov (United States)

    Zhou, Ruokun; Tseng, Chiao-Li; Huan, Tao; Li, Liang

    2014-05-20

    A chemical isotope labeling or isotope coded derivatization (ICD) metabolomics platform uses a chemical derivatization method to introduce a mass tag to all of the metabolites having a common functional group (e.g., amine), followed by LC-MS analysis of the labeled metabolites. To apply this platform to metabolomics studies involving quantitative analysis of different groups of samples, automated data processing is required. Herein, we report a data processing method based on the use of a mass spectral feature unique to the chemical labeling approach, i.e., any differential-isotope-labeled metabolites are detected as peak pairs with a fixed mass difference in a mass spectrum. A software tool, IsoMS, has been developed to process the raw data generated from one or multiple LC-MS runs by peak picking, peak pairing, peak-pair filtering, and peak-pair intensity ratio calculation. The same peak pairs detected from multiple samples are then aligned to produce a CSV file that contains the metabolite information and peak ratios relative to a control (e.g., a pooled sample). This file can be readily exported for further data and statistical analysis, which is illustrated in an example of comparing the metabolomes of human urine samples collected before and after drinking coffee. To demonstrate that this method is reliable for data processing, five (13)C2-/(12)C2-dansyl labeled metabolite standards were analyzed by LC-MS. IsoMS was able to detect these metabolites correctly. In addition, in the analysis of a (13)C2-/(12)C2-dansyl labeled human urine, IsoMS detected 2044 peak pairs, and manual inspection of these peak pairs found 90 false peak pairs, representing a false positive rate of 4.4%. IsoMS for Windows running R is freely available for noncommercial use from www.mycompoundid.org/IsoMS.

  6. Changing activity in MS lesions

    International Nuclear Information System (INIS)

    Kermode, A.G.; Tofts, P.S.; Thompson, A.J.; Rudge, P.; MacManus, D.G.; Kendall, B.E.; Moseley, I.F.; Kingsley, D.P.E.; McDonald, W.I.

    1989-01-01

    Gd-DTPA enhanced T1 weighted MRI is a discriminating test for a defective blood-brain barrier, with MS lesions showing considerable variation in the pattern of enhancement. Since little is known of the changes in the blood-brain barrier in the active plaque over time, the natural history of blood-brain barrier disturbance in the MS lesion was examined to confirm earlier reports that Gd-DTPA enhancement is a consistent early event in new lesions of relapsing/remitting MS. This knowledge is essential for the use of MRI in monitoring treatment. (author). 9 refs

  7. Postmortem Kanda LC-MS MS ile Yasadışı Madde Taraması 62 Postmortem Adli Olguda Uygulanması

    Directory of Open Access Journals (Sweden)

    Serap Annette Akgür

    2007-04-01

    Full Text Available Biyolojik örneklerdeki yasadışı madde taraması adli olaylarda büyük bir öneme sahiptir. Kan veya plazma, madde derişim-leri ile bu maddelerin farmakolojik etkileri arasında iyi bir korelasyonun bulunması nedeniyle genellikle tercih edilen materyallerdir. Yasadışı madde analizinde, birçok laboratuar immunoassay yöntemleri ile tarama ve Gaz Kromatografi-Kütle Spektrometresi (GC-MS ile doğrulama şeklinde bir uygulama yapmaktadır. Bununla birlikte, sıvı kromatografi tekniklerinin gelişmesiyle birlikte Sıvı Kromatografisi-Kütle Spektrometresi (LC-MS ve tandem LC-MS (LC-MS/MS birleştirilmiş tekniklerinde özellikle polar ve ısıya dayanıksız olan maddelerin nitel ve nicel analiz amaçlı olarak kullanımı zamanla artmaktadır. Bu çalışmada, LC-ESI (Electrospray İonisation-MS/MS de morfin, (±-amfetamin, (+-metamfetamin, kokain, benzolekgonin, kokaetilen ve (--ll-nor-9-karboksi-t9-THC maddeleri taranmış ve tayin edilmiştir. Sonuç olarak, postmortem kanda uygulanabilecek, türevlendirme işlemine gerek duymayan, duyarlı ve seçimli olarak, çok düşük düzeylerdeki maddelerin doğru ve kesin olarak saptanmasını sağlayacak, LC-MS/MS yöntemi geliştirilmiş ve 62 postmortem adli olguya başarıyla uygulanmıştır. Anahtar kelimeler: Yasadışı madde, tarama, LC/MS/MS, postmortem kan

  8. RAId_aPS: MS/MS analysis with multiple scoring functions and spectrum-specific statistics.

    Science.gov (United States)

    Alves, Gelio; Ogurtsov, Aleksey Y; Yu, Yi-Kuo

    2010-11-16

    Statistically meaningful comparison/combination of peptide identification results from various search methods is impeded by the lack of a universal statistical standard. Providing an E-value calibration protocol, we demonstrated earlier the feasibility of translating either the score or heuristic E-value reported by any method into the textbook-defined E-value, which may serve as the universal statistical standard. This protocol, although robust, may lose spectrum-specific statistics and might require a new calibration when changes in experimental setup occur. To mitigate these issues, we developed a new MS/MS search tool, RAId_aPS, that is able to provide spectrum-specific-values for additive scoring functions. Given a selection of scoring functions out of RAId score, K-score, Hyperscore and XCorr, RAId_aPS generates the corresponding score histograms of all possible peptides using dynamic programming. Using these score histograms to assign E-values enables a calibration-free protocol for accurate significance assignment for each scoring function. RAId_aPS features four different modes: (i) compute the total number of possible peptides for a given molecular mass range, (ii) generate the score histogram given a MS/MS spectrum and a scoring function, (iii) reassign E-values for a list of candidate peptides given a MS/MS spectrum and the scoring functions chosen, and (iv) perform database searches using selected scoring functions. In modes (iii) and (iv), RAId_aPS is also capable of combining results from different scoring functions using spectrum-specific statistics. The web link is http://www.ncbi.nlm.nih.gov/CBBresearch/Yu/raid_aps/index.html. Relevant binaries for Linux, Windows, and Mac OS X are available from the same page.

  9. UFLC-ESI-MS/MS analysis of multiple mycotoxins in medicinal and edible Areca catechu.

    Science.gov (United States)

    Liu, Hongmei; Luo, Jiaoyang; Kong, Weijun; Liu, Qiutao; Hu, Yichen; Yang, Meihua

    2016-05-01

    A robust, sensitive and reliable ultra fast liquid chromatography combined with electrospray ionization tandem mass spectrometry (UFLC-ESI-MS/MS) was optimized and validated for simultaneous identification and quantification of eleven mycotoxins in medicinal and edible Areca catechu, based on one-step extraction without any further clean-up. Separation and quantification were performed in both positive and negative modes under multiple reaction monitoring (MRM) in a single run with zearalanone (ZAN) as internal standard. The chromatographic conditions and MS/MS parameters were carefully optimized. Matrix-matched calibration was recommended to reduce matrix effects and improve accuracy, showing good linearity within wide concentration ranges. Limits of quantification (LOQ) were lower than 50 μg kg(-1), while limits of detection (LOD) were in the range of 0.1-20 μg kg(-1). The accuracy of the developed method was validated for recoveries, ranging from 85% to 115% with relative standard deviation (RSD) ≤14.87% at low level, from 75% to 119% with RSD ≤ 14.43% at medium level and from 61% to 120% with RSD ≤ 13.18% at high level, respectively. Finally, the developed multi-mycotoxin method was applied for screening of these mycotoxins in 24 commercial samples. Only aflatoxin B2 and zearalenone were found in 2 samples. This is the first report on the application of UFLC-ESI(+/-)-MS/MS for multi-class mycotoxins in A. catechu. The developed method with many advantages of simple pretreatment, rapid determination and high sensitivity is a proposed candidate for large-scale detection and quantification of multiple mycotoxins in other complex matrixes. Copyright © 2016 Elsevier Ltd. All rights reserved.

  10. Non-enzymolytic adenosine barcode-mediated dual signal amplification strategy for ultrasensitive protein detection using LC-MS/MS.

    Science.gov (United States)

    Yang, Wen; Li, Tengfei; Shu, Chang; Ji, Shunli; Wang, Lei; Wang, Yan; Li, Duo; Mtalimanja, Michael; Sun, Luning; Ding, Li

    2018-05-10

    A method is described for the determination of proteins with LC-MS/MS enabled by a small molecule (adenosine) barcode and based on a double-recognition sandwich structure. The coagulation protein thrombin was chosen as the model analyte. Magnetic nanoparticles were functionalized with aptamer29 (MNP/apt29) and used to capture thrombin from the samples. MNP/apt29 forms a sandwich with functionalized gold nanoparticles modified with (a) aptamer15 acting as thrombin-recognizing element and (b) a large number of adenosine as mass barcodes. The sandwich formed (MNP/apt29-thrombin-apt15/AuNP/adenosine) can ben magnetically separated from the sample. Mass barcodes are subsequently released from the sandwiched structure for further analysis by adding 11-mercaptoundecanoic acid. Adenosine is then detected by LC-MS/MS as it reflects the level of thrombin with impressively amplified signal. Numerous adenosines introduced into the sandwich proportional to the target concentration further amplify the signal. Under optimized conditions, the response is linearly proportional to the thrombin concentration in the range of 0.02 nM to 10 nM, with a detection limit of 9 fM. The application of this method to the determination of thrombin in spiked plasma samples gave recoveries that ranged from 92.3% to 104.7%. Graphical abstract Schematic representation of a method for the determination of thrombin with LC-MS/MS. The method is based on a double-recognition sandwiched structure. With LC-MS/MS, mass barcodes (adenosine) are detected to quantify thrombin, which amplifies the detection signal impressively.

  11. Identification of the Chemical Constituents in Simiao Wan and Rat Plasma after Oral Administration by GC-MS and LC-MS

    Directory of Open Access Journals (Sweden)

    Yunshuang Fan

    2017-01-01

    Full Text Available Simiao Wan (SMW, an important multiherbal formula used in traditional Chinese medicine, is extensively used to treat rheumatoid arthritis. However, the knowledge of the bioactive components of SMW remains unclear. Thus, gas chromatography–mass spectrometry (GC-MS and liquid chromatography–mass spectrometry (LC-MS were used to analyze the chemical constituents of volatile and nonvolatile extracts of SMW, as well as its absorbed components in rat plasma after oral SMW administration. Identification of several compounds was enabled by comparison of retention times, MS spectra, and MS/MS spectral data with the standard substance and reference materials reported in the literature. In the volatile extracts, GC-MS identified 26 compounds in vitro, three of which observed in blood by GC-MS. In the nonvolatile extracts, LC-MS identified 49 compounds in SMW; 18 compounds containing 7 prototype compounds, 5 metabolites, and 6 unknown compounds were absorbed by blood. The proposed GC-MS and LC-MS method was appropriate not only for the rapid screening and identification of multiple components of an SMW extract but also for screening its bioactive constituents in vivo. The proposed method could be a promising tool for the quality control of other Chinese herbal medicines.

  12. Determination of chlormequat in pig serum and sow milk by LC-MS/MS.

    Science.gov (United States)

    Poulsen, M E; Christensen, H B; Sørensen, M T; Leffers, H; Andersen, J H

    2007-11-01

    Chlormequat is a plant growth regulator widely used on cereals, and there is general concern that it may impair human fertility. A LC-MS/MS method for the analysis of chlormequat in milk and serum was developed and validated in connection with an investigation on the effect of chlormequat on pig reproduction. Validation of the method was based on recovery tests at three spiking levels, determined as double determinations and repeated at least four times. Samples were extracted with methanol-water-acetic acid, centrifuged, filtrated and determined by LC-MS/MS. The mean recoveries were in the range 80-110%, and the LOD was 0.2 ng/g for serum and 0.3 ng/g for milk. The values for repeatability and reproducibility were within 2/3 of the limits given by the Horwitz equation. Samples of pig serum (59) and sow milk (27) were analyzed using the method. Chlormequat was determined in four milk samples in the range of 0.4 ng/g to 1.2 ng/g and in all serum samples in the range of 0.2 ng/g-4.0 ng/g.

  13. Determination of selected bisphenols, parabens and estrogens in human plasma using LC-MS/MS

    Czech Academy of Sciences Publication Activity Database

    Kolatorova Sosvorova, L.; Chlupacova, T.; Vitku, J.; Vlk, Martin; Heráček, J.; Stárka, L.; Šaman, David; Šimková, M.; Hampl, R.

    2017-01-01

    Roč. 174, NOV 1 (2017), s. 21-28 ISSN 0039-9140 Institutional support: RVO:61389030 ; RVO:61388963 Keywords : Alternative bisphenol * Bisphenol A * Bisphenol F * Endocrine disruptor * lc-ms/ms * Paraben Subject RIV: CC - Organic Chemistry OBOR OECD: Analytical chemistry; Organic chemistry (UOCHB-X) Impact factor: 4.162, year: 2016

  14. J-R Fracture Resistance of SA533 Gr.B-Cl.1 Steel for Reactor Pressure Vessel

    Energy Technology Data Exchange (ETDEWEB)

    Yoon, Ji-Hyun; Hong, Seokmin; Lee, Bong-Sang [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

    2016-10-15

    A rolled plate might show different mechanical behaviors from a forging, even though they contain same chemical compositions. Furthermore, it is known that the fracture behavior of a rolled plate is very sensitive to material orientation comparing to a forging. In this study, the J-R fracture resistances of SA533 Gr.B-Cl.1 plate were measured at reactor operating temperature and the material orientation sensitivity was discussed. The decrease of fracture resistance of this kind of low alloy steel at an elevated temperature is known as the effect of dynamic strain aging (DSA). It was attributed to that the carbides and grains elongated to primary rolling direction, so that the aspect ratio of carbides and grains in the specimen with T-L orientation is larger. Generally, the hard second phase could take a roll of trigger point of unstable fracture. It is needed that the fracture surfaces of the tested specimens to be examined profoundly.

  15. Desenvolvimento pós-embrionário do intestino anterior de Dermatobia hominis (Linnaeus Jr. (Diptera, Cuterebridae Post-embryonic development of Dermatobia hominis (Linnaeus Jr. (Diptera, Cuterebridae foregut

    Directory of Open Access Journals (Sweden)

    Ana Maria Vieira

    2001-03-01

    Full Text Available Foregut in D. hominis (Linnaeus Jr., 1781 as the majority of the larval Diptera somatic tissue, is made up of polytenic cells, and grows at the expenses of the polytenization of its nuclei followed by the increase in size of each cell. The oesophagus, of ectodermic origem, is interiorly covered by a chitinous squamous epithelium that rests upon a very thin basal lamina. This sheet is surrounded by thick muscle bundles. The oesophagus intussuscepts the midgut forming the cardia. The cardia, with three epithelial layers: two internal ones, of ectodermal origin and one external of endodermic origin. At the anterior portion of the cardia, between these two types of epithelium, there is a cluster of small, non polytenic cells, forming the imaginal disk of the foregut. Metamoiphosis begins at the end of the larval period with signs of nuclear degeneration of all the polytenic cells, as well as the increase in number of the imaginal disk ones. The oesophagic portion intussuscepted into the cardia, everts; its cells suffer apoptosis and are replaced by the new cells growing from the imaginal disk. The external layer cells also degenerate and are pinched off into the lumen of the very anterior portion of the midgut. The newly formed oesophagus intussuscepts "de novo" to form the two internal layers of the adult cardia. At the same time the midgut regenerative cells grow anteriorly to form the new external layer of the adult cardia.

  16. Profiling the Oxylipin and Endocannabinoid Metabolome by UPLC-ESI-MS/MS in Human Plasma to Monitor Postprandial Inflammation.

    Science.gov (United States)

    Gouveia-Figueira, Sandra; Späth, Jana; Zivkovic, Angela M; Nording, Malin L

    2015-01-01

    Bioactive lipids, including oxylipins, endocannabinoids, and related compounds may function as specific biochemical markers of certain aspects of inflammation. However, the postprandial responsiveness of these compounds is largely unknown; therefore, changes in the circulating oxylipin and endocannabinoid metabolome in response to a challenge meal were investigated at six occasions in a subject who freely modified her usual diet. The dietary change, and especially the challenge meal itself, represented a modification of precursor fatty acid status, with expectedly subtle effects on bioactive lipid levels. To detect even the slightest alteration, highly sensitive ultra-performance liquid chromatography (UPLC) coupled to electrospray ionization (ESI) tandem mass spectrometry (MS/MS) methods for bioactive lipid profiling was employed. A previously validated UPLC-ESI-MS/MS method for profiling the endocannabinoid metabolome was used, while validation of an UPLC-ESI-MS/MS method for oxylipin analysis was performed with acceptable outcomes for a majority of the parameters according to the US Food and Drug Administration guidelines for linearity (0.9938 metabolome, caused by changes in diet and ii) responsiveness to a challenge meal for a subset of the oxylipin and endocannabinoid metabolome. To summarize, we have shown proof-of-concept of our UPLC-ESI-MS/MS bioactive lipid protocols for the purpose of monitoring subtle shifts, and thereby useful to address lipid-mediated postprandial inflammation.

  17. Direct, rapid quantitative analyses of BVOCs using SIFT-MS and PTR-MS obviating sample collection

    Czech Academy of Sciences Publication Activity Database

    Smith, D.; Španěl, Patrik

    2011-01-01

    Roč. 30, č. 7 (2011), s. 945-959 ISSN 0165-9936 Institutional research plan: CEZ:AV0Z40400503 Keywords : SIFT-MS * PTR-MS * Absolute quantification Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 6.273, year: 2011

  18. Lycopene Supplementation in the Complementary Management of PSA Failure: A Randomized Placebo-Controlled Trial for Prostate Cancer Survivors

    Science.gov (United States)

    2007-01-01

    N Wells, JA Smith, Jr. and MS Cookson. Intrarectal Lidocaine During Transrectal Prostate Biopsy. Journal of Urology 166: 2178-2180, 2001. -113...steroid hormone and growth factor activation/ synthesis and signaling in the prostate (55, 56). These ability to reduce normal and cancerous cell

  19. Factors Associated with Neurologists' Provision of MS Patient Care

    Science.gov (United States)

    Halpern, Michael T.; Teixeira-Poit, Stephanie M.; Kane, Heather; Frost, Corey; Keating, Michael; Olmsted, Murrey

    2014-01-01

    Neurologists are central to providing quality care for individuals with MS. However, neurologist shortages may restrict access to care for MS patients. To examine factors influencing neurologists' provision of MS care, we surveyed 1,700 US neurologists to assess demographic/practice characteristics, training, and attitudes toward MS care. The study population consisted of 573 respondents: 87 (15.2%) MS subspecialists and 486 (84.8%) “other neurologists,” including subspecialists in other neurology areas (i.e., non-MS) and general neurologists. MS subspecialists indicating they “enjoy interacting with MS patients” had a significantly greater rate of MS patients seen per week. In separate analyses of the “other neurologists” group, the rate of MS patients seen was lower among neurologists in university-based groups or those practicing in major cities; female neurologists; and neurologists who indicated lack of sufficient knowledge regarding MS patient care. Rates of MS patients seen were significantly greater for other neurologists who agreed that MS care involved “ability to improve patient outcomes and quality of life”; “dynamic area with evolving treatment options”; and “enjoy interacting with MS patients.” Understanding factors influencing MS patient care by neurologists and developing policies for appropriate access to care is critical for optimal outcomes among this population. PMID:24949203

  20. Factors Associated with Neurologists’ Provision of MS Patient Care

    Directory of Open Access Journals (Sweden)

    Michael T. Halpern

    2014-01-01

    Full Text Available Neurologists are central to providing quality care for individuals with MS. However, neurologist shortages may restrict access to care for MS patients. To examine factors influencing neurologists’ provision of MS care, we surveyed 1,700 US neurologists to assess demographic/practice characteristics, training, and attitudes toward MS care. The study population consisted of 573 respondents: 87 (15.2% MS subspecialists and 486 (84.8% “other neurologists,” including subspecialists in other neurology areas (i.e., non-MS and general neurologists. MS subspecialists indicating they “enjoy interacting with MS patients” had a significantly greater rate of MS patients seen per week. In separate analyses of the “other neurologists” group, the rate of MS patients seen was lower among neurologists in university-based groups or those practicing in major cities; female neurologists; and neurologists who indicated lack of sufficient knowledge regarding MS patient care. Rates of MS patients seen were significantly greater for other neurologists who agreed that MS care involved “ability to improve patient outcomes and quality of life”; “dynamic area with evolving treatment options”; and “enjoy interacting with MS patients.” Understanding factors influencing MS patient care by neurologists and developing policies for appropriate access to care is critical for optimal outcomes among this population.

  1. What Is in Your Wallet? Quantitation of Drugs of Abuse on Paper Currency with a Rapid LC-MS/MS Method

    Science.gov (United States)

    Parker, Patrick D.; Beers, Brandon; Vergne, Matthew J.

    2017-01-01

    Laboratory experiments were developed to introduce students to the quantitation of drugs of abuse by high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). Undergraduate students were introduced to internal standard quantitation and the LC-MS/MS method optimization for cocaine. Cocaine extracted from paper currency was…

  2. Comparison of piracetam measured with HPLC-DAD, HPLC-ESI-MS, DIP-APCI-MS, and a newly developed and optimized DIP-ESI-MS.

    Science.gov (United States)

    Lenzen, Claudia; Winterfeld, Gottfried A; Schmitz, Oliver J

    2016-06-01

    The direct inlet probe-electrospray ionization (DIP-ESI) presented here was based on the direct inlet probe-atmospheric pressure chemical ionization (DIP-APCI) developed by our group. It was coupled to an ion trap mass spectrometer (MS) for the detection of more polar compounds such as degradation products from pharmaceuticals. First, the position of the ESI tip, the gas and solvent flow rates, as well as the gas temperature were optimized with the help of the statistic program Minitab® 17 and a caffeine standard. The ability to perform quantitative analyses was also tested by using different concentrations of caffeine and camphor. Calibration curves with a quadratic calibration regression of R (2) = 0.9997 and 0.9998 for caffeine and camphor, respectively, were obtained. The limit of detection of 2.5 and 1.7 ng per injection for caffeine and camphor were determined, respectively. Furthermore, a solution of piracetam was used to compare established analytical methods for this drug and its impurities such as HPLC-diode array detector (DAD) and HPLC-ESI-MS with the DIP-APCI and the developed DIP-ESI. With HPLC-DAD and 10 μg piracetam on column, no impurity could be detected. With HPLC-ESI-MS, two impurities (A and B) were identified with only 4.6 μg piracetam on column, while with DIP-ESI, an amount of 1.6 μg piracetam was sufficient. In the case of the DIP-ESI measurements, all detected impurities could be identified by MS/MS studies. Graphical Abstract Scheme of the DIP-ESI principle.

  3. Comprehensive comparison of in silico MS/MS fragmentation tools of the CASMI contest: database boosting is needed to achieve 93% accuracy.

    Science.gov (United States)

    Blaženović, Ivana; Kind, Tobias; Torbašinović, Hrvoje; Obrenović, Slobodan; Mehta, Sajjan S; Tsugawa, Hiroshi; Wermuth, Tobias; Schauer, Nicolas; Jahn, Martina; Biedendieck, Rebekka; Jahn, Dieter; Fiehn, Oliver

    2017-05-25

    In mass spectrometry-based untargeted metabolomics, rarely more than 30% of the compounds are identified. Without the true identity of these molecules it is impossible to draw conclusions about the biological mechanisms, pathway relationships and provenance of compounds. The only way at present to address this discrepancy is to use in silico fragmentation software to identify unknown compounds by comparing and ranking theoretical MS/MS fragmentations from target structures to experimental tandem mass spectra (MS/MS). We compared the performance of four publicly available in silico fragmentation algorithms (MetFragCL, CFM-ID, MAGMa+ and MS-FINDER) that participated in the 2016 CASMI challenge. We found that optimizing the use of metadata, weighting factors and the manner of combining different tools eventually defined the ultimate outcomes of each method. We comprehensively analysed how outcomes of different tools could be combined and reached a final success rate of 93% for the training data, and 87% for the challenge data, using a combination of MAGMa+, CFM-ID and compound importance information along with MS/MS matching. Matching MS/MS spectra against the MS/MS libraries without using any in silico tool yielded 60% correct hits, showing that the use of in silico methods is still important.

  4. PyMS: a Python toolkit for processing of gas chromatography-mass spectrometry (GC-MS data. Application and comparative study of selected tools

    Directory of Open Access Journals (Sweden)

    O'Callaghan Sean

    2012-05-01

    Full Text Available Abstract Background Gas chromatography–mass spectrometry (GC-MS is a technique frequently used in targeted and non-targeted measurements of metabolites. Most existing software tools for processing of raw instrument GC-MS data tightly integrate data processing methods with graphical user interface facilitating interactive data processing. While interactive processing remains critically important in GC-MS applications, high-throughput studies increasingly dictate the need for command line tools, suitable for scripting of high-throughput, customized processing pipelines. Results PyMS comprises a library of functions for processing of instrument GC-MS data developed in Python. PyMS currently provides a complete set of GC-MS processing functions, including reading of standard data formats (ANDI- MS/NetCDF and JCAMP-DX, noise smoothing, baseline correction, peak detection, peak deconvolution, peak integration, and peak alignment by dynamic programming. A novel common ion single quantitation algorithm allows automated, accurate quantitation of GC-MS electron impact (EI fragmentation spectra when a large number of experiments are being analyzed. PyMS implements parallel processing for by-row and by-column data processing tasks based on Message Passing Interface (MPI, allowing processing to scale on multiple CPUs in distributed computing environments. A set of specifically designed experiments was performed in-house and used to comparatively evaluate the performance of PyMS and three widely used software packages for GC-MS data processing (AMDIS, AnalyzerPro, and XCMS. Conclusions PyMS is a novel software package for the processing of raw GC-MS data, particularly suitable for scripting of customized processing pipelines and for data processing in batch mode. PyMS provides limited graphical capabilities and can be used both for routine data processing and interactive/exploratory data analysis. In real-life GC-MS data processing scenarios PyMS performs

  5. Determination of post-culture processing with carbohydrates by MALDI-MS and TMS derivatization GC-MS.

    Science.gov (United States)

    Wunschel, David S; Wahl, Karen L; Melville, Angela M; Sorensen, Christina M; Colburn, Heather A; Valentine, Nancy B; Stamper, Casey L

    2011-10-15

    Biological materials generally require stabilization to retain activity or viability in a dry form. A number of industrial products, such as vaccines, probiotics and biopesticides have been produced as dry preparations. The same methods and materials used for stabilizing commercial microbial products may be applicable to preserving biothreat pathogens in a dry form. This is a likely step that may be encountered when looking at samples from terrorism attempts since only spores, such as those from Bacillus anthracis, are inherently stable when dried. The stabilizers for microbial preparations generally include one or more small carbohydrates. Different formulations have been reported for different industrial products and are often determined empirically. However sugar alcohols (mannitol and sorbitol) and disaccharides (lactose, sucrose and trehalose) are the common constituents of these formulations. We have developed an analytical method for sample preparation and detection of these simple carbohydrates using two complementary analytical tools, MALDI-MS and GC-MS. The native carbohydrates and other constituents of the formulation are detected by MALDI-MS as a screening tool. A longer and more detailed analysis is then used to specifically identify the carbohydrates by derivatization and GC-MS detection. Both techniques were tested against ten different types of stabilization recipes with Yersinia pestis cell mass cultured on different media types used as the biological component. A number of additional components were included in these formulations including proteins and peptides from serum or milk, polymers (e.g. poly vinyl pyrrolidone - PVP) and detergents (e.g. Tween). The combined method was characterized to determine several figures of merit. The accuracy of the method was 98% for MALDI-MS and 100% for GC-MS. The repeatability for detection of carbohydrates by MALDI-MS was determined to be 96%. The repeatability of compound identification by GC-MS was

  6. Phenolic Profiling of Duchesnea indica Combining Macroporous Resin Chromatography (MRC with HPLC-ESI-MS/MS and ESI-IT-MS

    Directory of Open Access Journals (Sweden)

    Mingzhi Zhu

    2015-12-01

    Full Text Available Duchesnea indica (D. indica is an important traditional Chinese medicine, and has long been clinically used to treat cancer in Asian countries. It has been described previously as a rich source of phenolic compounds with a broad array of diversified structures, which are the major active ingredients. However, an accurate and complete phenolic profiling has not been determined yet. In the present work, the total phenolic compounds in crude extracts from D. indica were enriched and fractionated over a macroporous resin column, then identified by HPLC-ESI-MS/MS and ESI-IT-MS (ion trap MS. A total of 27 phenolic compounds were identified in D. indica, of which 21 compounds were identified for the first time. These 27 phenolic compounds encompassing four phenolic groups, including ellagitannins, ellagic acid and ellagic acid glycosides, hydroxybenzoic acid and hydroxycinnamic acid derivatives, and flavonols, were then successfully quantified using peak areas against those of the corresponding standards with good linearity (R2 > 0.998 in the range of the tested concentrations. As a result, the contents of individual phenolic compounds varied from 6.69 mg per 100 g dry weight (DW for ellagic acid to 71.36 mg per 100 g DW for brevifolin carboxylate. Not only did this study provide the first phenolic profiling of D. indica, but both the qualitative identification and the subsequent quantitative analysis of 27 phenolic compounds from D. indica should provide a good basis for future exploration of this valuable medicinal plant.

  7. Rapid Determination of Isomeric Benzoylpaeoniflorin and Benzoylalbiflorin in Rat Plasma by LC-MS/MS Method

    Directory of Open Access Journals (Sweden)

    Chuanqi Zhou

    2017-01-01

    Full Text Available Benzoylpaeoniflorin (BP is a potential therapeutic agent against oxidative stress related Alzheimer’s disease. In this study, a more rapid, selective, and sensitive liquid chromatography-tandem mass spectrometric (LC-MS/MS method was developed to determine BP in rat plasma distinguishing with a monoterpene isomer, benzoylalbiflorin (BA. The method showed a linear response from 1 to 1000 ng/mL (r>0.9950. The precision of the interday and intraday ranged from 2.03 to 12.48% and the accuracy values ranged from −8.00 to 10.33%. Each running of the method could be finished in 4 minutes. The LC-MS/MS method was validated for specificity, linearity, precision, accuracy, recovery, and stability and was found to be acceptable for bioanalytical application. Finally, this fully validated method was successfully applied to a pharmacokinetic study in rats following oral administration.

  8. Complex mixture analysis of peptides using LC/LC-MS/MS and data-dependent protein identification

    International Nuclear Information System (INIS)

    Wasinger, V.; Corthals, G.

    2001-01-01

    The comprehensive identification of proteins within complex solutions by mass-spectrometry largely depends on the sensitivity, resolving power and sampling efficiency of the technology. An integrated orthogonal approach using Strong Cation Exchange-Reverse Phase-MS/MS (SCX-RP-MS/MS) was used to evaluate the data-dependent Collision Induced Dissociation (CID) of yeast peptides. Reverse phase gradient times of 4, 10. 30, 90, and 180 minutes allowed the identification of hundreds of proteins in a nearly automated fashion from nuclear, membrane, and cytosolic distributions. Many proteins from typically difficult to resolve regions of two-dimensional gels, such as >100kDa, > pI 9.0 and Codon Adaptation Index < 0.2, were also identified using this multi-dimensional separation technology. Few low mass proteins (<10kDa) were identified. The impact of scan-range and duty-cycle on CID of peptides will be discussed

  9. Evaluation of a Method for Nitrotyrosine Site Identification and Relative Quantitation Using a Stable Isotope-Labeled Nitrated Spike-In Standard and High Resolution Fourier Transform MS and MS/MS Analysis

    Directory of Open Access Journals (Sweden)

    Kent W. Seeley

    2014-04-01

    Full Text Available The overproduction of reactive oxygen and nitrogen species (ROS and RNS can have deleterious effects in the cell, including structural and possible activity-altering modifications to proteins. Peroxynitrite is one such RNS that can result in a specific protein modification, nitration of tyrosine residues to form nitrotyrosine, and to date, the identification of nitrotyrosine sites in proteins continues to be a major analytical challenge. We have developed a method by which 15N-labeled nitrotyrosine groups are generated on peptide or protein standards using stable isotope-labeled peroxynitrite (O15NOO−, and the resulting standard is mixed with representative samples in which nitrotyrosine formation is to be measured by mass spectrometry (MS. Nitropeptide MS/MS spectra are filtered using high mass accuracy Fourier transform MS (FTMS detection of the nitrotyrosine immonium ion. Given that the nitropeptide pair is co-isolated for MS/MS fragmentation, the nitrotyrosine immonium ions (at m/z = 181 or 182 can be used for relative quantitation with negligible isotopic interference at a mass resolution of greater than 50,000 (FWHM, full width at half-maximum. Furthermore, the standard potentially allows for the increased signal of nitrotyrosine-containing peptides, thus facilitating selection for MS/MS in a data-dependent mode of acquisition. We have evaluated the methodology in terms of nitrotyrosine site identification and relative quantitation using nitrated peptide and protein standards.

  10. Comparison of LC-ESI-MS and GC-MS for the Analysis of a Synthetic Tabun Sample

    National Research Council Canada - National Science Library

    D'Agostino, Paul

    2003-01-01

    Packed capillary LC-ESI-MS and capillary column GC-MS were compared for the analysis of a synthetic tabun sample as each method has advantages for the analysis of samples containing chemical warfare...

  11. Analytical Method Details (MS): SE59_MS01 [Metabolonote[Archive

    Lifescience Database Archive (English)

    Full Text Available argeted metabolomic analysis using LC-QTOF-MS and the metabolome data processing of alignment, de-isotoping, noise cutting, and normalization was conducted as previously described. ...

  12. Evaluation of laser diode thermal desorption-tandem mass spectrometry (LDTD-MS-MS) in forensic toxicology.

    Science.gov (United States)

    Bynum, Nichole D; Moore, Katherine N; Grabenauer, Megan

    2014-10-01

    Many forensic laboratories experience backlogs due to increased drug-related cases. Laser diode thermal desorption (LDTD) has demonstrated its applicability in other scientific areas by providing data comparable with instrumentation, such as liquid chromatography-tandem mass spectrometry, in less time. LDTD-MS-MS was used to validate 48 compounds in drug-free human urine and blood for screening or quantitative analysis. Carryover, interference, limit of detection, limit of quantitation, matrix effect, linearity, precision and accuracy and stability were evaluated. Quantitative analysis indicated that LDTD-MS-MS produced precise and accurate results with the average overall within-run precision in urine and blood represented by a %CV forensic toxicology but before it can be successfully implemented that there are some challenges that must be addressed. Although the advantages of the LDTD system include minimal maintenance and rapid analysis (∼10 s per sample) which makes it ideal for high-throughput forensic laboratories, a major disadvantage is its inability or difficulty analyzing isomers and isobars due to the lack of chromatography without the use of high-resolution MS; therefore, it would be best implemented as a screening technique. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  13. Comparison of Proteins in Whole Blood and Dried Blood Spot Samples by LC/MS/MS

    Science.gov (United States)

    Chambers, Andrew G.; Percy, Andrew J.; Hardie, Darryl B.; Borchers, Christoph H.

    2013-09-01

    Dried blood spot (DBS) sampling methods are desirable for population-wide biomarker screening programs because of their ease of collection, transportation, and storage. Immunoassays are traditionally used to quantify endogenous proteins in these samples but require a separate assay for each protein. Recently, targeted mass spectrometry (MS) has been proposed for generating highly-multiplexed assays for biomarker proteins in DBS samples. In this work, we report the first comparison of proteins in whole blood and DBS samples using an untargeted MS approach. The average number of proteins identified in undepleted whole blood and DBS samples by liquid chromatography (LC)/MS/MS was 223 and 253, respectively. Protein identification repeatability was between 77 %-92 % within replicates and the majority of these repeated proteins (70 %) were observed in both sample formats. Proteins exclusively identified in the liquid or dried fluid spot format were unbiased based on their molecular weight, isoelectric point, aliphatic index, and grand average hydrophobicity. In addition, we extended this comparison to include proteins in matching plasma and serum samples with their dried fluid spot equivalents, dried plasma spot (DPS), and dried serum spot (DSS). This work begins to define the accessibility of endogenous proteins in dried fluid spot samples for analysis by MS and is useful in evaluating the scope of this new approach.

  14. Obituary: Benjamin Franklin Peery Jr. (1922-2010)

    Science.gov (United States)

    Cowley, Charles

    2011-12-01

    Professor Benjamin F. Peery, Jr. died at his home in Silver Spring, MD of natural causes on 30 November 2010. His full life began in St. Joseph, MO (home of the Pony Express) on 4 March 1922. His father was a railway mail clerk, so his family moved frequently. Most of his childhood was spent in southeastern Minnesota. He enlisted in the army in 1942, and served in campaigns in North Africa and Italy. After his discharge in 1945, he enrolled in the University of Minnesota, earning a BS in Physics in 1949. One of his early hobbies was to build and fly model airplanes. His intention to pursue aeronautical engineering changed to physics, but after receiving a MS in physics from Fisk University in 1955, he decided on a career in astronomy. He told the editors of the PBS series The Astronomers (1991, in which his career is highlighted) he thought it was shamefully absurd not to know what made the stars shine. So he began PhD studies in astronomy at the University of Michigan (Ann Arbor). His dissertation was on the complex eclipsing binary VV Cephei, where a compact hot star passes behind a cool giant star, revealing the structure of that giant's atmosphere. This task was especially demanding because of the complexity of the system's spectrum and the formidable array of observations assembled by Ben's advisor, Dean McLaughlin. Fortunately, Ben's strong physics background enabled him to design and construct one of the first oscilloscope measuring engines, which his fellow students called the PeeryScope. The final (1961) dissertation is an impressive combination of observational and astrophysical analysis. His degree was obtained in 1962; he had already begun a career at the University of Indiana, where he taught and did research (1959--1976). The Indiana years were highly productive. In addition to his own research, he was advisor on six PhD dissertations, and a master's thesis. Several of his students have also had productive careers. An ADS search on his students' names

  15. Detection of mono- and di-hexoses as metabolites of 4-bromoaniline using HPLC-TOF-MS/MS.

    Science.gov (United States)

    Major, H; Castro-Perez, J; Nicholson, J K; Wilson, I D

    2003-08-01

    1. The metabolic fate of 4-bromoaniline (4-BrA) was investigated in rat following intraperitoneal administration at 50 mg kg(-1) using HPLC-TOF-MS/MS. 2. The sensitivity provided by the use of TOF-MS/MS, aided by the distinctive isotope pattern resulting from the presence of the bromine substituent in the molecule, enabled the detection of many previously uncharacterized metabolites in the samples. 3. Several groups of minor metabolites were detected in the urine that corresponded to a number of isomeric hexose and di-hexose-containing conjugates (possibly glucosides and diglucosides) of 4-BrA. 4. As well as hexose and di-hexose conjugates of 4-BrA, several further groups of metabolites that also contained either a sulphamate or sulphate group in addition to the sugar moieties were also detected.

  16. Hip-Hop to Health Jr. Obesity Prevention Effectiveness Trial: Post-Intervention Results

    Science.gov (United States)

    Fitzgibbon, M. L.; Stolley, M. R.; Schiffer, L.; Braunschweig, C. L.; Gomez, S. L.; Van Horn, L.; Dyer, A.

    2013-01-01

    The preschool years offer an opportunity to interrupt the trajectory toward obesity in black children. The Hip-Hop to Health Jr. Obesity Prevention Effectiveness Trial was a group-randomized controlled trial assessing the feasibility and effectiveness of a teacher-delivered weight control intervention for black preschool children. The 618 participating children were enrolled in 18 schools administered by the Chicago Public Schools. Children enrolled in the 9 schools randomized to the intervention group received a 14-week weight control intervention delivered by their classroom teachers. Children in the 9 control schools received a general health intervention. Height and weight, physical activity, screen time, and diet data were collected at baseline and post-intervention. At post-intervention, children in the intervention schools engaged in more moderate-to vigorous physical activity than children in the control schools (difference between adjusted group means=7.46 min/day, p=.02). Also, children in the intervention group had less total screen time (−27.8 min/day, p=.05). There were no significant differences in BMI, BMI Z score, or dietary intake. It is feasible to adapt an obesity prevention program to be taught by classroom teachers. The intervention showed positive influences on physical activity and screen time, but not diet. Measuring diet and physical activity in preschool children remains a challenge, and interventions delivered by classroom teachers require both intensive initial training and ongoing individualized supervision. PMID:21193852

  17. Venocentric lesions: an MRI marker of MS?

    Directory of Open Access Journals (Sweden)

    Matthew P. Quinn

    2013-07-01

    Full Text Available From the earliest descriptions of MS, the venocentric characteristic of plaques was noted. Recently, numerous MRI studies have proposed this finding as a prospective biomarker for MS, which might aid in differentiating MS from other diseases with similar MRI findings. High field MRI studies have shown that penetrating veins can be detected in most MS lesions using T2* weighted or susceptibility weighted imaging. Future studies must address the feasibility of imaging such veins in a clinically practical context. The specificity of this biomarker has been studied only in a limited capacity. Results in microangiopathic lesions are conflicting, whereas asymptomatic white matter hyperintensities as well as lesions of NMO are less frequently venocentric compared to MS plaques. Prospective studies have shown that the presence of venocentric lesions at an early clinical presentation is highly predictive of future MS diagnosis. This is very promising, but work remains to be done to confirm or exclude lesions of common MS mimics, such as ADEM, as venocentric. A number of technical challenges must be addressed before the introduction of this technique as a complementary tool in current diagnostic procedures.

  18. siMS Score: Simple Method for Quantifying Metabolic Syndrome.

    Science.gov (United States)

    Soldatovic, Ivan; Vukovic, Rade; Culafic, Djordje; Gajic, Milan; Dimitrijevic-Sreckovic, Vesna

    2016-01-01

    To evaluate siMS score and siMS risk score, novel continuous metabolic syndrome scores as methods for quantification of metabolic status and risk. Developed siMS score was calculated using formula: siMS score = 2*Waist/Height + Gly/5.6 + Tg/1.7 + TAsystolic/130-HDL/1.02 or 1.28 (for male or female subjects, respectively). siMS risk score was calculated using formula: siMS risk score = siMS score * age/45 or 50 (for male or female subjects, respectively) * family history of cardio/cerebro-vascular events (event = 1.2, no event = 1). A sample of 528 obese and non-obese participants was used to validate siMS score and siMS risk score. Scores calculated as sum of z-scores (each component of metabolic syndrome regressed with age and gender) and sum of scores derived from principal component analysis (PCA) were used for evaluation of siMS score. Variants were made by replacing glucose with HOMA in calculations. Framingham score was used for evaluation of siMS risk score. Correlation between siMS score with sum of z-scores and weighted sum of factors of PCA was high (r = 0.866 and r = 0.822, respectively). Correlation between siMS risk score and log transformed Framingham score was medium to high for age groups 18+,30+ and 35+ (0.835, 0.707 and 0.667, respectively). siMS score and siMS risk score showed high correlation with more complex scores. Demonstrated accuracy together with superior simplicity and the ability to evaluate and follow-up individual patients makes siMS and siMS risk scores very convenient for use in clinical practice and research as well.

  19. Measurement of trace levels of antibiotics in river water using on-line enrichment and triple-quadrupole LC-MS/MS.

    Science.gov (United States)

    Dinh, Quoc Tuc; Alliot, Fabrice; Moreau-Guigon, Elodie; Eurin, Joëlle; Chevreuil, Marc; Labadie, Pierre

    2011-09-15

    This study presents the development of an automated on-line solid phase extraction (SPE)-liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of 23 antibiotics in environmental water samples. After optimisation of LC-MS/MS conditions, SPE parameters such as sorbent type, sample pH or sample volume were optimised. Antibiotic recoveries ranged from 64% to 98% and compared favourably with those achieved using off-line SPE. Limits of detection were in the range 0.5-13.7 ng L(-1). This on-line SPE-LC-MS/MS procedure was applied to the analysis of water samples taken in three rivers within the Seine River basin, near Paris (France). The obtained results revealed the occurrence of 12 antibiotics, including tylosin, erythromycin, tetracycline, amoxicillin, trimethoprim, sulfamethoxazole, oxolinic acid, flumequine, norfloxacin, ciprofloxacin, ofloxacin, and vancomycin (2-1435 ng L(-1)). Copyright © 2011 Elsevier B.V. All rights reserved.

  20. Determination of isosteviol by LC-MS/MS and its application for evaluation of pharmacokinetics of isosteviol in rat

    Directory of Open Access Journals (Sweden)

    Bazargan M.

    2007-06-01

    Full Text Available Isosteviol has been found to have potential preventive or therapeutic effects against hypertension, ischemia reperfusion injury, diabetes and cancer, but little is known about the pharmacokinetics (PK of the compound. The aim of this study was to develop a liquid chromatographic-tandem mass spectrometric (LC-MS/MS method for determination of isosteviol in rat plasma and to assess in a preliminary manner the PK of isosteviol after intravenous bolus injection.Ions of analytes were generated using electro-spray ionization and detected in the positive-ion mode in LC-MS/MS. Multiple reaction monitoring was performed, using the precursor product ion combination for isosteviol m/z 319.4→273.4. Progesterone was used as an internal standard. Nitrogen was used as the nebulising gas and unit resolution was set for Q1 and Q3. Isosteviol solution was injected through the penile vein of rats at a dose of 8 mg/kg. Blood samples were collected from a jugular vein cannula. The PK parameters were calculated using a two - compartment PK model.The LC-MS/MS assay for isosteviol in rat plasma was linear over the range of 0.5-80 μg/ml. The terminal half life of isosteviol (t 1/2 was 406 ± 31.7 min and clearance (CL was 2.9 ± 0.3 ml/min/kg. A sensitive LC-MS/MS assay for isosteviol in plasma has been successfully established and used in a preliminary PK evaluation of isosteviol in rats.

  1. Method-MS. Final report

    International Nuclear Information System (INIS)

    Skipperud, L.; Popic, J.M.; Roos, P.; Salminen, S.; Nygren, U.; Sigmarsson, O.; Palsson, S.E.

    2011-05-01

    Radiometric determination methods, such as alpha spectrometry require long counting times when low activities are to be determined. Mass spectrometric techniques as Inductively Coupled Plasma Mass Spectrometry (ICP-MS), Thermal Ionisation Mass Spectrometry (TIMS) and Accelerator Mass Spectrometry (AMS) have shown several advantages compared to traditional methods when measuring long-lived radionuclides. Mass spectrometric methods for determination of very low concentrations of elemental isotopes, and thereby isotopic ratios, have been developed using a variety of ion sources. Although primarily applied to the determination of the lighter stable element isotopes and radioactive isotopes in geological studies, the techniques can equally well be applied to the measurement of activity concentrations of long-lived low-level radionuclides in various samples using 'isotope dilution' methods such as those applied in inductively coupled plasma mass spectrometry (ICP-MS). Due to the low specific activity of long-lived radionuclides, many of these are more conveniently detected using mass spectrometric techniques. Mass spectrometry also enables the individual determination of Pu-239 and Pu-240, which cannot be obtained by alpha spectrometry. Inductively Coupled Plasma Mass Spectrometry (ICP-MS) are rapidly growing techniques for the ultra-trace analytical determination of stable and long-lived isotopes and have a wide potential within environmental science, including ecosystem tracers and radio ecological studies. Such instrumentation, of course needs good radiochemical separation, to give best performance. The objectives of the project is to identify current needs and problems within low-level determination of long-lived radioisotopes by ICP-MS, to perform intercalibration and development and improvement of ICP-MS methods for the measurement of radionuclides and isotope ratios and to develop new methods based on modified separation chemistry applied to new auxiliary

  2. Method-MS. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Skipperud, L.; Popic, J.M. (Norwegian Univ. of Life Science (UMB), Isotope Lab. (Norway)); Roos, P. (Technical Univ. of Denmark, Risoe National Lab. for Sustainable Energy, Roskilde (Denmark)); Salminen, S. (Univ. of Helsinki (UH) (Finland)); Nygren, U. (Swedish Defence Research Agency (FOI) (Sweden)); Sigmarsson, O.; Palsson, S.E. (Univ. of Iceland/Icelandic Radiation Protection Institute (Iceland))

    2011-05-15

    Radiometric determination methods, such as alpha spectrometry require long counting times when low activities are to be determined. Mass spectrometric techniques as Inductively Coupled Plasma Mass Spectrometry (ICP-MS), Thermal Ionisation Mass Spectrometry (TIMS) and Accelerator Mass Spectrometry (AMS) have shown several advantages compared to traditional methods when measuring long-lived radionuclides. Mass spectrometric methods for determination of very low concentrations of elemental isotopes, and thereby isotopic ratios, have been developed using a variety of ion sources. Although primarily applied to the determination of the lighter stable element isotopes and radioactive isotopes in geological studies, the techniques can equally well be applied to the measurement of activity concentrations of long-lived low-level radionuclides in various samples using 'isotope dilution' methods such as those applied in inductively coupled plasma mass spectrometry (ICP-MS). Due to the low specific activity of long-lived radionuclides, many of these are more conveniently detected using mass spectrometric techniques. Mass spectrometry also enables the individual determination of Pu-239 and Pu-240, which cannot be obtained by alpha spectrometry. Inductively Coupled Plasma Mass Spectrometry (ICP-MS) are rapidly growing techniques for the ultra-trace analytical determination of stable and long-lived isotopes and have a wide potential within environmental science, including ecosystem tracers and radio ecological studies. Such instrumentation, of course needs good radiochemical separation, to give best performance. The objectives of the project is to identify current needs and problems within low-level determination of long-lived radioisotopes by ICP-MS, to perform intercalibration and development and improvement of ICP-MS methods for the measurement of radionuclides and isotope ratios and to develop new methods based on modified separation chemistry applied to new

  3. ICP-MS/MS-Based Ionomics: A Validated Methodology to Investigate the Biological Variability of the Human Ionome.

    Science.gov (United States)

    Konz, Tobias; Migliavacca, Eugenia; Dayon, Loïc; Bowman, Gene; Oikonomidi, Aikaterini; Popp, Julius; Rezzi, Serge

    2017-05-05

    We here describe the development, validation and application of a quantitative methodology for the simultaneous determination of 29 elements in human serum using state-of-the-art inductively coupled plasma triple quadrupole mass spectrometry (ICP-MS/MS). This new methodology offers high-throughput elemental profiling using simple dilution of minimal quantity of serum samples. We report the outcomes of the validation procedure including limits of detection/quantification, linearity of calibration curves, precision, recovery and measurement uncertainty. ICP-MS/MS-based ionomics was used to analyze human serum of 120 older adults. Following a metabolomic data mining approach, the generated ionome profiles were subjected to principal component analysis revealing gender and age-specific differences. The ionome of female individuals was marked by higher levels of calcium, phosphorus, copper and copper to zinc ratio, while iron concentration was lower with respect to male subjects. Age was associated with lower concentrations of zinc. These findings were complemented with additional readouts to interpret micronutrient status including ceruloplasmin, ferritin and inorganic phosphate. Our data supports a gender-specific compartmentalization of the ionome that may reflect different bone remodelling in female individuals. Our ICP-MS/MS methodology enriches the panel of validated "Omics" approaches to study molecular relationships between the exposome and the ionome in relation with nutrition and health.

  4. Development and Validation of a Novel LC-MS/MS Opioid Confirmation Assay: Evaluation of β-glucuronidase Enzymes and Sample Cleanup Methods.

    Science.gov (United States)

    Yang, He S; Wu, Alan H B; Lynch, Kara L

    2016-06-01

    With the rise in the use and misuse of prescription opioids, there is an increasing need for the confirmed identification of opioid analgesics in toxicology laboratories. The goals of this study were to (i) systematically evaluate the hydrolysis efficiency of four β-glucuronidase enzymes under optimized condition; (ii) evaluate compound recovery, matrix effects and precision of three protein precipitation plates and (iii) develop and validate a qualitative liquid-chromatography mass spectrometry (LC-MS/MS) assay to identify 13 opioids in urine. A recombinant β-glucuronidase exhibited the best overall hydrolysis efficiency for seven opioid glucuronide conjugates compared with β-glucuronidase from red abalone, Escherichia coli and Patella vulgata One of the protein precipitation plates tested exhibited overall better recovery of the opioids and lower ion suppression compared with the other two plates. An ESI positive mode LC-MS/MS assay for qualitative opioid analysis was developed and validated. Linearity, LOD, precision, matrix effect, recovery, carryover and interference of the method were evaluated. Sixty-two patient samples were analyzed by both a legacy GC-MS opioid method and the LC-MS/MS method, and 22 samples were analyzed by the LC-MS/MS and an LC-MS/MS reference method. The results of the comparisons showed good concordance. Overall, we described an efficient sample preparation procedure for a sensitive qualitative opioid confirmation assay in urine. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  5. Profiling and characterization of sialylated N-glycans by 2D-HPLC (HIAX/PGC) with online orbitrap MS/MS and offline MSn.

    Science.gov (United States)

    Hanneman, Andrew J S; Strand, James; Huang, Chi-Ting

    2014-02-01

    Glycosylation is a critical parameter used to evaluate protein quality and consistency. N-linked glycan profiling is fundamental to the support of biotherapeutic protein manufacturing from early stage process development through drug product commercialization. Sialylated glycans impact the serum half-life of receptor-Fc fusion proteins (RFPs), making their quality and consistency a concern during the production of fusion proteins. Here, we describe an analytical approach providing both quantitative profiling and in-depth mass spectrometry (MS)-based structural characterization of sialylated RFP N-glycans. Aiming to efficiently link routine comparability studies with detailed structural characterization, an integrated workflow was implemented employing fluorescence detection, online positive and negative ion tandem mass spectrometry (MS/MS), and offline static nanospray ionization-sequential mass spectrometry (NSI-MS(n)). For routine use, high-performance liquid chromatography profiling employs established fluorescence detection of 2-aminobenzoic acid derivatives (2AA) and hydrophilic interaction anion-exchange chromatography (HIAX) charge class separation. Further characterization of HIAX peak fractions is achieved by online (-) ion orbitrap MS/MS, offering the advantages of high mass accuracy and data-dependent MS/MS. As required, additional characterization uses porous graphitized carbon in the second chromatographic dimension to provide orthogonal (+) ion MS/MS spectra and buffer-free liquid chromatography peak eluants that are optimum for offline (+)/(-) NSI-MS(n) investigations to characterize low-abundance species and specific moieties including O-acetylation and sulfation. © 2013 Wiley Periodicals, Inc. and the American Pharmacists Association.

  6. Determination of carbohydrates in medicinal plants--comparison between TLC, mf-MELDI-MS and GC-MS.

    Science.gov (United States)

    Qureshi, Muhammad Nasimullah; Stecher, Guenther; Sultana, Tahira; Abel, Gudrun; Popp, Michael; Bonn, Guenther K

    2011-01-01

    Quality control in the pharmaceutical and phytopharmaceutical industries requires fast and reliable methods for the analysis of raw materials and final products. This study evaluates different analytical approaches in order to recognise the most suitable technique for the analysis of carbohydrates in herbal drug preparations. The specific focus of the study is on thin-layer chromatography (TLC), gas chromatography (GC), and a newly developed mass spectrometric method, i.e. matrix free material enhanced laser desorption/ionisation time of flight mass spectrometry (mf-MELDI-MS). Samples employed in the study were standards and microwave-assisted water extracts from Quercus. TLC analysis proved the presence of mono-, di- and trisaccharides within the biological sample and hinted at the existence of an unknown carbohydrate of higher oligomerisation degree. After evaluation of different derivatisation techniques, GC-MS confirmed data obtained via TLC for mono- to trisaccharides, delivering additionally quantified values under a considerable amount of time. A carbohydrate of higher oligomerisation degree could not be found. The application of mf-MELDI-MS further confirmed the presence of carbohydrates up to trisaccharides, also hinting at the presence of a form of tetrasaccharide. Besides this information, mf-MELDI-MS delivered further data about other substances present in the extract. Quantitative determination resulted in 1.750, 1.736 and 0.336 mg/mL for glucose, sucrose and raffinose respectively. Evaluation of all three techniques employed, clearly proved the heightened performance of mf-MELDI-MS for the qualitative analysis of complex mixtures, as targets do not need modification and analysis requires only a few minutes. In addition, GC-MS is suitable for quantitative analysis. Copyright © 2011 John Wiley & Sons, Ltd.

  7. Wavelet-based peak detection and a new charge inference procedure for MS/MS implemented in ProteoWizard's msConvert.

    Science.gov (United States)

    French, William R; Zimmerman, Lisa J; Schilling, Birgit; Gibson, Bradford W; Miller, Christine A; Townsend, R Reid; Sherrod, Stacy D; Goodwin, Cody R; McLean, John A; Tabb, David L

    2015-02-06

    We report the implementation of high-quality signal processing algorithms into ProteoWizard, an efficient, open-source software package designed for analyzing proteomics tandem mass spectrometry data. Specifically, a new wavelet-based peak-picker (CantWaiT) and a precursor charge determination algorithm (Turbocharger) have been implemented. These additions into ProteoWizard provide universal tools that are independent of vendor platform for tandem mass spectrometry analyses and have particular utility for intralaboratory studies requiring the advantages of different platforms convergent on a particular workflow or for interlaboratory investigations spanning multiple platforms. We compared results from these tools to those obtained using vendor and commercial software, finding that in all cases our algorithms resulted in a comparable number of identified peptides for simple and complex samples measured on Waters, Agilent, and AB SCIEX quadrupole time-of-flight and Thermo Q-Exactive mass spectrometers. The mass accuracy of matched precursor ions also compared favorably with vendor and commercial tools. Additionally, typical analysis runtimes (∼1-100 ms per MS/MS spectrum) were short enough to enable the practical use of these high-quality signal processing tools for large clinical and research data sets.

  8. siMS Score: Simple Method for Quantifying Metabolic Syndrome

    OpenAIRE

    Soldatovic, Ivan; Vukovic, Rade; Culafic, Djordje; Gajic, Milan; Dimitrijevic-Sreckovic, Vesna

    2016-01-01

    Objective To evaluate siMS score and siMS risk score, novel continuous metabolic syndrome scores as methods for quantification of metabolic status and risk. Materials and Methods Developed siMS score was calculated using formula: siMS score = 2*Waist/Height + Gly/5.6 + Tg/1.7 + TAsystolic/130?HDL/1.02 or 1.28 (for male or female subjects, respectively). siMS risk score was calculated using formula: siMS risk score = siMS score * age/45 or 50 (for male or female subjects, respectively) * famil...

  9. ToF-SIMS Parallel Imaging MS/MS of Lipid Species in Thin Tissue Sections.

    Science.gov (United States)

    Bruinen, Anne Lisa; Fisher, Gregory L; Heeren, Ron M A

    2017-01-01

    Unambiguous identification of detected species is essential in complex biomedical samples. To date, there are not many mass spectrometry imaging techniques that can provide both high spatial resolution and identification capabilities. A new and patented imaging tandem mass spectrometer, exploiting the unique characteristics of the nanoTOF II (Physical Electronics, USA) TOF-SIMS TRIFT instrument, was developed to address this.Tandem mass spectrometry is based on the selection of precursor ions from the full secondary ion spectrum (MS 1 ), followed by energetic activation and fragmentation, and collection of the fragment ions to obtain a tandem MS spectrum (MS 2 ). The PHI NanoTOF II mass spectrometer is equipped with a high-energy collision induced dissociation (CID) fragmentation cell as well as a second time-of-flight analyzer developed for simultaneous ToF-SIMS and tandem MS imaging experiments.We describe here the results of a ToF-SIMS imaging experiment on a thin tissue section of an infected zebrafish as a model organism for tuberculosis. The focus is on the obtained ion distribution plot of a fatty acid as well as its identification by tandem mass spectrometry.

  10. Identifying inaccuracy of MS Project using system analysis

    Science.gov (United States)

    Fachrurrazi; Husin, Saiful; Malahayati, Nurul; Irzaidi

    2018-05-01

    The problem encountered in project owner’s financial accounting report is the difference in total project costs of MS Project to the Indonesian Standard (Standard Indonesia Standard / Cost Estimating Standard Book of Indonesia). It is one of the MS Project problems concerning to its cost accuracy, so cost data cannot be used in an integrated way for all project components. This study focuses on finding the causes of inaccuracy of the MS Projects. The aim of this study, which is operationally, are: (i) identifying cost analysis procedures for both current methods (SNI) and MS Project; (ii) identifying cost bias in each element of the cost analysis procedure; and (iii) analysing the cost differences (cost bias) in each element to identify what the cause of inaccuracies in MS Project toward SNI is. The method in this study is comparing for both the system analysis of MS Project and SNI. The results are: (i) MS Project system in Work of Resources element has limitation for two decimal digits only, have led to its inaccuracy. Where the Work of Resources (referred to as effort) in MS Project represents multiplication between the Quantities of Activities and Requirements of resources in SNI; (ii) MS Project and SNI have differences in the costing methods (the cost estimation methods), in which the SNI uses the Quantity-Based Costing (QBC), meanwhile MS Project uses the Time-Based Costing (TBC). Based on this research, we recommend to the contractors who use SNI should make an adjustment for Work of Resources in MS Project (with correction index) so that it can be used in an integrated way to the project owner’s financial accounting system. Further research will conduct for improvement the MS Project as an integrated tool toward all part of the project participant.

  11. New application and future of ICP-MS

    International Nuclear Information System (INIS)

    Masuda, Kimihiko

    1994-01-01

    By ICP-MS, since high sensibility, multi-element rapid analysis and isotope ratio analysis can be carried out, the position as the analysis for ultra-minute amount of elements has been established. Further recently, sample feeder system has been developed, and the multi-collector type device for the purpose of high resolution type isotope ratio analysis has appeared, so the range of its application is spreading more and more. In this report, the examples of application which were able to be attained accompanying the development of these devices are introduced, and the development of the ICP-MS hereafter is described. At present, about 1000 apparatuses are in operation in the world, and the application spread to the fields of semiconductors and materials, earth science, environment, atomic energy and so on. The ICP-MS was developed for the purpose of easily carrying out spectral analysis with high sensibility by using argon ICP as the ion source and doing ion detection which is more efficient than light detection, and has lower background. The progress and the present status of the ICP-MS are reported. As the latest examples of application of the ICP-MS, the analysis of iron by quadrupole type ICP-MS, the small region measurement of solids by laser abrasion, ultra-minute amount analysis by high resolution ICP-MS, the isotope ratio measurement of lead by multi-collector type ICP-MS are reported. (K.I.)

  12. Segmental analysis of amphetamines in hair using a sensitive UHPLC-MS/MS method.

    Science.gov (United States)

    Jakobsson, Gerd; Kronstrand, Robert

    2014-06-01

    A sensitive and robust ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed and validated for quantification of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine and 3,4-methylenedioxy methamphetamine in hair samples. Segmented hair (10 mg) was incubated in 2M sodium hydroxide (80°C, 10 min) before liquid-liquid extraction with isooctane followed by centrifugation and evaporation of the organic phase to dryness. The residue was reconstituted in methanol:formate buffer pH 3 (20:80). The total run time was 4 min and after optimization of UHPLC-MS/MS-parameters validation included selectivity, matrix effects, recovery, process efficiency, calibration model and range, lower limit of quantification, precision and bias. The calibration curve ranged from 0.02 to 12.5 ng/mg, and the recovery was between 62 and 83%. During validation the bias was less than ±7% and the imprecision was less than 5% for all analytes. In routine analysis, fortified control samples demonstrated an imprecision <13% and control samples made from authentic hair demonstrated an imprecision <26%. The method was applied to samples from a controlled study of amphetamine intake as well as forensic hair samples previously analyzed with an ultra high performance liquid chromatography time of flight mass spectrometry (UHPLC-TOF-MS) screening method. The proposed method was suitable for quantification of these drugs in forensic cases including violent crimes, autopsy cases, drug testing and re-granting of driving licences. This study also demonstrated that if hair samples are divided into several short segments, the time point for intake of a small dose of amphetamine can be estimated, which might be useful when drug facilitated crimes are investigated. Copyright © 2014 John Wiley & Sons, Ltd.

  13. Efficient analysis and extraction of MS/MS result data from Mascot™ result files

    Directory of Open Access Journals (Sweden)

    Sickmann Albert

    2005-12-01

    Full Text Available Abstract Background Mascot™ is a commonly used protein identification program for MS as well as for tandem MS data. When analyzing huge shotgun proteomics datasets with Mascot™'s native tools, limits of computing resources are easily reached. Up to now no application has been available as open source that is capable of converting the full content of Mascot™ result files from the original MIME format into a database-compatible tabular format, allowing direct import into database management systems and efficient handling of huge datasets analyzed by Mascot™. Results A program called mres2x is presented, which reads Mascot™ result files, analyzes them and extracts either selected or all information in order to store it in a single file or multiple files in formats which are easier to handle downstream of Mascot™. It generates different output formats. The output of mres2x in tab format is especially designed for direct high-performance import into relational database management systems using native tools of these systems. Having the data available in database management systems allows complex queries and extensive analysis. In addition, the original peak lists can be extracted in DTA format suitable for protein identification using the Sequest™ program, and the Mascot™ files can be split, preserving the original data format. During conversion, several consistency checks are performed. mres2x is designed to provide high throughput processing combined with the possibility to be driven by other computer programs. The source code including supplement material and precompiled binaries is available via http://www.protein-ms.de and http://sourceforge.net/projects/protms/. Conclusion The database upload allows regrouping of the MS/MS results using a database management system and complex analyzing queries using SQL without the need to run new Mascot™ searches when changing grouping parameters.

  14. Identification and Quantification of Several Mammalian Steroid Hormones in Plants by UPLC-MS/MS

    Czech Academy of Sciences Publication Activity Database

    Simerský, Radim; Novák, Ondřej; Morris, David; Pouzar, Vladimír; Strnad, Miroslav

    2009-01-01

    Roč. 28, č. 2 (2009), s. 125-136 ISSN 0721-7595 R&D Projects: GA AV ČR KAN200380801 Institutional research plan: CEZ:AV0Z50380511; CEZ:AV0Z40550506 Keywords : Ultra-performance liquid chromatography (UPLC) * Tandem mass spectrometry (MS/MS) * Immunoaffinity purification * Steroids * Plant extracts * Digitalis purpurea * Nicotiana tabacum * Inula helenium Subject RIV: EC - Immunology Impact factor: 2.438, year: 2009

  15. Dried blood spot analysis of creatinine with LC-MS/MS in addition to immunosuppressants analysis

    NARCIS (Netherlands)

    Koster, Remco A.; Greijdanus, Ben; Alffenaar, Jan-Willem C.; Touw, Daan J.

    In order to monitor creatinine levels or to adjust the dosage of renally excreted or nephrotoxic drugs, the analysis of creatinine in dried blood spots (DBS) could be a useful addition to DBS analysis. We developed a LC-MS/MS method for the analysis of creatinine in the same DBS extract that was

  16. Chemical characterization of neonicotinoids in surface waters by high performance liquid chromatography with Tandem Mass Spectrometry (HPLC MS/MS)

    International Nuclear Information System (INIS)

    Amaral, Priscila Oliveira

    2017-01-01

    The present study aimed to develop a method for the determination and validation of a method for the identification and quantification of Neonicotinoids in surface waters collected in the Bauru region, in the state of São Paulo. The analytical techniques studied for the development of this method were the high performance liquid chromatography with tandem mass spectrometry (HPLC - MS / MS), gas chromatography with mass spectrometry (GC / MS) and gas chromatography with electron capture detector (GC / ECD). The class of pesticides Neonicotinoids was chosen for this work because it is related to a sudden disappearance of bees in colonies around the world. This phenomenon is known as Colony Collapse Disorder (CCD) and it is characterized by a rapid loss in the population of adult bees. The Neonicotinoids used in this study were the compounds Clothianidin, Imidacloprid and Thiamethoxam which were banned in their use as pesticides in Europe by Implementing Regulation No. 540/2011. The samples were concentrated using solid phase extraction (SPE) and liquid liquid extraction (LLE) techniques and injected into HPLC-MS / MS, GC / MS and GC / ECD. The GC / ECD and GC / MS techniques were not satisfactory for determination in the water matrix because the detection limit (10 mg L -1 ) is above the maximum allowed by the US Environmental Protection Agency (0.6 μg L -1 ). The HPLC - MS / MS technique using the multiple reaction monitoring (MRM) proved to be adequate for this study because it obtained quantification limits between 5.89 and 8.06 μg L -1 and a linearity between 0.9963 and 0.9999 for the three compounds. (author)

  17. Alberto Urrets-Zavalía Jr (1920-2010): An Argentinian contributor to ophthalmology.

    Science.gov (United States)

    Grzybowski, Andrzej; Urrets-Zavalía, Julio A; Ascaso, Francisco J

    2016-05-01

    Alberto Urrets-Zavalía Jr was born in Córdoba (Argentina) in 1920. Chairman of the Department of Ophthalmology of the National University of Córdoba and founder of the Cornea and Glaucoma Surgical Center in the same city, in 1956 he created the first residency programme in Ophthalmology in his country. He founded the first Eye Bank and introduced one of the first argon laser photocoagulators in South America. He authored around 200 scientific presentations and publications, describing new findings and clinical entities. Thus, his individualisation of the cyclovertical component in strabismus contributed to important evolution of ideas concerning pathogenesis and therapy in oculomotor disorders of infancy. He was the first to propose the dehydration of the vitreous body in glaucoma patients before ocular surgery and developed a fixation pick and scleral depressor for retinal detachment surgery. He also described a new technique, the V-Z procedures for the correction of senile ectropion. In 1968, he published his Décollement de la rétine, considered a masterpiece in retinal detachment literature for many years. Urrets-Zavalía died in his native city at the age of 89. His prolific scientific and educational contributions make him one of the most brilliant and influential ophthalmologists of the 20th-century. © The Author(s) 2014.

  18. Analysis of multiple vitamin D metabolites by ultra-performance supercritical fluid chromatography-tandem mass spectrometry (UPSFC-MS/MS).

    Science.gov (United States)

    Jenkinson, Carl; Taylor, Angela; Storbeck, Karl-Heinz; Hewison, Martin

    2018-06-15

    In recent years, increased interest in the human health benefits of vitamin D has led to demand for improved analysis of patient vitamin D 'status'. Studies to date have focused primarily on a single vitamin D metabolite, 25-hydroxyvitamin D, despite the existence of a broad range of vitamin D metabolites, referred to as the vitamin D metabolome. This study reports on the development of a rapid UPSFC-MS/MS method for the analysis of nine vitamin D metabolites in human serum. Optimum separation was obtained with a Lux-Cellulose chiral column. We observed an orthogonal elution order when compared with ultra-high performance liquid chromatography (UHPLC). The order of elution was reversed based on hydroxyl- group number, however elution order did not differ between isomeric changes in hydroxyl- group position or epimers. Although UPSFC yielded superior resolution and selectivity over previously developed UHPLC-MS/MS methods, improvements in sensitivity could not be achieved owing to the lower injection volume required for UPSFC relative to UHPLC. Method validation was performed on the developed UPSFC-MS/MS method and found to be within acceptable limits. Applying the method to the analysis of human serum samples showed a significant correlation with serum concentrations of metabolites measured by UHPLC-MS/MS (25OHD3 r = 0.997, P=<0.001, and 3-epi-25OHD3 r = 0.996, P ≤0.001). These data indicate that UPSFC provides an efficient analytical platform for rapid analysis of multiple vitamin D metabolites from serum. Crown Copyright © 2018. Published by Elsevier B.V. All rights reserved.

  19. Development of an LC-MS/MS method for the determination of pesticides and patulin in apples

    DEFF Research Database (Denmark)

    Christensen, Hanne Bjerre; Poulsen, Mette Erecius; Rasmussen, Peter Have

    2009-01-01

    A method for the simultaneous determination of 33 pesticides or degradation products together with patulin in apples by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed. The method involved homogenization of the apples, extraction with ammonium acetate-acetic acid solution...... in methanol-water by ultrasonication, filtration, and determination by LC-MS/MS. The repeatability and within-laboratory reproducibility for the three spiking levels 0.02, 0.04 and 0.2 mg kg(-1) were between 4% and 35%. In general, the repeatability and reproducibility were about 10-20%. The limits...... of quantification (LOQs) were between 0.01 and 0.14 mg kg(-1). The method was used on incurred samples from parts of the ISAFRUIT project financed by the European Commission under the 6th Framework Programme. Samples were analysed at four different stages: after harvest, after storage (controlled), after a water...

  20. Taxus ingredients in the red arils of Taxus baccata L. determined by HPLC-MS/MS.

    Science.gov (United States)

    Siegle, Lydia; Pietsch, Jörg

    2018-02-09

    Taxus baccata L. is an evergreen conifer whose plant parts are cardiotoxic. Only the red arils of the berries are described as non-toxic and taxane-free. Extraction and HPLC-MS/MS methods were developed for the investigation of the Taxus compounds 3,5-dimethoxyphenol, 10-deacetylbaccatin III, baccatin III, cephalomannine, taxol A and taxinine M in the red arils of the yew berries. MethodologyA liquid-liquid extraction method for the red arils of the fruits from three yews were developed. An accurate (ESI+) HPLC-MS/MS method was performed for the simultaneous detection and determination of the target compounds in multiple reaction monitoring (MRM) mode. All Taxus agents obtained were detected in the red arils. Highest concentrations were determined for baccatin III and 10-deacetylbaccatin III. The developed quantitative method is reliable and selective and was successfully applied for quantification of selected Taxus ingredients in red arils of Taxus baccata. It was disproved that the red arils of the berries do not contain the selected Taxus compounds. Copyright © 2018 John Wiley & Sons, Ltd.

  1. UPLC-MS/MS based diagnostics for epithelial ovarian cancer using fully sialylated C4-binding protein.

    Science.gov (United States)

    Tanabe, Kazuhiro; Matsuo, Koji; Miyazawa, Masaki; Hayashi, Masaru; Ikeda, Masae; Shida, Masako; Hirasawa, Takeshi; Sho, Ryuichiro; Mikami, Mikio

    2018-05-01

    Serum levels of fully sialylated C4-binding protein (FS-C4BP) are remarkably elevated in patients with epithelial ovarian cancer (EOC) and can be used as a marker to distinguish ovarian clear cell carcinoma from endometrioma. This study aimed to develop a stable, robust and reliable liquid chromatography-hybrid mass spectrometry (UPLC-MS/MS) based diagnostic method that would generalize FS-C4BP as a clinical EOC biomarker. Glycopeptides derived from 20 μL of trypsin-digested serum glycoprotein were analyzed via UPLC equipped with an electrospray ionization time-of-flight mass spectrometer. This UPLC-MS/MS-based diagnostic method was optimized for FS-C4BP and validated using sera from 119 patients with EOC and 127 women without cancer. A1958 (C4BP peptide with two fully sialylated biantennary glycans) was selected as a marker of FS-C4BP because its level in serum was highest among FS-C4BP family members. Preparation and UPLC-MS/MS were optimized for A1958, and performance and robustness were significantly improved relative to our previous method. An area under the curve analysis of the FS-C4BP index receiver operating characteristic curve revealed that the ratio between A1958 and A1813 (C4BP peptide with two partially sialylated biantennary glycans) reached 85%. A combination of the FS-C4BP index and carbohydrate antigen-125 levels further enhanced the sensitivity and specificity. © 2017 The Authors. Biomedical Chromatography published by John Wiley & Sons Ltd.

  2. Report on the survey of geothermal development at Okushiri Island, Hokkaido. Geochemical survey (GC/MS and MS method); Hokkaido Okushiritou chinetsu kaihatsu chosa chikagaku chosa (GC/MS and MS ho) hokokusho

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1991-09-01

    To elucidate chemical components of soil gas in the Okushiri Island area, soil gas was collected by the method using charcoal adsorbent, and analysis was made by the GC/MS method. Out of the 19 measuring points, 17 points were set up near the measuring points in the FY 1998 survey by the finger print method. At the same measuring points, analytical survey by the MS method was also conducted to sort the type of soil gas. As a result of the GC/MS analysis, xylene or ethyl benzene was detected at 12 measuring points of all 19 measuring points, and from the distribution, it was predicted that there were anomaly zones in the district along the road of the Okushiri Island line and the district southward from the 5.8K Pass. These results were in harmony with the results of the survey by the finger print method. As to the sorting of soil gas based on the results of the MS analysis, the results were different at 8 measuring points from those of the survey by the finger print method in FY 1998. It was considered that the cause was the accidental vaporization of a large quantity of acetaldehyde, and acetaldehyde was regarded as a noise gas component that does not reflect the geothermal structure. (NEDO)

  3. Determination of rhenium traces in river water by Q-ICP-MS and HR-ICP-MS

    International Nuclear Information System (INIS)

    Uchida, S.; Tagami, K.; Saito, M.

    2003-01-01

    A simple separation method was applied to determine rhenium in river water using Q-ICP-MS and HR-ICP-MS. Re was concentrated from 420-925 ml river water using a TEVA resin minicolumn. Such extraction using a resin could separate Re from most sample matrices and trace elements. Almost 100% recovery was found throughout the method as determined with radioactive multitracers. The HR-ICP-MS was also used for the direct determination because of its low detection limit for Re (0.007 pg/ml). The Re concentration in the river water samples ranged from 0.9 to 6.5 pg/ml and the three analysis results showed good agreement with each other. (author)

  4. Simultaneous quantitative analysis of nine vitamin D compounds in human blood using LC-MS/MS.

    Science.gov (United States)

    Abu Kassim, Nur Sofiah; Gomes, Fabio P; Shaw, Paul Nicholas; Hewavitharana, Amitha K

    2016-01-01

    It has been suggested that each member of the family of vitamin D compounds may have different function(s). Therefore, selective quantification of each compound is important in clinical research. Development and validation attempts of a simultaneous determination method of 12 vitamin D compounds in human blood using precolumn derivatization followed by LC-MS/MS is described. Internal standard calibration with 12 stable isotope labeled analogs was used to correct for matrix effects in MS detector. Nine vitamin D compounds were quantifiable in blood samples with detection limits within femtomole levels. Serum (compared with plasma) was found to be a more suitable sample type, and protein precipitation (compared with saponification) a more effective extraction method for vitamin D assay.

  5. O desenvolvimento de competências por meio da extensão universitária: o caso da Global Jr. ESPM-SP na formação do diplomata corporativo

    Directory of Open Access Journals (Sweden)

    Diego Bonaldo Coelho

    2017-09-01

    Full Text Available O artigo apresenta o debate sobre a relevância da extensão universitária como ação para o desenvolvimento de competências acadêmicas e profissionais em graduandos de Relações Internacionais. Para investigação, utilizou-se como fio condutor de análise um modelo específico de atividade extensionista, a empresa júnior, por meio de estudo de caso da Global Jr. da ESPM-SP. Os resultados observados sugerem impactos positivos do empreendimento tanto na formação quanto na empregabilidade dos estudantes, corroborando estudos realizados por Terrim et al (2015 e Barbosa et al (2016. The paper presents the debate over the relevancy of university extension as a source of academic and professional skills development in undergraduate students of International Relations. For the investigation it was used a specific model of extensionist activity, the junior company, through the case study of Global Jr. from ESPM-SP. The results which were observed suggest positive impacts of the enterprise both in education and in employment of the students, corroborating with studies conducted by Terrim et al (2015 and Barbosa et al (2016.

  6. Preclinical pharmacokinetic evaluation and metabolites identification of methyl salicylate-2-O-β-d-lactoside in rats using LC-MS/MS and Q-TOF-MS methods.

    Science.gov (United States)

    Zhang, Dan; Huang, Chao; Xin, Wenyu; Ma, Xiaowei; Zhang, Weiku; Zhang, Tiantai; Du, Guanhua

    2015-05-10

    Methyl salicylate-2-O-β-d-lactoside (MSL) is a natural salicylate derivative from the traditional Chinese medicine of Gaultheria yunnanensis (Franch.) Rehder (G. yunnanensis). As a non-steroidal anti-inflammatory drug (NSAID), MSL exerts a significant anti-arthritis effect but hardly has any gastrointestinal toxicity. In this paper, the pharmacokinetics, distribution, excretion and identification of MSL and its metabolites are described following rat oral and intravenous administration. The biological samples were quantified by UPLC-MS/MS and the metabolites in urine and feces were identified by using Q-TOF-MS. These results will support future investigations leading to clinical development of this drug. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. STS-48 MS Buchli and MS Gemar on MB SMS middeck during JSC training session

    Science.gov (United States)

    1991-01-01

    STS-48 Discovery, Orbiter Vehicle (OV) 103, Mission Specialist (MS) James F. Buchli (left) and MS Charles D. Gemar listen to instructions while on the middeck of JSC's Motion Based (MB) Shuttle Mission Simulator (SMS). Buchli and Gemar are reviewing inflight procedures during this preflight familiarization session held in the Mission Simulation and Training Facility Bldg 5.

  8. Study of the performance of three LC-MS/MS platforms for analysis of perfluorinated compounds

    Energy Technology Data Exchange (ETDEWEB)

    Llorca, Marta; Farre, Marinella [IDAEA-CSIC, Department of Environmental Chemistry, Barcelona (Spain); Pico, Yolanda [Universitat de Valencia, Laboratori de Nutricio i Bromatologia, Facultat de Farmacia, Burjassot, Valencia (Spain); Barcelo, Damia [IDAEA-CSIC, Department of Environmental Chemistry, Barcelona (Spain); King Saud University, Riyadh (Saudi Arabia)

    2010-10-15

    The analytical suitabilities of three different liquid chromatography-tandem mass spectrometry (LC-MS/MS) systems, (1) triple quadrupole (QqQ), (2) conventional 3D ion trap (IT), and (3) quadrupole-linear IT (QqLIT), to determine trace levels of perfluorinated compounds (PFCs) in fish and shellfish were compared. Sample preparation was performed using alkaline extraction and solid-phase-extraction cleanup. This evaluation was focused on both quantitative (sensitivity, precision, and accuracy) and qualitative (identification capabilities) aspects. In the three instruments, the former facet was evaluated using selected reaction monitoring (SRM), which is the standard mode for quantitative LC-MS/MS analysis. Accuracy was similar in the three systems, with recoveries always over 70 %. Precision was better for the QqLIT and QqQ systems (7-15%) than for the IT system (10-17%). The QqLIT (working in SRM mode) and QqQ systems offered a linear dynamic range of at least 3 orders of magnitude, whereas that of the IT system was 2 orders of magnitude. The QqLIT system achieved at least 20-fold higher sensitivity than the QqQ system, and this was at least tenfold higher sensitivity than for the IT system. In the IT system, identification was based on sensitive full mass range acquisition and MS{sup n} fragmentation and in the QqLIT system, it was based on the use of an information-dependent-acquisition scan function, which allows the combination of an SRM or MS full scan acting as the survey scan and an enhanced product ion scan followed by MS{sup 3} as the dependent scan in the same analysis. Three instruments were applied to monitor the content in fish and shellfish (anchovies, swordfish, tuna, mussels, and oysters) obtained from Valencia and Barcelona markets (Spain). The eight target PFCs were detected at mean concentrations in the range from 10 ng kg {sup -1} (perfluoro-7-methyloctanoic acid and perfluoro-1-decanesulfonate) to 4,200 ng kg {sup -1} (perfluoropentanoic acid

  9. HPLC-MS and GC-MS analyses combined with orthogonal partial least squares to identify cytotoxic constituents from turmeric (Curcuma longa L.).

    Science.gov (United States)

    Jiang, Jianlan; Zhang, Huan; Li, Zidan; Zhang, Xiaohang; Su, Xin; Li, Yan; Qiao, Bin; Yuan, Yingjin

    2013-08-01

    We investigated the fingerprints of 48 batches of turmeric total extracts (TTE) by HPLC-MS-MS and GC-MS analyses and 43 characteristic peaks (22 constituents from HPLC-MS-MS; 21 from GC-MS) were analyzed qualitatively and quantitatively. An MTT {3-(4,5-dimethylthiazol-2-yl)- 2,5-diphenyltetrazolium bromide} assay was implemented to measure the cytotoxicity of the TTE against HeLa cells. Then we utilized orthogonal partial least squares analysis, which correlated the chemical composition of the TTE to its cytotoxic activity, to identify potential cytotoxic constituents from turmeric. The result showed that 19 constituents contributed significantly to the cytotoxicity. The obtained result was verified by canonical correlation analysis. Comparison with previous reports also indicated some interaction between the curcuminoids and sesquiterpenoids in turmeric.

  10. Effect of Genetics, Environment, and Phenotype on the Metabolome of Maize Hybrids Using GC/MS and LC/MS.

    Science.gov (United States)

    Tang, Weijuan; Hazebroek, Jan; Zhong, Cathy; Harp, Teresa; Vlahakis, Chris; Baumhover, Brian; Asiago, Vincent

    2017-06-28

    We evaluated the variability of metabolites in various maize hybrids due to the effect of environment, genotype, phenotype as well as the interaction of the first two factors. We analyzed 480 forage and the same number of grain samples from 21 genetically diverse non-GM Pioneer brand maize hybrids, including some with drought tolerance and viral resistance phenotypes, grown at eight North American locations. As complementary platforms, both GC/MS and LC/MS were utilized to detect a wide diversity of metabolites. GC/MS revealed 166 and 137 metabolites in forage and grain samples, respectively, while LC/MS captured 1341 and 635 metabolites in forage and grain samples, respectively. Univariate and multivariate analyses were utilized to investigate the response of the maize metabolome to the environment, genotype, phenotype, and their interaction. Based on combined percentages from GC/MS and LC/MS datasets, the environment affected 36% to 84% of forage metabolites, while less than 7% were affected by genotype. The environment affected 12% to 90% of grain metabolites, whereas less than 27% were affected by genotype. Less than 10% and 11% of the metabolites were affected by phenotype in forage and grain, respectively. Unsupervised PCA and HCA analyses revealed similar trends, i.e., environmental effect was much stronger than genotype or phenotype effects. On the basis of comparisons of disease tolerant and disease susceptible hybrids, neither forage nor grain samples originating from different locations showed obvious phenotype effects. Our findings demonstrate that the combination of GC/MS and LC/MS based metabolite profiling followed by broad statistical analysis is an effective approach to identify the relative impact of environmental, genetic and phenotypic effects on the forage and grain composition of maize hybrids.

  11. Accurate determination of ultra-trace levels of Ti in blood serum using ICP-MS/MS

    International Nuclear Information System (INIS)

    Balcaen, Lieve; Bolea-Fernandez, Eduardo; Resano, Martín; Vanhaecke, Frank

    2014-01-01

    Graphical abstract: -- Highlights: •Novel method for determination of Ti at ultra-trace levels in clinical samples (serum). •Novel method based on Ti(NH 3 ) 6 + reaction product ion formation and double mass selection using recently introduced ICP-QQQ instrumentation. •Lowest limits of detection ever obtained using quadrupole-based instrumentation for Ti. •Accurate determination of basal levels of Ti in blood serum. -- Abstract: Ti is frequently used in implants and prostheses and it has been shown before that the presence of these in the human body can lead to elevated Ti concentrations in body fluids such as serum and urine. As identification of the exact mechanisms responsible for this increase in Ti concentrations, and the risks associated with it, are not fully understood, it is important to have sound analytical methods that enable straightforward quantification of Ti levels in body fluids (for both implanted and non-implanted individuals). Until now, only double-focusing sector field ICP-mass spectrometry (SF-ICP-MS) offered limits of detection that are good enough to deal with the very low basal levels of Ti in human serum. This work reports on the development of a novel method for the accurate and precise determination of trace levels of Ti in human serum samples, based on the use of ICP-MS/MS. O 2 and NH 3 /He have been compared as reaction gases. While the use of O 2 did not enable to overcome all spectral interferences, it has been shown that conversion of Ti + ions into Ti(NH 3 ) 6 + cluster ions by using NH 3 /He as a reaction gas in an ICP-QQQ-MS system, operated in MS/MS mode, provided interference-free conditions and sufficiently low limits of detection, down to 3 ng L −1 (instrumental detection limit obtained for the most abundant Ti isotope). The accuracy of the method proposed was evaluated by analysis of a Seronorm Trace Elements Serum L-1 reference material and by comparing the results obtained with those achieved by means of SF-ICP-MS

  12. 76 FR 76480 - Request for Comments on Canada's Expression of Interest in the Proposed Trans-Pacific Partnership...

    Science.gov (United States)

    2011-12-07

    ... Trade Representative. ACTION: Request for comments. SUMMARY: Canadian Prime Minister Stephen Harper... Minister Stephen Harper stated Canada's interest in joining the TPP negotiations. The Chair of the...) Relevant electronic commerce issues. (g) Relevant trade-related intellectual property rights issues. (h...

  13. Potential Health Benefits and Metabolomics of Camel Milk by GC-MS and ICP-MS.

    Science.gov (United States)

    Ahamad, Syed Rizwan; Raish, Mohammad; Ahmad, Ajaz; Shakeel, Faiyaz

    2017-02-01

    None of the research reports reveals the metabolomics and elemental studies on camel milk. Recent studies showed that camel milk possesses anticancer and anti-inflammatory activity. Metabolomics and elemental studies were carried out in camel milk which showed us the pathways and composition that are responsible for the key biological role of camel milk. Camel milk was dissolved in methanol and chloroform fraction and then vortexed and centrifuged. Both the fractions were derivatized by N,O-bis-(trimethylsilyl)trifluoroacetamide (BSTFA) and TMCS after nitrogen purging and analyzed by GC-MS. Camel milk was also analyzed by ICP-MS after microwave digestion. We found that higher alkanes and fatty acids are present in the chloroform fraction and amino acids, sugars and fatty acid derivatives are present in aqueous fractions. All the heavy metals like As, Pb, Cd, Co, Cu, and Ni were in the safe limits in terms of maximum daily intake of these elements. Na, K, Mg, and Ca were also present in the safe limits in terms of maximum daily intake of these elements. These results suggested that the camel milk drinking is safe and there is no health hazard. The present data of GC-MS and ICP-MS correlate the activities related to camel milk.

  14. Wavelet-Based Peak Detection and a New Charge Inference Procedure for MS/MS Implemented in ProteoWizard’s msConvert

    Science.gov (United States)

    2015-01-01

    We report the implementation of high-quality signal processing algorithms into ProteoWizard, an efficient, open-source software package designed for analyzing proteomics tandem mass spectrometry data. Specifically, a new wavelet-based peak-picker (CantWaiT) and a precursor charge determination algorithm (Turbocharger) have been implemented. These additions into ProteoWizard provide universal tools that are independent of vendor platform for tandem mass spectrometry analyses and have particular utility for intralaboratory studies requiring the advantages of different platforms convergent on a particular workflow or for interlaboratory investigations spanning multiple platforms. We compared results from these tools to those obtained using vendor and commercial software, finding that in all cases our algorithms resulted in a comparable number of identified peptides for simple and complex samples measured on Waters, Agilent, and AB SCIEX quadrupole time-of-flight and Thermo Q-Exactive mass spectrometers. The mass accuracy of matched precursor ions also compared favorably with vendor and commercial tools. Additionally, typical analysis runtimes (∼1–100 ms per MS/MS spectrum) were short enough to enable the practical use of these high-quality signal processing tools for large clinical and research data sets. PMID:25411686

  15. Analysis of the constituents in jojoba wax used as a food additive by LC/MS/MS.

    Science.gov (United States)

    Tada, Atsuko; Jin, Zhe-Long; Sugimoto, Naoki; Sato, Kyoko; Yamazaki, Takeshi; Tanamoto, Kenichi

    2005-10-01

    Jojoba wax is a natural gum base used as a food additive in Japan, and is obtained from jojoba oil with a characteristically high melting point. Although the constituents of jojoba oil have been reported, the quality of jojoba wax used as a food additive has not yet been clarified. In order to evaluate its quality as a food additive and to obtain basic information useful for setting official standards, we investigated the constituents and their concentrations in jojoba wax. LC/MS analysis of the jojoba wax showed six peaks with [M+H]+ ions in the range from m/z 533.6 to 673.7 at intervals of m/z 28. After isolation of the components of the four main peaks by preparative LC/MS, the fatty acid and long chain alcohol moieties of the wax esters were analyzed by methanolysis and hydrolysis, followed by GC/MS. The results indicated that the main constituents in jojoba wax were various kinds of wax esters, namely eicosenyl octadecenoate (C20:1-C18:1) (1), eicosenyl eicosenoate (C20:1-C20:1) (II), docosenyl eicosenoate (C22:1-C20:1) (III), eicosenyl docosenoate (C20:1-C22:1) (IV) and tetracosenyl eiosenoate (C24:1-C20:1) (V). To confirm and quantify the wax esters in jojoba wax directly, LC/MS/MS analysis was performed. The product ions corresponding to the fatty acid moieties of the wax esters were observed, and by using the product ions derived from the protonated molecular ions of wax esters the fatty acid moieties were identified by MRM analysis. The concentrations of the wax esters I, II and III, in jojoba wax were 5.5, 21.4 and 37.8%, respectively. In summary, we clarified the main constituents of jojoba wax and quantified the molecular species of the wax esters without hydrolysis by monitoring their product ions, using a LC/MS/MS system.

  16. Importance of MS selectivity and chromatographic separation in LC-MS/MS-based methods when investigating pharmaceutical metabolites in water. Dipyrone as a case of study.

    Science.gov (United States)

    Ibáñez, M; Gracia-Lor, E; Sancho, J V; Hernández, F

    2012-08-01

    Pharmaceuticals are emerging contaminants of increasing concern because of their presence in the aquatic environment and potential to reach drinking-water sources. After human and/or veterinary consumption, pharmaceuticals can be excreted in unchanged form, as the parent compound, and/or as free or conjugated metabolites. Determination of most pharmaceuticals and metabolites in the environment is commonly made by liquid chromatography (LC) coupled to mass spectrometry (MS). LC coupled to tandem MS is the technique of choice nowadays in this field. The acquisition of two selected reaction monitoring (SRM) transitions together with the retention time is the most widely accepted criterion for a safe quantification and confirmation assay. However, scarce attention is normally paid to the selectivity of the selected transitions as well as to the chromatographic separation. In this work, the importance of full spectrum acquisition high-resolution MS data using a hybrid quadrupole time-of-flight analyser and/or a suitable chromatographic separation (to reduce the possibility of co-eluting interferences) is highlighted when investigating pharmaceutical metabolites that share common fragment ions. For this purpose, the analytical challenge associated to the determination of metabolites of the widely used analgesic dipyrone (also known as metamizol) in urban wastewater is discussed. Examples are given on the possibilities of reporting false positives of dypirone metabolites by LC-MS/MS under SRM mode due to a wrong assignment of identity of the compounds detected. Copyright © 2012 John Wiley & Sons, Ltd.

  17. Gaining knowledge from previously unexplained spectra-application of the PTM-Explorer software to detect PTM in HUPO BPP MS/MS data.

    Science.gov (United States)

    Chamrad, Daniel C; Körting, Gerhard; Schäfer, Heike; Stephan, Christian; Thiele, Herbert; Apweiler, Rolf; Meyer, Helmut E; Marcus, Katrin; Blüggel, Martin

    2006-09-01

    A novel software tool named PTM-Explorer has been applied to LC-MS/MS datasets acquired within the Human Proteome Organisation (HUPO) Brain Proteome Project (BPP). PTM-Explorer enables automatic identification of peptide MS/MS spectra that were not explained in typical sequence database searches. The main focus was detection of PTMs, but PTM-Explorer detects also unspecific peptide cleavage, mass measurement errors, experimental modifications, amino acid substitutions, transpeptidation products and unknown mass shifts. To avoid a combinatorial problem the search is restricted to a set of selected protein sequences, which stem from previous protein identifications using a common sequence database search. Prior to application to the HUPO BPP data, PTM-Explorer was evaluated on excellently manually characterized and evaluated LC-MS/MS data sets from Alpha-A-Crystallin gel spots obtained from mouse eye lens. Besides various PTMs including phosphorylation, a wealth of experimental modifications and unspecific cleavage products were successfully detected, completing the primary structure information of the measured proteins. Our results indicate that a large amount of MS/MS spectra that currently remain unidentified in standard database searches contain valuable information that can only be elucidated using suitable software tools.

  18. High temperature liquid chromatography hyphenated with ESI-MS and ICP-MS detection for the structural characterization and quantification of halogen containing drug metabolites

    International Nuclear Information System (INIS)

    Vlieger, Jon S.B. de; Giezen, Mark J.N.; Falck, David; Tump, Cornelis; Heuveln, Fred van; Giera, Martin; Kool, Jeroen; Lingeman, Henk; Wieling, Jaap; Honing, Maarten; Irth, Hubertus; Niessen, Wilfried M.A.

    2011-01-01

    Highlights: → Hyphenation of high temperature liquid chromatography to ICP-MS and ESI-MS. → Structural characterization of kinase inhibitor metabolites with high resolution MS n experiments. → Quantification of drug metabolites with ICP-MS based on Iodine detection. → Significant changes in ESI-MS response after small structural changes. - Abstract: In this paper we describe the hyphenation of high temperature liquid chromatography with ICP-MS and ESI-MS for the characterization of halogen containing drug metabolites. The use of temperature gradients up to 200 deg. C enabled the separation of metabolites with low organic modifier content. This specific property allowed the use of detection methods that suffer from (significant) changes in analyte response factors as a function of the organic modifier content such as ICP-MS. Metabolites of two kinase inhibitors (SB-203580-Iodo and MAPK inhibitor VIII) produced by bacterial cytochrome P450 BM3 mutants and human liver microsomes were identified based on high resolution MS n data. Quantification was done using their normalized and elemental specific response in the ICP-MS. The importance of these kinds of quantification strategies is stressed by the observation that the difference of the position of one oxygen atom in a structure can greatly affect its response in ESI-MS and UV detection.

  19. In vivo Phosphoproteome of Human Skeletal Muscle Revealed by Phosphopeptide Enrichment and HPLC-ESI-MS/MS

    DEFF Research Database (Denmark)

    Højlund, Kurt; Bowen, Benjamin P; Hwang, Hyonson

    2009-01-01

    volunteers. Trypsin digestion of 3-5 mg human skeletal muscle protein was followed by phosphopeptide enrichment using SCX and TiO2. The resulting phosphopeptides were analyzed by HPLC-ESI-MS/MS. Using this unbiased approach, we identified 306 distinct in vivo phosphorylation sites in 127 proteins, including...

  20. Biodiesel production from microalgal isolates of southern Pakistan and quantification of FAMEs by GC-MS/MS analysis

    Directory of Open Access Journals (Sweden)

    Musharraf Syed

    2012-12-01

    Full Text Available Abstract Background Microalgae have attracted major interest as a sustainable source for biodiesel production on commercial scale. This paper describes the screening of six microalgal species, Scenedesmus quadricauda, Scenedesmus acuminatus, Nannochloropsis sp., Anabaena sp., Chlorella sp. and Oscillatoria sp., isolated from fresh and marine water resources of southern Pakistan for biodiesel production and the GC-MS/MS analysis of their fatty acid methyl esters (FAMEs. Results Growth rate, biomass productivity and oil content of each algal species have been investigated under autotrophic condition. Biodiesel was produced from algal oil by acid catalyzed transesterification reaction and resulting fatty acid methyl esters (FAMEs content was analyzed by GC/MS. Fatty acid profiling of the biodiesel, obtained from various microalgal oils showed high content of C-16:0, C-18:0, cis-Δ9C-18:1, cis-Δ11C-18:1 (except Scenedesmus quadricauda and 10-hydroxyoctadecanoic (except Scenedesmus acuminatus. Absolute amount of C-14:0, C-16:0 and C-18:0 by a validated GC-MS/MS method were found to be 1.5-1.7, 15.0-42.5 and 4.2-18.4 mg/g, respectively, in biodiesel obtained from various microalgal oils. Biodiesel was also characterized in terms of cetane number, kinematic viscosity, density and higher heating value and compared with the standard values. Conclusion Six microalgae of local origin were screened for biodiesel production. A method for absolute quantification of three important saturated fatty acid methyl esters (C-14, C-16 and C-18 by gas chromatography-tandem mass spectrometry (GC-MS/MS, using multiple reactions monitoring (MRM mode, was employed for the identification and quantification of biodiesels obtained from various microalgal oils. The results suggested that locally found microalgae can be sustainably harvested for the production of biodiesel. This offers the tremendous economic opportunity for an energy-deficient nation.

  1. A comparison of the determination and speciation of inorganic arsenic using general HPLC methodology with UV, MS and MS/MS detection.

    Science.gov (United States)

    Gilmartin, Gregory; Gingrich, Diane

    2018-04-15

    The determination and speciation of arsenic in natural resources such as drinking water and agricultural soils has been a growing concern in recent years due to its many toxicological effects [1-3]. To speciate and quantitate concentrations of arsenic, typically an ion chromatograph (IC) interfaced to an inductively coupled plasma mass spectrometer (ICP-MS) is employed [4-9]. This methodology may be very robust and sensitive, but it is expensive and not as ubiquitous as high performance liquid chromatography (HPLC) with ultraviolet (UV) absorbance detection or electrospray ionization mass spectrometry (ESI-MS). Anion exchange chromatography is a well-documented means of speciating arsenite (As(III), As 2 O 3 ) and arsenate (As(V), AsO 4 ) using UV [10], conductivity [11], or ESI-MS detection [12,13]. This paper demonstrates the utilization of common liquid chromatographic instrumentation to speciate and determines inorganic Arsenic compounds using UV or MS via selected ion recording (SIR) or multiple reaction monitoring (MRM) detection. This paper describes the analysis of arsenite and arsenate samples prepared using both deionized and ground water. The limit of quantitation for the techniques described in this paper for samples spiked in ground water were 454 ppb (As(III)) and 562 ppb (As(V)) for UV detection, 45.4 ppb (As(III)) and 56.2 ppb (As(V)) for SIR detection, and 4.54 ppb (As(III)) and 5.62 ppb (As(V)) for MRM detection. Copyright © 2018 Elsevier B.V. All rights reserved.

  2. UP-HILIC-MS/MS to Determine the Action Pattern of Penicillium sp. Dextranase

    Science.gov (United States)

    Yi, Lin; Sun, Xue; Du, Kenze; Ouyang, Yilan; Wu, Chengling; Xu, Naiyu; Linhardt, Robert J.; Zhang, Zhenqing

    2015-07-01

    Investigation of the action pattern of enzymes acting on carbohydrates is challenging, as both the substrate and the digestion products are complex mixtures. Dextran and its enzyme-derived oligosaccharides are widely used for many industrial applications. In this work, a new method relying on ultra-performance hydrophilic interaction liquid chromatography quadrupole time-of-flight tandem mass spectrometry (UP-HILIC- Q/TOF-MS/MS) was developed to analyze a complex mixture of dextran oligosaccharide products to determine the action pattern of dextranase. No derivatization of oligosaccharides was required and the impact of the α- and β-configurations of the native oligosaccharides on the chromatographic separation was eliminated. The 1→6, 1→3, 1→4 backbone linkages and the branch linkages of these oligosaccharides were all distinguished from diagnostic ions in their MS/MS spectra, including fragments corresponding to 0,2A, 0,3A, 0,4A, B-H2O, 2,5A, and 3,5A. The sequences of the oligosaccharide products were similarly established. Thus, the complex oligosaccharide mixtures in dextran digestion products were profiled and identified using this method. The more enzyme-resistant structures in dextran were established using much less sample, labor, time, and uncertainty than in previous studies. This method provides an efficient, sensitive, and straightforward way to monitor the entire process of digestion, establish the action pattern of the dextranase from Penicillium sp., and to support the proper industrial application of dextranase.

  3. Analysis of pesticides in fruit, vegetables and cereals using methanolic extraction and detection by LC-MS/MS

    DEFF Research Database (Denmark)

    Granby, Kit; Andersen, Jens Hinge; Christensen, Hanne Bjerre

    2004-01-01

    Abstract: A method for analysing carbamates and other relatively polar pesticides by LC–MS–MS with electrospray ionisation has been developed. The method is based on extraction by ultrasonication using a methanolic ammonium acetate–acetic acid buffer. After centrifugation the samples are filtered...... in Miniprep filter HPLC vials and detected by LC–MS–MS. To compensate for variations in the MS response [13C6]-carbaryl was used as internal standard and matrix-matched pesticide solutions were used as external standards for the quantification. The method has been validated for the matrices apple, avocado...

  4. Analysis of a Brazilian green propolis from Baccharis dracunculifolia by HPLC-APCI-MS and GC-MS

    Directory of Open Access Journals (Sweden)

    Roberto Chang

    Full Text Available Ethanol and dichloromethane extracts of a Brazilian green propolis from Baccharis dracunculifolia were analyzed by HPLC-APCI-MS and GC-MS, respectively. The HPLC-APCI-MS technique, at the positive mode, furnished a complete and unequivocal chemical composition of the green propolis sample. It serves as fingerprint for different propolis samples. The composition of the ethanol extract consisted mainly of cinnamic acid and derivatives, flavonoids, benzoic acid and a few benzoates, non-hydroxylated aromatics, and aliphatic acids and esters, which are normally not reported in the literature because they do not absorb UV light. The main constituents of the dichloromethane extract were prenylated compounds, alkanes and terpenoids.

  5. 78 FR 77780 - Qualification of Drivers; Exemption Applications; Vision

    Science.gov (United States)

    2013-12-24

    ...), Stephen R. Marshall (MS), Edgar H. Meraz (NM), Ralph Reno (NJ), Glennis R. Reynolds (KY), Joseph B... Thomas (PA), Clifford B. Thompson, Jr. (SC), Donald L. Urmston (OH), Steven M. Veloz (CA), Stephen H...), James L. Hawthorne (TX), Johnny D. Ivey (NC), Darryl H. Johnson (WV), David Jones (FL), Thomas L...

  6. Progression in familial and nonfamilial MS

    NARCIS (Netherlands)

    Koch, Marcus; Uyttenboogaart, Maarten; Heerings, Marco; Heersema, Dorothea; Mostert, Jop; De Keyser, Jacques

    Objective To investigate whether the timing of secondary or primary progression is different between patients with familial and nonfamilial multiple sclerosis (MS). Methods Information on the family history of 313 patients with MS was taken from our prospective hospital-based database. We used

  7. Analytical Method Details (MS): SE60_MS01 [Metabolonote[Archive

    Lifescience Database Archive (English)

    Full Text Available stem and Waters Q-Tof Premier UPLC-QTOF-MS ESI Positive The supernatant (3 μl) were subsequently subjected to metabolome...g were conducted according to a previously described method (Matsuda et al., 2009, 2010). Briefly, metabolome

  8. Analytical Method Details (MS): SE53_MS01 [Metabolonote[Archive

    Lifescience Database Archive (English)

    Full Text Available .25-μl film Rtx-5 Sil MS stationary phase (RESTEK, Bellefonte, USA) for metabolome... analysis. Helium was used as the carrier gas at a constant flow rate of 1 ml min-1. The temperature program for metabolome

  9. PCI-GC-MS-MS approach for identification of non-amino organic acid and amino acid profiles.

    Science.gov (United States)

    Luan, Hemi; Yang, Lin; Ji, Fenfen; Cai, Zongwei

    2017-03-15

    Alkyl chloroformate have been wildly used for the fast derivatization of metabolites with amino and/or carboxyl groups, coupling of powerful separation and detection systems, such as GC-MS, which allows the comprehensive analysis of non-amino organic acids and amino acids. The reagents involving n-alkyl chloroformate and n-alcohol are generally employed for providing symmetric labeling terminal alkyl chain with the same length. Here, we developed an asymmetric labeling strategy and positive chemical ionization gas chromatography-tandem mass spectrometry (PCI-GC-MS-MS) approach for determination of non-amino organic acids and amino acids, as well as the short chain fatty acids. Carboxylic and amino groups could be selectively labelled by propyl and ethyl groups, respectively. The specific neutral loss of C 3 H 8 O (60Da), C 3 H 5 O 2 (74Da) and C 4 H 8 O 2 (88Da) were useful in the selective identification for qualitative analysis of organic acids and amino acid derivatives. PCI-GC-MS-MS using multiple reaction monitoring (MRM) was applied for semi-quantification of typical non-amino organic acids and amino acids. This method exhibited a wide range of linear range, good regression coefficient (R 2 ) and repeatability. The relative standard deviation (RSD) of targeted metabolites showed excellent intra- and inter-day precision (chloroformate derivatization. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. High-throughput screening and confirmation of 22 banned veterinary drugs in feedstuffs using LC-MS/MS and high-resolution Orbitrap mass spectrometry.

    Science.gov (United States)

    Wang, Xufeng; Liu, Yanghong; Su, Yijuan; Yang, Jianwen; Bian, Kui; Wang, Zongnan; He, Li-Min

    2014-01-15

    A new analytical strategy based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) combined with accurate mass high-resolution Orbitrap mass spectrometry (HR-Orbitrap MS) was performed for high-throughput screening, confirmation, and quantification of 22 banned or unauthorized veterinary drugs in feedstuffs according to Bulletin 235 of the Ministry of Agriculture, China. Feed samples were extracted with acidified acetonitrile, followed by cleanup using solid-phase extraction cartridge. The extracts were first screened by LC-MS/MS in a single selected reaction monitoring mode. The suspected positive samples were subjected to a specific pretreatment for confirmation and quantification of analyte of interest with LC-MS/MS and HR-Orbitrap MS. Mean recoveries for all target analytes (except for carbofuran and chlordimeform, which were about 35 and 45%, respectively) ranged from 52.2 to 90.4%, and the relative standard deviations were screening of real samples obtained from local feed markets and confirmation of the suspected target analytes. It provides a high-throughput, sensitive, and reliable screening, identification, and quantification of banned veterinary drugs in routine monitoring programs of feedstuffs.

  11. Detecting pM concentrations of prostaglandins in cell culture supernatants by capillary SCX-LC-MS/MS

    DEFF Research Database (Denmark)

    Dahl, Sandra Rinne; Kleiveland, Charlotte Ramstad; Kassem, Moustapha

    2008-01-01

    A highly sensitive, improved online strong cation exchange (SCX)--RP capillary liquid chromatographic (cLC) method with IT mass spectrometric (IT-MS/MS) detection for the simultaneous determination of prostaglandin (PG)A(1), PGD(2), PGE(1), PGE(2), PGF(2alpha), 8-iso-(8i)PGF(2alpha), 6-keto-(6k...

  12. Simultaneous quantitation of sphingoid bases by UPLC-ESI-MS/MS with identical (13)C-encoded internal standards

    NARCIS (Netherlands)

    Mirzaian, M.; Wisse, P.; Ferraz, M. J.; Marques, A. R. A.; Gaspar, P.; Oussoren, S. V.; Kytidou, K.; Codée, J. D. C.; van der Marel, G.; Overkleeft, H. S.; Aerts, J. M.

    2017-01-01

    Free sphingoid bases (lysosphingolipids) of primary storage sphingolipids are increased in tissues and plasma of several sphingolipidoses. As shown earlier by us, sphingoid bases can be accurately quantified using UPLC-ESI-MS/MS, particularly in combination with identical (13)C-encoded internal

  13. Multisteroid LC–MS/MS assay for glucocorticoids and androgens and its application in Addison's disease

    Science.gov (United States)

    Methlie, Paal; Hustad, Steinar; Kellman, Ralf; Almås, Bjørg; Erichsen, Martina M; Husebye, Eystein S; Løvås, Kristian

    2013-01-01

    Objective Liquid chromatography–tandem mass spectrometry (LC–MS/MS) offers superior analytical specificity compared with immunoassays, but it is not available in many regions and hospitals due to expensive instrumentation and tedious sample preparation. Thus, we developed an automated, high-throughput LC–MS/MS assay for simultaneous quantification of ten endogenous and synthetic steroids targeting diseases of the hypothalamic–pituitary–adrenal axis and gonads. Methods Deuterated internal standards were added to 85 μl serum and processed by liquid–liquid extraction. Cortisol, cortisone, prednisolone, prednisone, 11-deoxycortisol, dexamethasone, testosterone, androstenedione and progesterone were resolved by ultra-high-pressure chromatography on a reversed-phase column in 6.1 min and detected by triple-quadrupole mass spectrometry. The method was used to assess steroid profiles in women with Addison's disease (AD, n=156) and blood donors (BDs, n=102). Results Precisions ranged from 4.5 to 10.1% relative standard deviations (RSD), accuracies from 95 to 108% and extraction recoveries from 60 to 84%. The method was practically free of matrix effects and robust to individual differences in serum composition. Most postmenopausal AD women had extremely low androstenedione concentrations, below 0.14 nmol/l, and median testosterone concentrations of 0.15 nmol/l (interquartile range 0.00–0.41), considerably lower than those of postmenopausal BDs (1.28 nmol/l (0.96–1.64) and 0.65 nmol/l (0.56–1.10) respectively). AD women in fertile years had androstenedione concentrations of 1.18 nmol/l (0.71–1.76) and testosterone concentrations of 0.44 nmol/l (0.22–0.63), approximately half of those found in BDs of corresponding age. Conclusion This LC–MS/MS assay provides highly sensitive and specific assessments of glucocorticoids and androgens with low sample volumes and is suitable for endocrine laboratories and research. Its utility has been

  14. MRI atlas of MS lesions

    Energy Technology Data Exchange (ETDEWEB)

    Sahraian, Mohammad Ali [Tehran Univ. of Medical Sciences Sina Hospital (Iran). Dept. of Neurology; Radue, Ernst-Wilhelm [Univ. Hospital Basel (Switzerland). Dept. of Neuroradiology

    2008-07-01

    MRI has become the main paraclinical test in the diagnosis and management of multiple sclerosis. We have demonstrated more than 400 pictures of different typical and atypical MS lesions in this atlas. Each image has a teaching point. New diagnostic criteria and differential diagnosis are discussed and the book is supported by a teaching DVD where the reader can see MS lesions in different slices and sequences. (orig.)

  15. Comparative study for toxic elements determination in air particulate reference material by INAA, CCT-ICP-MS, and ICP-MS

    International Nuclear Information System (INIS)

    Lim, J.M.; Lee, J.H.; Kim, K.H.; Moon, J.H.; Chung, Y.S.

    2005-01-01

    Although toxic elements are minor components in the atmospheric environment, they play a significant role as important marker for atmospheric science such as risk assessment, long-range transfer study, and source apportionment. Therefore, the techniques, which allow accurate and fast elemental analysis with a minimum pre-treatment, are very important. INAA has a main advantage of non-destruction of air particulate samples, while inductively Coupled plasma with mass spectrometry (ICP-MS) encounters the most significant difficulties in pre-treatment (digestion, fusion, and dilution) and polyatomic spectral interferences for interest toxic elements, Although INAA is still reference method, a number of factors (disadvantages of cost, complexity of the instruments, and scarcity of nuclear reactor) limit its applications. To date, the use of collision cell technology ICP-MS (CCT-ICP-MS) is recommended instead of typical ICP-MS for the analysis of the toxic elements; this is because CCT-ICP-MS technique prevents polyatomic spectral interferences despite of contamination and volatile effects. In this study, a number of toxic elements in reference material, NIST SRM 2783 (air particulate on filter media) were determined by INAA, CCT-ICP-MS, and ICP-MS. For both ICP methods, the filters were decomposed by microwave digestion with 5mL nitric acid. The analytical results by three methods were compared with certificated data; the INAA results showed the most accurate and precise data sets for all target elements among three methods. In detail, the deviation between analytical results and SRM's by INAA fell below 10% for all elements excluding As (14%), while those by CCT-ICP-MS were about 20%. For ICP-MS, the result does not agree with certificated data for several elements, because polyatomic spectral interference (due to 40 Ar 35 Cl, 40 Ar 23 Na, and 35 Cl 16 O) generate positive error of analytical result for As, Cu, and V. Based on our result, INAA is still one of the most

  16. Integrated Solid-Phase Extraction-Capillary Liquid Chromatography (speLC) Interfaced to ESI-MS/MS for Fast Characterization and Quantification of Protein and Proteomes

    DEFF Research Database (Denmark)

    Falkenby, Lasse Gaarde; Such-Sanmartín, Gerard; Larsen, Martin Røssel

    2014-01-01

    min speLC-MS/MS experiment. Analysis by selected reaction monitoring by speLC-SRM-MS/MS of distinct peptides derived from the blood proteins IGF1, IGF2, IBP2, and IBP3 demonstrated protein quantification with CV values below 10% across 96 replicates. The speLC-MS/MS system is ideally suited for fast......The high peptide sequencing speed provided by modern hybrid tandem mass spectrometers enables the utilization of fast liquid chromatographic (LC) separation techniques. We present a robust solid-phase extraction/capillary LC system (speLC) for 5-10 min separation of semicomplex peptide mixtures...

  17. ESI(+-MS and GC-MS Study of the Hydrolysis of N-Azobenzyl Derivatives of Chitosan

    Directory of Open Access Journals (Sweden)

    Fernanda S. Pereira

    2014-10-01

    Full Text Available New N-p-chloro-, N-p-bromo-, and N-p-nitrophenylazobenzylchitosan derivatives, as well as the corresponding azophenyl and azophenyl-p-sulfonic acids, were synthesized by coupling N-benzylvchitosan with aryl diazonium salts. The synthesized molecules were analyzed by UV-Vis, FT-IR, 1H-NMR and 15N-NMR spectroscopy. The capacity of copper chelation by these materials was studied by AAS. Chitosan and the derivatives were subjected to hydrolysis and the products were analyzed by ESI(+-MS and GC-MS, confirming the formation of N-benzyl chitosan. Furthermore, the MS results indicate that a nucleophilic aromatic substitution (SnAr reaction occurs under hydrolysis conditions, yielding chloroaniline from N-p-bromo-, and N-p-nitrophenylazo-benzylchitosan as well as bromoaniline from N-p-chloro-, and N-p-nitrophenylazobenzyl-chitosan.

  18. Identification of hormone esters in injection site in muscle tissues by LC/MS/MS.

    Science.gov (United States)

    Costain, R M; Fesser, A C E; McKenzie, D; Mizuno, M; MacNeil, J D

    2008-12-01

    The detection of hormone abuse for growth promotion in food animal production is a global concern. Initial testing for hormones in Canada was directed at the compounds approved for use in beef cattle, melengestrol acetate, trenbolone acetate and zeranol, and the banned compound diethylstilbestrol (DES). No hormonal growth promoters are approved for use in veal production in Canada. However, instances of use of trenbolone and clenbuterol were detected in Canada in the 1990s. During the development of a new analytical method for testosterone and progesterone, there were reports of suspicious injection sites being found in veal calves. Upon implementation of the method, analysis of investigative samples revealed significant residues of testosterone in some injection sites. To prove that the source of these residues was exogenous, a fully validated method for hormone esters was developed to confirm the presence of exogenous hormones in these injection sites. The QUECHERS model was employed in methods development and resulted in a simple, effective extraction technique that consisted of sample pre-homogenization, liquid/liquid partitioning, extract dilution, filtration and use of LC/MS/MS to provide detection selectivity. The result was an adaptable MS/MS confirmation technique that meets the needs of Canadian regulatory authorities to confirm the misuse of injectable testosterone, and potentially other hormones, in food animal production.

  19. A sensitive LC-MS/MS method for measurement of organophosphorus pesticides and their oxygen analogs in air sampling matrices.

    Science.gov (United States)

    Armstrong, Jenna L; Dills, Russell L; Yu, Jianbo; Yost, Michael G; Fenske, Richard A

    2014-01-01

    A rapid liquid chromatography tandem mass spectrometry (LC-MS/MS) method has been developed for determination of levels of the organophosphorus (OP) pesticides chlorpyrifos (CPF), azinphos methyl (AZM), and their oxygen analogs chlorpyrifos-oxon (CPF-O) and azinphos methyl-oxon (AZM-O) on common active air sampling matrices. XAD-2 resin and polyurethane foam (PUF) matrices were extracted with acetonitrile containing stable-isotope labeled internal standards (ISTD). Analysis was accomplished in Multiple Reaction Monitoring (MRM) mode, and analytes in unknown samples were identified by retention time (±0.1 min) and qualifier ratio (±30% absolute) as compared to the mean of calibrants. For all compounds, calibration linearity correlation coefficients were ≥0.996. Limits of detection (LOD) ranged from 0.15-1.1 ng/sample for CPF, CPF-O, AZM, and AZM-O on active sampling matrices. Spiked fortification recoveries were 78-113% from XAD-2 active air sampling tubes and 71-108% from PUF active air sampling tubes. Storage stability tests also yielded recoveries ranging from 74-94% after time periods ranging from 2-10 months. The results demonstrate that LC-MS/MS is a sensitive method for determining these compounds from two different matrices at the low concentrations that can result from spray drift and long range transport in non-target areas following agricultural applications. In an inter-laboratory comparison, the limit of quantification (LOQ) for LC-MS/MS was 100 times lower than a typical gas chromatography-mass spectrometry (GC-MS) method.

  20. Simultaneous Determination of Multi-Mycotoxins in Cereal Grains Collected from South Korea by LC/MS/MS

    Directory of Open Access Journals (Sweden)

    Dong-Ho Kim

    2017-03-01

    Full Text Available An improved analytical method compared with conventional ones was developed for simultaneous determination of 13 mycotoxins (deoxynivalenol, nivalenol, 3-acetylnivalenol, aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, fumonisin B1, fumonisin B2, T-2, HT-2, zearalenone, and ochratoxin A in cereal grains by liquid chromatography-tandem mass spectrometry (LC/MS/MS after a single immunoaffinity column clean-up. The method showed a good linearity, sensitivity, specificity, and accuracy in mycotoxin determination by LC/MS/MS. The levels of 13 mycotoxins in 5 types of commercial grains (brown rice, maize, millet, sorghum, and mixed cereal from South Korea were determined in a total of 507 cereal grains. Mycotoxins produced from Fusarium sp. (fumonisins, deoxynivalenol, nivalenol, and zearalenone were more frequently (more than 5% and concurrently detected in all cereal grains along with higher mean levels (4.3–161.0 ng/g in positive samples than other toxins such as aflatoxins and ochratoxin A (less than 9% and below 5.2 ng/g in positive samples from other fungal species.

  1. METHOD 544. DETERMINATION OF MICROCYSTINS AND NODULARIN IN DRINKING WATER BY SOLID PHASE EXTRACTION AND LIQUID CHROMATOGRAPHY/TANDEM MASS SPECTROMETRY (LC/MS/MS)

    Science.gov (United States)

    Method 544 is an accurate and precise analytical method to determine six microcystins (including MC-LR) and nodularin in drinking water using solid phase extraction and liquid chromatography tandem mass spectrometry (SPE-LC/MS/MS). The advantage of this SPE-LC/MS/MS is its sensi...

  2. Simultaneous quantification of the organophosphorus pesticides dimethoate and omethoate in porcine plasma and urine by LC-ESI-MS/MS and flow-injection-ESI-MS/MS.

    Science.gov (United States)

    John, Harald; Eddleston, Michael; Clutton, R Eddie; Worek, Franz; Thiermann, Horst

    2010-05-15

    Dimethoate is an organophosphorus toxicant used in agri- and horticulture as a systemic broad-spectrum insecticide. It also exhibits toxic activity towards mammalian organism provoked by catalytic desulfuration in the liver producing its oxon-derivative omethoate thus inhibiting acetylcholinesterase, initiating cholinergic crisis and ultimately leading to death by respiratory paralysis and cardiovascular collapse. Pharmaco- and toxicokinetic studies in animal models help to broaden basic understanding of medical intervention by antidotes and supportive care. Therefore, we developed and validated a LC-ESI-MS/MS method suitable for the simultaneous, selective, precise (RSD(intra-day) 1-8%; RSD(inter-day) 5-14%), accurate (intra-day: 95-107%; inter-day: 90-115%), and robust quantification of both pesticides from porcine urine and plasma after deproteinization by precipitation and extensive dilution (1:11,250 for plasma and 1:40,000 for urine). Accordingly, lower limits of quantification (0.24-0.49 microg/ml plasma and 0.78-1.56 microg/ml urine) and lower limits of detection (0.12-0.24 microg/ml plasma and 0.39-0.78 microg/ml urine) were equivalent to quite low absolute on-column amounts (1.1-2.1 pg for plasma and 2.0-3.9 pg for urine). The calibration range (0.24-250 microg/ml plasma and 0.78-200 microg/ml urine) was subdivided into two linear ranges (r(2)>or=0.998) each covering nearly two orders of magnitude. The lack of any interfering peak in 6 individual blank specimens from plasma and urine demonstrated the high selectivity of the method. Furthermore, extensive sample dilution causing lowest concentration of potentially interfering matrix ingredients prompted us to develop and validate an additional flow-injection method (FI-ESI-MS/MS). Validation characteristics were as good as for the chromatographic method but sample throughput was enhanced by a factor of 6. Effects on ionization provoked by plasma and urine matrix from 6 individuals as well as in the

  3. Methylation-Sensitive High Resolution Melting (MS-HRM).

    Science.gov (United States)

    Hussmann, Dianna; Hansen, Lise Lotte

    2018-01-01

    Methylation-Sensitive High Resolution Melting (MS-HRM) is an in-tube, PCR-based method to detect methylation levels at specific loci of interest. A unique primer design facilitates a high sensitivity of the assays enabling detection of down to 0.1-1% methylated alleles in an unmethylated background.Primers for MS-HRM assays are designed to be complementary to the methylated allele, and a specific annealing temperature enables these primers to anneal both to the methylated and the unmethylated alleles thereby increasing the sensitivity of the assays. Bisulfite treatment of the DNA prior to performing MS-HRM ensures a different base composition between methylated and unmethylated DNA, which is used to separate the resulting amplicons by high resolution melting.The high sensitivity of MS-HRM has proven useful for detecting cancer biomarkers in a noninvasive manner in urine from bladder cancer patients, in stool from colorectal cancer patients, and in buccal mucosa from breast cancer patients. MS-HRM is a fast method to diagnose imprinted diseases and to clinically validate results from whole-epigenome studies. The ability to detect few copies of methylated DNA makes MS-HRM a key player in the quest for establishing links between environmental exposure, epigenetic changes, and disease.

  4. Quantitation of iothalamate in urine and plasma using liquid chromatography electrospray tandem mass spectrometry (HPLC-ESI-MS/MS).

    Science.gov (United States)

    Molinaro, Ross J; Ritchie, James C

    2010-01-01

    The following chapter describes a method to measure iothalamate in plasma and urine samples using high performance liquid chromatography combined with electrospray positive ionization tandem mass spectrometry (HPLC-ESI-MS/MS). Methanol and water are spiked with the internal standard (IS) iohexol. Iothalamate is isolated from plasma after IS spiked methanol extraction and from urine by IS spiked water addition and quick-spin filtration. The plasma extractions are dried under a stream of nitrogen. The residue is reconstituted in ammonium acetate-formic acid-water. The reconstituted plasma and filtered urine are injected into the HPLC-ESI-MS/MS. Iothalamate and iohexol show similar retention times in plasma and urine. Quantification of iothalamate in the samples is made by multiple reaction monitoring using the hydrogen adduct mass transitions, from a five-point calibration curve.

  5. UPLC-MS/MS determination of ptaquiloside and pterosin B in preserved natural water.

    Science.gov (United States)

    Clauson-Kaas, Frederik; Hansen, Hans Christian Bruun; Strobel, Bjarne W

    2016-11-01

    The naturally occurring carcinogen ptaquiloside and its degradation product pterosin B are found in water leaching from bracken stands. The objective of this work is to present a new sample preservation method and a fast UPLC-MS/MS method for quantification of ptaquiloside and pterosin B in environmental water samples, employing a novel internal standard. A faster, reliable, and efficient method was developed for isolation of high purity ptaquiloside and pterosin B from plant material for use as analytical standards, with purity verified by 1 H-NMR. The chemical analysis was performed by cleanup and preconcentration of samples with solid phase extraction, before analyte quantification with UPLC-MS/MS. By including gradient elution and optimizing the liquid chromatography mobile phase buffer system, a total run cycle of 5 min was achieved, with method detection limits, including preconcentration, of 8 and 4 ng/L for ptaquiloside and pterosin B, respectively. The use of loganin as internal standard improved repeatability of the determination of both analytes, though it could not be employed for sample preparation. Buffering raw water samples in situ with ammonium acetate to pH ∼5.5 decisively increased sample integrity at realistic transportation and storing conditions prior to extraction. Groundwater samples collected in November 2015 at the shallow water table below a Danish bracken stand were preserved and analyzed using the above methods, and PTA concentrations of 3.8 ± 0.24 μg/L (±sd, n = 3) were found, much higher than previously reported. Graphical abstract Workflow overview of ptaquiloside determination.

  6. Characterization of the Photon Counting CHASE Jr., Chip Built in a 40-nm CMOS Process With a Charge Sharing Correction Algorithm Using a Collimated X-Ray Beam

    Energy Technology Data Exchange (ETDEWEB)

    Krzyżanowska, A. [AGH-UST, Cracow; Deptuch, G. W. [Fermilab; Maj, P. [AGH-UST, Cracow; Gryboś, P. [AGH-UST, Cracow; Szczygieł, R. [AGH-UST, Cracow

    2017-08-01

    This paper presents the detailed characterization of a single photon counting chip, named CHASE Jr., built in a CMOS 40-nm process, operating with synchrotron radiation. The chip utilizes an on-chip implementation of the C8P1 algorithm. The algorithm eliminates the charge sharing related uncertainties, namely, the dependence of the number of registered photons on the discriminator’s threshold, set for monochromatic irradiation, and errors in the assignment of an event to a certain pixel. The article presents a short description of the algorithm as well as the architecture of the CHASE Jr., chip. The analog and digital functionalities, allowing for proper operation of the C8P1 algorithm are described, namely, an offset correction for two discriminators independently, two-stage gain correction, and different operation modes of the digital blocks. The results of tests of the C8P1 operation are presented for the chip bump bonded to a silicon sensor and exposed to the 3.5- μm -wide pencil beam of 8-keV photons of synchrotron radiation. It was studied how sensitive the algorithm performance is to the chip settings, as well as the uniformity of parameters of the analog front-end blocks. Presented results prove that the C8P1 algorithm enables counting all photons hitting the detector in between readout channels and retrieving the actual photon energy.

  7. Assessment of global proteome in LNCaP cells by 2D-RP/RP LC–MS/MS following sulforaphane exposure

    Directory of Open Access Journals (Sweden)

    Gregory W. Watson

    2015-12-01

    Full Text Available The phytochemical sulforaphane can induce cell cycle arrest and apoptosis in metastatic prostate cancer cells, though the mechanism of action is not fully known. We conducted a global proteome analysis in LNCaP metastatic prostate cancer cells to characterize how global protein signature responds to sulforaphane. We conducted parallel analyses to evaluate semi-quantitative 1-dimensional versus 2-dimensional liquid chromatography tandem mass spectrometry (LC–MS/MS and their utility in characterizing whole cell lysate. We show that 2-dimensional LC–MS/MS can be a useful tool for characterizing global protein profiles and identify TRIAP1 as a novel regulator of cell proliferation in LNCaP metastatic prostate cancer cells.

  8. UPLC-MS/MS determination of ptaquiloside and pterosin B in preserved natural water

    DEFF Research Database (Denmark)

    Clauson-Kaas, Frederik; Hansen, Hans Chr. Bruun; Strobel, Bjarne W.

    2016-01-01

    and preconcentration of samples with solid phase extraction, before analyte quantification with UPLC-MS/MS. By including gradient elution and optimizing the liquid chromatography mobile phase buffer system, a total run cycle of 5 min was achieved, with method detection limits, including preconcentration, of 8 and 4 ng....../L for ptaquiloside and pterosin B, respectively. The use of loganin as internal standard improved repeatability of the determination of both analytes, though it could not be employed for sample preparation. Buffering raw water samples in situ with ammonium acetate to pH ∼5.5 decisively increased sample integrity...

  9. Polyphasic Approach Including MALDI-TOF MS/MS Analysis for Identification and Characterisation of Fusarium verticillioides in Brazilian Corn Kernels

    Directory of Open Access Journals (Sweden)

    Susane Chang

    2016-02-01

    Full Text Available Fusarium verticillioides is considered one of the most important global sources of fumonisins contamination in food and feed. Corn is one of the main commodities produced in the Northeastern Region of Brazil. The present study investigated potential mycotoxigenic fungal strains belonging to the F. verticillioides species isolated from corn kernels in 3 different Regions of the Brazilian State of Pernambuco. A polyphasic approach including classical taxonomy, molecular biology, MALDI-TOF MS and MALDI-TOF MS/MS for the identification and characterisation of the F. verticillioides strains was used. Sixty F. verticillioides strains were isolated and successfully identified by classical morphology, proteomic profiles of MALDI-TOF MS, and by molecular biology using the species-specific primers VERT-1 and VERT-2. FUM1 gene was further detected for all the 60 F. verticillioides by using the primers VERTF-1 and VERTF-2 and through the amplification profiles of the ISSR regions using the primers (GTG5 and (GACA4. Results obtained from molecular analysis shown a low genetic variability among these isolates from the different geographical regions. All of the 60 F. verticillioides isolates assessed by MALDI-TOF MS/MS presented ion peaks with the molecular mass of the fumonisin B1 (721.83 g/mol and B2 (705.83 g/mol.

  10. Pharmacokinetic studies of bergapten in dog plasma by using a LC-MS/MS method studies.

    Science.gov (United States)

    Gao, Y; Liu, Y Z; Zhang, X-M; Zhou, Y; Zhang, X; Dong, C-Y

    2013-07-01

    A sensitive LC-MS/MS method was developed for the determination of bergapten in dog plasma. The chromatographic separation was carried out on a Hypersil ODS column with a mobile phase consisting of methanol-water. The plasma sample was precipitated with methanol and prepare for injecting onto the LC-MS/MS system. The detection was performed on a triple quadrupole tandem mass spectrometer by MRM via electro spray ionization source. The standard curve for bergapten was linear over the concentration range of 0.5-500 ng/mL with a lower limit of quantification of 0.5 ng/mL. The inter-day and intra-day precision (R.S.D.%) for bergapten varied between 3.4 and 11.5. The corresponding inter-day and intra-day accuracy (Bias%) ranged between -3.8 and 6.9. For the pharmacokinetic analysis of serum, the mean (SD) values obtained for the bergapten were as follows: Cmax, 228.5 (14.3) ng/ml; Tmax, 4.2 (0.4) h; t1/2, 6.9 (2.3) h; AUC0-t h, 2507.2 (168.5) ng · h/mL and AUC0-∞, 3 219.2 (211.4) ng · h/mL, respectively. © Georg Thieme Verlag KG Stuttgart · New York.

  11. UPLC-MS/MS Method for Simultaneous Determination of Three Major Metabolites of Mequindox in Holothurian

    Directory of Open Access Journals (Sweden)

    Huihui Liu

    2018-01-01

    Full Text Available This study developed an ultraperformance liquid chromatography tandem mass spectrometry (UPLC-MS/MS method for the detection of three major metabolites of mequindox, including 3-methyl-quinoxaline-2-carboxylic acid, 1-desoxymequindox, and 1,4-bisdesoxymequindox (MQCA, 1-DMEQ, and BDMEQ, in holothurian. Target analytes were simplified with ultrasound-assisted acidolysis extracted without complicated enzymolysis steps. After that, each sample was centrifuged and purified by an Oasis MAX cartridge. Then, the processed samples were separated and monitored by UPLC-MS/MS. This developed method has been validated according to FDA criteria. At fortified levels of 2, 10, and 20 μg/kg, recoveries ranged from 82.5% to 93.5% with the intraday RSD less than 7.27% and interday RSD less than 11.8%. The limit of detection (LOD of all the three metabolites ranged from 0.21 to 0.48 μg/kg, while the limit of quantification (LOQ ranged from 0.79 to 1.59 μg/kg. On application to commercial samples, 14 of 20 samples were detected positive for the three target analytes, with positive rate at 70 percentage. The result indicated that this method was specific, sensitive, and suitable for the quantification and conformation of the three major metabolites of MEQ in holothurian.

  12. Development of an Advanced HPLC–MS/MS Method for the Determination of Carotenoids and Fat-Soluble Vitamins in Human Plasma

    Directory of Open Access Journals (Sweden)

    Barbora Hrvolová

    2016-10-01

    Full Text Available The concentration of carotenoids and fat-soluble vitamins in human plasma may play a significant role in numerous chronic diseases such as age-related macular degeneration and some types of cancer. Although these compounds are of utmost interest for human health, methods for their simultaneous determination are scarce. A new high pressure liquid chromatography (HPLC-tandem mass spectrometry (MS/MS method for the quantification of selected carotenoids and fat-soluble vitamins in human plasma was developed, validated, and then applied in a pilot dietary intervention study with healthy volunteers. In 50 min, 16 analytes were separated with an excellent resolution and suitable MS signal intensity. The proposed HPLC–MS/MS method led to improvements in the limits of detection (LOD and quantification (LOQ for all analyzed compounds compared to the most often used HPLC–DAD methods, in some cases being more than 100-fold lower. LOD values were between 0.001 and 0.422 µg/mL and LOQ values ranged from 0.003 to 1.406 µg/mL, according to the analyte. The accuracy, precision, and stability met with the acceptance criteria of the AOAC (Association of Official Analytical Chemists International. According to these results, the described HPLC-MS/MS method is adequately sensitive, repeatable and suitable for the large-scale analysis of compounds in biological fluids.

  13. Development of an Advanced HPLC–MS/MS Method for the Determination of Carotenoids and Fat-Soluble Vitamins in Human Plasma

    Science.gov (United States)

    Hrvolová, Barbora; Martínez-Huélamo, Miriam; Colmán-Martínez, Mariel; Hurtado-Barroso, Sara; Lamuela-Raventós, Rosa Maria; Kalina, Jiří

    2016-01-01

    The concentration of carotenoids and fat-soluble vitamins in human plasma may play a significant role in numerous chronic diseases such as age-related macular degeneration and some types of cancer. Although these compounds are of utmost interest for human health, methods for their simultaneous determination are scarce. A new high pressure liquid chromatography (HPLC)-tandem mass spectrometry (MS/MS) method for the quantification of selected carotenoids and fat-soluble vitamins in human plasma was developed, validated, and then applied in a pilot dietary intervention study with healthy volunteers. In 50 min, 16 analytes were separated with an excellent resolution and suitable MS signal intensity. The proposed HPLC–MS/MS method led to improvements in the limits of detection (LOD) and quantification (LOQ) for all analyzed compounds compared to the most often used HPLC–DAD methods, in some cases being more than 100-fold lower. LOD values were between 0.001 and 0.422 µg/mL and LOQ values ranged from 0.003 to 1.406 µg/mL, according to the analyte. The accuracy, precision, and stability met with the acceptance criteria of the AOAC (Association of Official Analytical Chemists) International. According to these results, the described HPLC-MS/MS method is adequately sensitive, repeatable and suitable for the large-scale analysis of compounds in biological fluids. PMID:27754400

  14. 50 CFR 660.150 - Mothership (MS) Coop Program.

    Science.gov (United States)

    2010-10-01

    ... follows: (i) Species with formal allocations to the MS Coop Program are Pacific whiting, canary rockfish... issuance for MS permit—(i) Eligibility criteria for MS permit. Only the current owner of a vessel that... mail the application by certified mail to the current address of record in the NMFS permit database...

  15. Video Release: 47th Vice President of the United States Joseph R. Biden Jr. Speech at HUPO2017 Global Leadership Gala | Office of Cancer Clinical Proteomics Research

    Science.gov (United States)

    The Human Proteome Organization (HUPO) has released a video of the keynote speech given by the 47th Vice President of the United States of America Joseph R. Biden Jr. at the HUPO2017 Global Leadership Gala. Under the gala theme “International Cooperation in the Fight Against Cancer,” Biden recognized cancer as a collection of related diseases, the importance of data sharing and harmonization, and the need for collaboration across scientific disciplines as inflection points in cancer research.

  16. High throughput LC-MS/MS method for the simultaneous analysis of multiple vitamin D analytes in serum.

    Science.gov (United States)

    Jenkinson, Carl; Taylor, Angela E; Hassan-Smith, Zaki K; Adams, John S; Stewart, Paul M; Hewison, Martin; Keevil, Brian G

    2016-03-01

    Recent studies suggest that vitamin D-deficiency is linked to increased risk of common human health problems. To define vitamin D 'status' most routine analytical methods quantify one particular vitamin D metabolite, 25-hydroxyvitamin D3 (25OHD3). However, vitamin D is characterized by complex metabolic pathways, and simultaneous measurement of multiple vitamin D metabolites may provide a more accurate interpretation of vitamin D status. To address this we developed a high-throughput liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to analyse multiple vitamin D analytes, with particular emphasis on the separation of epimer metabolites. A supportive liquid-liquid extraction (SLE) and LC-MS/MS method was developed to quantify 10 vitamin D metabolites as well as separation of an interfering 7α-hydroxy-4-cholesten-3-one (7αC4) isobar (precursor of bile acid), and validated by analysis of human serum samples. In a cohort of 116 healthy subjects, circulating concentrations of 25-hydroxyvitamin D3 (25OHD3), 3-epi-25-hydroxyvitamin D3 (3-epi-25OHD3), 24,25-dihydroxyvitamin D3 (24R,25(OH)2D3), 1,25-dihydroxyvitamin D3 (1α,25(OH)2D3), and 25-hydroxyvitamin D2 (25OHD2) were quantifiable using 220μL of serum, with 25OHD3 and 24R,25(OH)2D3 showing significant seasonal variations. This high-throughput LC-MS/MS method provides a novel strategy for assessing the impact of vitamin D on human health and disease. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. It is not Just a Press Conference: The Consequences of Crisis Communication While the World Watches

    Science.gov (United States)

    2014-03-01

    Abraham H. Maslow , Motivation and Personality (New York, NY: Harper and Row, 1970). 26 THIS PAGE INTENTIONALLY LEFT BLANK 27 III. RESEARCH DESIGN...http://www.forbes.com/sites/kenmakovsky/2013/10/03/1159/. Maslow , Abraham H. Motivation and Personality. New York, NY: Harper and Row, 1970. Miles

  18. Dopamine, T cells and multiple sclerosis (MS).

    Science.gov (United States)

    Levite, Mia; Marino, Franca; Cosentino, Marco

    2017-05-01

    Dopamine is a key neurotransmitter that induces critical effects in the nervous system and in many peripheral organs, via 5 dopamine receptors (DRs): D1R-D5R. Dopamine also induces many direct and very potent effects on many DR-expressing immune cells, primarily T cells and dendritic cells. In this review, we focus only on dopamine receptors, effects and production in T cells. Dopamine by itself (at an optimal concentration of~0.1 nM) induces multiple function of resting normal human T cells, among them: T cell adhesion, chemotactic migration, homing, cytokine secretion and others. Interestingly, dopamine activates resting effector T cells (Teffs), but suppresses regulatory T cells (Tregs), and both effects lead eventually to Teff activation. Dopamine-induced effects on T cells are dynamic, context-sensitive and determined by the: T cell activation state, T cell type, DR type, and dopamine concentration. Dopamine itself, and also few dopaminergic molecules/ drugs that are in clinical use for cardiac, neurological and other non-immune indications, have direct effects on human T cells (summarized in this review). These dopaminergic drugs include: dopamine = intropin, L-DOPA, bromocriptine, pramipexole, pergolide, haloperidol, pimozide, and amantadine. Other dopaminergic drugs were not yet tested for their direct effects on T cells. Extensive evidence in multiple sclerosis (MS) and experimental autoimmune encephalomyelitis (EAE) show dopaminergic dysregulations in T cells in these diseases: D1-like DRs are decreased in Teffs of MS patients, and dopamine does not affect these cells. In contrast, D1-like DRs are increased in Tregs of MS patients, possibly causing functional Treg impairment in MS. Treatment of MS patients with interferon β (IFN-β) increases D1-like DRs and decreases D2-like DRs in Teffs, decreases D1-like DRs in Tregs, and most important: restores responsiveness of patient's Teffs to dopamine. DR agonists and antagonists confer some benefits in

  19. LIQUID: an-open source software for identifying lipids in LC-MS/MS-based lipidomics data

    Energy Technology Data Exchange (ETDEWEB)

    Kyle, Jennifer E.; Crowell, Kevin L.; Casey, Cameron P.; Fujimoto, Grant M.; Kim, Sangtae; Dautel, Sydney E.; Smith, Richard D.; Payne, Samuel H.; Metz, Thomas O.

    2017-01-31

    We introduce an open-source software, LIQUID, for semi-automated processing and visualization of LC-MS/MS based lipidomics data. LIQUID provides users with the capability to process high throughput data and contains a customizable target library and scoring model per project needs. The graphical user interface provides visualization of multiple lines of spectral evidence for each lipid identification, allowing rapid examination of data for making confident identifications of lipid molecular species.

  20. Method Development and Validation for UHPLC-MS-MS Determination of Hop Prenylflavonoids in Human Serum

    OpenAIRE

    Yuan, Yang; Qiu, Xi; Nikolic, Dejan; Dahl, Jeffrey H.; van Breemen, Richard B.

    2012-01-01

    Hops (Humulus lupulus L.) are used in the brewing of beer, and hop extracts containing prenylated compounds such as xanthohumol and 8-prenylnaringenin are under investigation as dietary supplements for cancer chemoprevention and for the management of hot flashes in menopausal women. To facilitate clinical studies of hop safety and efficacy, a selective, sensitive, and fast ultra-high pressure liquid chromatography tandem mass spectrometry (UHPLC-MS-MS) method was developed and validated for t...

  1. Survival and mortality rates among Danes with MS

    DEFF Research Database (Denmark)

    Brønnum-Hansen, H; Stenager, Egon; Hansen, Thomas

    2006-01-01

    Long-term survival and trends in overall and cause-specific excess mortality among people with MS have been studied using the Danish Multiple Sclerosis Registry, which contains information about all Danish MS patients since the mid-20th Century. A total of 4254 deaths among approximately 10......,000 people with MS, representing more than 200,000 person-years of observation, have been analysed. Overall, mortality was almost three times higher and life expectancy 10 years less among people with MS than for the general population. However, excess mortality has declined significantly since 1950....

  2. Time correlation between mononucleosis and initial symptoms of MS

    Science.gov (United States)

    Endriz, John; Ho, Peggy P.

    2017-01-01

    Objective: To determine the average age of MS onset vs the age at which Epstein-Barr infection has previously occurred and stratify this analysis by sex and the blood level of Epstein-Barr nuclear antigen 1 (EBNA1) antibody. Methods: Using infectious mononucleosis (IM) as a temporal marker in data from the Swedish epidemiologic investigation of MS, 259 adult IM/MS cases were identified and then augmented to account for “missing” childhood data so that the average age of MS onset could be determined for cases binned by age of IM (as stratified by sex and EBNA1 titer level). Results: Mean age of IM vs mean age of MS reveals a positive time correlation for all IM ages (from ∼5 to ∼30 years), with IM-to-MS delay decreasing with increased age. When bifurcated by sex or EBNA1 blood titer levels, males and high-titer subpopulations show even stronger positive time correlation, while females and low-titer populations show negative time correlation in early childhood (long IM/MS delay). The correlation becomes positive in females beyond puberty. Conclusions: IM/MS time correlation implies causality if IM is time random. Alternative confounding models seem implausible, in light of constraints imposed by time-invariant delay observed here. Childhood infection with Epstein-Barr virus (EBV) in females and/or those genetically prone to low EBNA1 blood titers will develop MS slowly. Males and/or high EBNA1-prone develop MS more rapidly following IM infection at all ages. For all, postpubescent EBV infection is critical for the initiation and rapid development of MS. PMID:28271078

  3. Computer-aided method for identification of major flavone/flavonol glycosides by high-performance liquid chromatography-diode array detection-tandem mass spectrometry (HPLC-DAD-MS/MS).

    Science.gov (United States)

    Wang, Zhengfang; Lin, Longze; Harnly, James M; Harrington, Peter de B; Chen, Pei

    2014-11-01

    A new computational tool is proposed here for tentatively identifying major (UV quantifiable) flavone/flavonol glycoside peaks of high performance liquid chromatogram (HPLC)-diode array detection (DAD)-tandem mass spectrometry (MS/MS) profiles based on a MATLAB-based script implementing an in-house algorithm. The HPLC-DAD-MS/MS profiles of red onion, Chinese lettuce, carrot leaf, and celery seed extracts were analyzed by the proposed computer-aided screening method for identifying possible flavone/flavonol glycoside peaks from the HPLC-UV and MS total ion current (TIC) chromatograms. The number of identified flavone/flavonol glycoside peaks of the HPLC-UV chromatograms is four, four, six, and nine for red onion, Chinese lettuce, carrot leaf, and celery seed, respectively. These results have been validated by human(s) experts. For the batch processing of nine HPLC-DAD-MS/MS profiles of celery seed extract, the entire script execution time was within 15 s while manual calculation of only one HPLC-DAD-MS/MS profile by a flavonoid expert could take hours. Therefore, this MATLAB-based screening method is able to facilitate the HPLC-DAD-MS/MS analysis of flavone/flavonol glycosides in plants to a large extent.

  4. Clinical laboratory verification of thyroglobulin concentrations in the presence of autoantibodies to thyroglobulin: comparison of EIA, radioimmunoassay and LC MS/MS measurements in an Urban Hospital.

    Science.gov (United States)

    Wheeler, Sarah E; Liu, Li; Blair, Harry C; Sivak, Richard; Longo, Nancy; Tischler, Jeffery; Mulvey, Kathryn; Palmer, Octavia M Peck

    2017-12-08

    Thyroglobulin (Tg) measurements assess recurrence in post-thyroidectomy thyroid cancer patients. Tg measurements by enzyme immunoassays (EIA) can be falsely elevated by interference from Tg autoantibodies (TgAb). Radioimmunoassay (RIA) is less susceptible to TgAb interference and has been the standard-of-care test for TgAb positive patients. Recently developed liquid chromatography tandem mass spectrometry (LC-MS/MS) methods may eliminate TgAb interference. We assessed the performance of Tg measurements by EIA, RIA and LC-MS/MS to evaluate TgAb interference differences. We measured TgAb and Tg in 50 plasma samples from 40 patients in whom Tg measurement was part of their routine follow-up and 10 healthy volunteers. Discrepancy between EIA and both LC-MS/MS and RIA was observed at low Tg concentrations (≤ 7.55 ng/mL) in TgAb positive specimens (LC-MS/MS = 1.9 * EIA - 0.03, r = 0.68). RIA and LC-MS/MS Tg measurements in TgAb positive specimens with low Tg concentrations had improved correlation but demonstrated bias (LC MS/MS = 0.6 * RIA - 1.4, r = 0.90). Disagreement between methods may be attributed to LC-MS/MS reported Tg concentrations as undetectable compared to RIA. It seems likely that most discrepant cases are falsely elevated in RIA due to TgAb interference, however, some cases appear below the detection limit of LC-MS/MS; implementation of LC-MS/MS by clinicians will require lower detection limits.

  5. Inductively coupled plasma mass spectrometry (ICP-MS)

    International Nuclear Information System (INIS)

    Shimamura, Tadashi

    1997-01-01

    The period of investigation for the previous general remarks on the progress of ICP-MS was from January, 1991 to September, 1993. In the investigation of this time, for the object of the Chemical Abstracts from January, 1994 to September, 1996, retrieval was carried out by using the STN International. As the key words, ICP-MS, Inductively Coupled Plasma Mass Spectrometry or Inductively Coupled Plasma Mass Spectrometer was used. The number of hit was 373 in 1994, 462 in 1995, and 356 as of September, 1996, 1191 in total. The cumulative number of the papers from 1980 to 1996 is shown. It is known how rapidly the ICP-MS has pervaded as the means of analysis. In order to cope with the enormous number of papers, this time, it was decided to do the review by limiting to the papers which were published in the main journals deeply related to analytical chemistry. As to the tendency in the last three years, it is summarized as how to overcome the spectrum interference and matrix effect in the ICP-MS and the trend of using the ICP-MS as the high sensitivity detector for separation techniques. The technical basic research of the ICP-MS on spectrum interference, sample introduction method and others and the analysis of living body samples are reported. (K.I.)

  6. Measurement of methionine level with the LC-ESI-MS/MS method in schizophrenic patients.

    Science.gov (United States)

    Kulaksizoglu, S; Kulaksizoglu, B; Ellidag, H Y; Eren, E; Yilmaz, N; Baykal, A

    2016-01-01

    The purpose of this study was to evaluate plasma methionine levels by using liquid chromatography electrospray ionization-tandem mass spectroscopy (LC-ESI-MS/MS) in schizophrenic patients. A twelve-point standard graph was drawn, and the recovery rate, the intra-day and inter-day coefficients of variation (CV), the limit of detection (LOD), and the limit of quantification (LOQ) were evaluated. The y and R2 values of the standard graph equation were determined as 0.011x + 0.0179 and 0.9989, respectively, and the graph remained linear until the 200 µmol/l level. The intra-day coefficients of variation of the samples (n = 10) containing 8, 28, and 58 µmol/l methionine were determined as 2.68, 3.10, and 3.79%, respectively; while their inter-day coefficients of variation were determined as 2.98, 3.19, and 3.84%. The LOD and LOQ values were determined as 0.04 and 0.1 µmol/l, respectively, while the mean recovery rates were determined as 101.7 and 99.3%. Plasma methionine values were measured as 21.5 (19.5-24,6) µmol/l for the patient group, 17.8 (16.3-20.1) µmol/l for the control group, and the difference between the two groups was statistically significant (p = 0.03). LC-ESI-MS/MS method represents a fairly sensitive, economic, and rapid analysis that requires very little sample and is suitable for measuring methionine levels in schizophrenic patients.

  7. Neutral Loss Scan - Based Strategy for Integrated Identification of Amorfrutin Derivatives, New Peroxisome Proliferator-Activated Receptor Gamma Agonists, from Amorpha Fruticosa by UPLC-QqQ-MS/MS and UPLC-Q-TOF-MS.

    Science.gov (United States)

    Chen, Chu; Xue, Ying; Li, Qing-Miao; Wu, Yan; Liang, Jian; Qing, Lin-Sen

    2018-04-01

    Amorfrutins with a 2-hydroxybenzoic acid core structure are promising natural PPARγ agonists with potent antidiabetic activity. Owing to the complex matrix and low concentration in botanical material, the identification of unknown amorfrutins remains a challenge. In the present study, a combined application of UPLC-Q-TOF-MS and UPLC-QqQ-MS was developed to discover unknown amorfrutins from fruits of Amorpha fruticosa. First, reference compounds of amorfrutin A (AA), amorfrutin B (AB), and 2-carboxy-3,5-dihydroxy-4-geranylbibenzyl (AC) were analyzed using UPLC-Q-TOF-MS to reveal the characteristic fragment ions and the possible neutral loss. Second, the extract of A. fruticosa was separated and screened by UPLC-QqQ-MS using neutral loss scan to find out suspect compounds associated with the specified neutral fragment Δm/z 44. Third, the extract was re-analyzed by UPLC-Q-TOF-MS to obtain the exact mass of quasi-molecular ion and fragment ions of each suspect compound, and to subsequently calculate their corresponding molecular formulas. Finally, according to the molecular formula of suspect compound and its fragment ions and comparing with literature data, structure elucidation of four unidentified amorfrutins was achieved. The results indicated that the combination of QqQ-MS neutral loss scan and Q-TOF-MS molecular formula calculation was proven to be a powerful tool for unknown natural product identification, and this strategy provides an effective solution to discover natural products or metabolites of trace content. Graphical Abstract ᅟ.

  8. [Separation and identification of red pigments in natural red yolk of duck's eggs by HPLC-MS-MS].

    Science.gov (United States)

    Liu, Liangzhong; Zhang, Min; Peng, Guanghua; Wang, Haibin; Zhang, Shenghua

    2004-05-01

    The natural red yolk of duck's eggs is produced by the laying duck in the lake areas in southward of China. In the laying duck breeding areas such as Honghu, Jianli, Xiantao, Tianmen and Hanchuan citys in Hubei Province, the culturists are used to feeding fresh pondweeds to the laying ducks. The yolk of duck's eggs is natural red with the chrominance reaching up to and/or above RCF (Roche Yolk Color Fan) 15. The red pigment components of natural red yolk of duck's eggs were separated and identified by thin layer chromatography (TLC), high performance liquid chromatography-mass spectrometry-mass spectrometry (HPLC-MS-MS) and high resolution electron impact-mass spectrometry (EI-MS). Four isomers of red pigments were separated by HPLC on a RP-C18 column with methanol-water (99.5:0.5, v/v) as mobile phase. The lambda(max) of the four components were 482, 488, 496, 501 nm, respectively, and all of them were single peak on chromatogram. They had the same molecular mass (Mr = 562), and had the same fragment peaks of MS2 with rhodoxanthin. The molecular formula of red pigments was determined as C40H50O2 by high resolution EI-MS. The results indicate that the red pigment is rhodoxanthin, and they are all cis-isomers of rhodoxanthin.

  9. Phytochemical Analysis of Pfaffia glomerata Inflorescences by LC-ESI-MS/MS

    Directory of Open Access Journals (Sweden)

    Daniele F. Felipe

    2014-09-01

    Full Text Available Pfaffia glomerata contains high levels of β-ecdysone, which has shown a range of beneficial pharmacological effects. The present study demonstrated that inflorescences of P. glomerata contain other important bioactive compounds in addition to β-ecdysone. The identification of compounds from inflorescences using liquid chromatography coupled with electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS was performed for the first time. The eight compounds identified were β-ecdysone, flavonoid glycosides such as quercetin-3-O-glucoside, kaempferol-3-O-glucoside and kaempferol-3-O-(6-p-coumaroyl-glucoside, oleanane-type triterpenoid saponins such as ginsenoside Ro and chikusetsusaponin IV, in addition to oleanonic acid and gluconic acid. This study provided information on the phytochemicals contained in P. glomerata inflorescences revealing the potential application of this plant part as raw material for the phytotherapeutic and cosmetic industries.

  10. Shotgun proteomics of plant plasma membrane and microdomain proteins using nano-LC-MS/MS.

    Science.gov (United States)

    Takahashi, Daisuke; Li, Bin; Nakayama, Takato; Kawamura, Yukio; Uemura, Matsuo

    2014-01-01

    Shotgun proteomics allows the comprehensive analysis of proteins extracted from plant cells, subcellular organelles, and membranes. Previously, two-dimensional gel electrophoresis-based proteomics was used for mass spectrometric analysis of plasma membrane proteins. In order to get comprehensive proteome profiles of the plasma membrane including highly hydrophobic proteins with a number of transmembrane domains, a mass spectrometry-based shotgun proteomics method using nano-LC-MS/MS for proteins from the plasma membrane proteins and plasma membrane microdomain fraction is described. The results obtained are easily applicable to label-free protein semiquantification.

  11. Multiresidue method for pesticide residue analysis in food of animal and plant origin based on GC or LC and MS or MS/MS.

    Science.gov (United States)

    Muñoz, Eva; Muñoz, Gloria; Pineda, Laura; Serrahima, Eulalia; Centrich, Francesc

    2012-01-01

    A multiresidue method based on GC or LC and MS or MS/MS for the determination of 204 pesticides in diverse food matrixes of animal and plant origin is described. The method can include different stages of cleanup according to the chemical characteristics of each sample. Samples were extracted using accelerated solvent extraction. Those with a high fat content or that contained chlorophyll required further purification by gel permeation chromatography and/or SPE (ENVI-Carb). The methodology developed here was fully validated; the LOQs for the 204 pesticides are presented. The LOQ values lie between 0.01 to 0.02 mg/kg. However, in some cases, mainly in baby food, they were as low as 0.003 mg/kg, thereby meeting European Union requirements on maximum residue levels for pesticides, as outlined in European regulation 396/2005 and the Commission Directive 2003/13/EC. The procedure has been accredited for a wide scope of pesticides and matrixes by the Spanish Accreditation Body (ENAC) following ISO/IEC 17025:2005, as outlined in ENAC technical note NT-19.

  12. HPLC-ESI-MS/MS analysis of oxidized di-caffeoylquinic acids generated by metalloporphyrin-catalyzed reactions

    International Nuclear Information System (INIS)

    Santos, Michel D.; Lopes, Norberto P.; Iamamoto, Yassuko

    2008-01-01

    This paper reports an HPLC-ESI-MS/MS investigation on the oxidation of 3,5- and 4,5- dicaffeoylquinic acid using iron(III) tetraphenylporphyrin chloride as catalyst. Two major mono-oxidised products of the quinic acid moiety have been identified for both compounds. However, only the 4,5-derivative afforded two different tri-oxo products. Thus, it seems that the oxidation pattern depends on the number and positions of the caffeic acid moieties present in caffeoylquinic acid molecules. (author)

  13. HPLC-ESI-MS/MS analysis of oxidized di-caffeoylquinic acids generated by metalloporphyrin-catalyzed reactions

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Michel D.; Lopes, Norberto P. [Universidade de Sao Paulo (USP), Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas. Dept. de Fisica e Quimica]. E-mail: npelopes@fcfrp.usp.br; Iamamoto, Yassuko [Universidade de Sao Paulo (USP), Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas. Dept. de Quimica

    2008-07-01

    This paper reports an HPLC-ESI-MS/MS investigation on the oxidation of 3,5- and 4,5- dicaffeoylquinic acid using iron(III) tetraphenylporphyrin chloride as catalyst. Two major mono-oxidised products of the quinic acid moiety have been identified for both compounds. However, only the 4,5-derivative afforded two different tri-oxo products. Thus, it seems that the oxidation pattern depends on the number and positions of the caffeic acid moieties present in caffeoylquinic acid molecules. (author)

  14. Social cognition in pediatric-onset multiple sclerosis (MS).

    Science.gov (United States)

    Charvet, L E; Cleary, R E; Vazquez, K; Belman, A L; Krupp, L B

    2014-10-01

    Pediatric-onset multiple sclerosis (MS) patients represent a subpopulation who are diagnosed during the course of development. Social cognitive deficits have recently been recognized in adults with MS. It is critical to identify whether these youngest patients with the disorder are also at risk. To determine whether pediatric-onset MS is associated with social cognitive deficits. Consecutively-recruited participants with pediatric-onset MS were compared to a group of age- and gender-matched healthy controls on Theory of Mind (ToM) task performance. Tasks measured facial affect recognition (Reading the Mind in the Eyes Test), detecting social faux pas (Faux Pas Test), and understanding the perspective of another (False Beliefs Task). Twenty-eight (28) pediatric-onset MS participants (median age 17 years) and 32 healthy controls (median age 16 years) completed the study. The MS participants performed worse than controls on all three ToM tasks: Reading the Mind in the Eyes Test (p = 0.008), the Faux Pas Test (p = 0.009), and the False Beliefs Task (p = 0.06). While more MS than control participants were impaired on a measure of information processing speed (the Symbol Digit Modalities Test; 38% versus 6%), it did not account for the differences in ToM performance. Social cognition may represent an area of cognitive functioning affected by MS in the pediatric-onset population. These processes are especially important to study in younger patients as they may have long range implications for social adjustment, employment, and well-being. © The Author(s) 2014.

  15. Two-dimensional HPLC coupled to ICP-MS and electrospray ionisation (ESI)-MS/MS for investigating the bioavailability in vitro of arsenic species from edible seaweed

    Energy Technology Data Exchange (ETDEWEB)

    Garcia-Sartal, Cristina; Barciela-Alonso, Maria del Carmen; Bermejo-Barrera, Pilar [University of Santiago de Compostela, Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, Santiago de Compostela (Spain); Taebunpakul, Sutthinun [LGC Limited, Teddington, Middlesex (United Kingdom); Imperial College of Science, Technology and Medicine, South Kensington, Department of Materials, London (United Kingdom); National Institute of Metrology (Thailand), Pathumthani (Thailand); Stokes, Emma; Goenaga-Infante, Heidi [LGC Limited, Teddington, Middlesex (United Kingdom)

    2012-04-15

    Edible seaweed consumption is a route of exposure to arsenic. However, little attention has been paid to estimate the bioaccessibility and/or bioavailability of arsenosugars in edible seaweed and their possible degradation products during gastrointestinal digestion. This work presents first use of combined inductively coupled plasma mass spectroscopy (ICP-MS) with electrospray ionization tandem mass spectrometry (ESI-MS/MS) with two-dimensional HPLC (size exclusion followed by anion exchange) to compare the qualitative and quantitative arsenosugars speciation of different edible seaweed with that of their bioavailable fraction as obtained using an in vitro gastrointestinal digestion procedure. Optimal extraction conditions for As species from four seaweed namely kombu, wakame, nori and sea lettuce were selected as a compromise between As extraction efficiency and preservation of compound identity. For most investigated samples, the use of ammonium acetate buffer as extractant and 1 h sonication in a water bath followed by HPLC-ICP-MS resulted in 40-61% of the total As to be found in the buffered aqueous extract, of which 86-110% was present as arsenosugars (glycerol sugar, phosphate sugar and sulfonate sugar for wakame and kombu and glycerol sugar and phosphate sugar for nori). The exception was sea lettuce, for which the arsenosugar fraction (glycerol sugar, phosphate sugar) only comprised 44% of the total extracted As. Interestingly, the ratio of arsenobetaine and dimethylarsinic acid to arsenosugars in sea lettuce extracts seemed higher than that for the rest of investigated samples. After in vitro gastrointestinal digestion, approximately 11-16% of the total As in the solid sample was found in the dialyzates with arsenosugars comprising 93-120% and 41% of the dialyzable As fraction for kombu, wakame, nori and sea lettuce, respectively. Moreover, the relative As species distribution in seaweed-buffered extracts and dialyzates was found to be very similar

  16. Identification and quantification of cardiac glycosides in blood and urine samples by HPLC/MS/MS.

    Science.gov (United States)

    Guan, F; Ishii, A; Seno, H; Watanabe-Suzuki, K; Kumazawa, T; Suzuki, O

    1999-09-15

    Cardiac glycosides (CG) are of forensic importance because of their toxicity and the fact that very limited methods are available for identification of CG in biological samples. In this study, we have developed an identification and quantification method for digoxin, digitoxin, deslanoside, digoxigenin, and digitoxigenin by high-performance liquid chromatography tandem mass spectrometry (HPLC/MS/MS). CG formed abundant [M + NH4]+ ions and much less abundant [M + H]+ ions as observed with electrospray ionization (ESI) source and ammonium formate buffer. Under mild conditions for collision-induced dissociation (CID), each [M + NH4]+ ion fragmented to produce a dominant daughter ion, which was essential to the sensitive method of selected reaction monitoring (SRM) quantification of CG achieved in this study. SRM was compared with selected ion monitoring (SIM) regarding the effects of sample matrixes on the methodology. SRM produced lower detection limits with biological samples than SIM, while both methods produced equal detection limits with CG standards. On the basis of the HPLC/MS/MS results for CG, we have proposed some generalized points for conducting sensitive SRM measurements, in view of the property of analytes as well as instrumental conditions such as the type of HPLC/MS interface and CID parameters. Analytes of which the molecular ion can produce one abundant daughter ion with high yield under CID conditions may be sensitively measured by SRM. ESI is the most soft ionization source developed so far and can afford formation of the fragile molecular ions that are necessary for sensitive SRM detection. Mild CID conditions such as low collision energy and low pressure of collision gas favor production of an abundant daughter ion that is essential to sensitive SRM detection. This knowledge may provide some guidelines for conducting sensitive SRM measurements of very low concentrations of drugs or toxicants in biological samples.

  17. Living in the not-yet

    African Journals Online (AJOL)

    2015-03-30

    Mar 30, 2015 ... to read online. ... Bible, within this approach, from an underlying progressive or trajectory hermeneutic (Webb .... John Calvin (2006:62) spoke to this mystery .... by which deification is enjoyed by measures, as Paul says ..... The cloud of unknowing, Harper Collins Spiritual Classics, HarperOne, New York.

  18. LC-MS/MS analysis of uncommon paracetamol metabolites derived through in vitro polymerization and nitration reactions in liquid nitrogen.

    Science.gov (United States)

    Trettin, Arne; Jordan, Jens; Tsikas, Dimitrios

    2014-09-01

    Paracetamol (acetaminophen, APAP) is a commonly used analgesic drug. Known paracetamol metabolites include the glucuronide, sulfate and mercapturate. N-Acetyl-benzoquinonimine (NAPQI) is considered the toxic intermediate metabolite of paracetamol. In vitro and in vivo studies indicate that paracetamol is also metabolized to additional poorly characterized metabolites. For example, metabolomic studies in urine samples of APAP-treated mice revealed metabolites such as APAP-sulfate-APAP and APAP-S-S-APAP in addition to the classical phase II metabolites. Here, we report on the development and application of LC-MS and LC-MS/MS approaches to study reactions of unlabelled and (2)H-labelled APAP with unlabelled and (15)N-labelled nitrite in aqueous phosphate buffers (pH 7.4) upon their immersion into liquid nitrogen (-196°C). In mechanistic studies, these reactions were also studied in aqueous buffer prepared in (18)O-labelled water. LC-MS and LC-MS/MS analyses were performed on a reverse-phase material (C18) using gradient elution (2mM ammonium acetate/acetonitrile), in positive and negative electrospray mode. We identified a series of APAP metabolites including di-, tri- and tetra-APAP, mono- and di-nitro-APAP and nitric ester of di-APAP. Our study indicates that nitrite induces oxidation, i.e., polymerization and nitration of APAP, when buffered APAP/nitrite solutions are immersed into liquid nitrogen. These reactions are specific for nitrite with respect to nitrate and do not proceed via intermediate formation of NAPQI. Potassium ions and physiological saline but not thiols inhibit nitrite- and shock-freeze-induced reactions of paracetamol. The underlying mechanism likely involves in situ formation of NO2 radicals from nitrite secondary to profound pH reduction (down to pH 1) and disproportionation. Polymeric paracetamol species can be analyzed as pentafluorobenzyl derivatives by LC-MS but not by GC-MS. Copyright © 2013 Elsevier B.V. All rights reserved.

  19. Can we trust mass spectrometry for determination of arsenic peptides in plants: comparison of LC-ICP-MS and LC-ES-MS/ICP-MS with XANES/EXAFS in analysis of Thunbergia alata.

    Science.gov (United States)

    Bluemlein, Katharina; Raab, Andrea; Meharg, Andrew A; Charnock, John M; Feldmann, Jörg

    2008-04-01

    The weakest step in the analytical procedure for speciation analysis is extraction from a biological material into an aqueous solution which undergoes HPLC separation and then simultaneous online detection by elemental and molecular mass spectrometry (ICP-MS/ES-MS). This paper describes a study to determine the speciation of arsenic and, in particular, the arsenite phytochelatin complexes in the root from an ornamental garden plant Thunbergia alata exposed to 1 mg As L(-1) as arsenate. The approach of formic acid extraction followed by HPLC-ES-MS/ICP-MS identified different As(III)-PC complexes in the extract of this plant and made their quantification via sulfur (m/z 32) and arsenic (m/z 75) possible. Although sulfur sensitivity could be significantly increased when xenon was used as collision gas in ICP-qMS, or when HR-ICP-MS was used in medium resolution, the As:S ratio gave misleading results in the identification of As(III)-PC complexes due to the relatively low resolution of the chromatography system in relation to the variety of As-peptides in plants. Hence only the parallel use of ES-MS/ICP-MS was able to prove the occurrence of such arsenite phytochelatin complexes. Between 55 and 64% of the arsenic was bound to the sulfur of peptides mainly as As(III)(PC(2))(2), As(III)(PC(3)) and As(III)(PC(4)). XANES (X-ray absorption near-edge spectroscopy) measurement, using the freshly exposed plant root directly, confirmed that most of the arsenic is trivalent and binds to S of peptides (53% As-S) while 38% occurred as arsenite and only 9% unchanged as arsenate. EXAFS data confirmed that As-S and As-O bonds occur in the plants. This study confirms, for the first time, that As-peptides can be extracted by formic acid and chromatographically separated on a reversed-phase column without significant decomposition or de-novo synthesis during the extraction step.

  20. Simple and rapid LC-MS/MS method for the absolute determination of cetuximab in human serum using an immobilized trypsin.

    Science.gov (United States)

    Shibata, Kaito; Naito, Takafumi; Okamura, Jun; Hosokawa, Seiji; Mineta, Hiroyuki; Kawakami, Junichi

    2017-11-30

    Proteomic approaches using liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) without an immunopurification technique have not been applied to the determination of serum cetuximab. This study developed a simple and rapid LC-MS/MS method for the absolute determination of cetuximab in human serum and applied it to clinical settings. Surrogate peptides derived from cetuximab digests were selected using a Fourier transform mass spectrometer. Reduced-alkylated serum cetuximab without immunopurification was digested for 20minutes using immobilized trypsin, and the digestion products were purified by solid-phase extraction. The LC-MS/MS was run in positive ion multiple reaction monitoring mode. This method was applied to the determination of serum samples in head and neck cancer patients treated with cetuximab. The chromatographic run time was 10minutes and no peaks interfering with surrogate peptides in serum digestion products were observed. The calibration curve of absolute cetuximab in serum was linear over the concentration range of 4-200μg/mL. The lower limit of quantification of cetuximab in human serum was 4μg/mL. The intra-assay and inter-assay precision and accuracy were less than 13.2% and 88.0-100.7%, respectively. The serum concentration range of cetuximab was 19-140μg/mL in patients. The serum cetuximab concentrations in LC-MS/MS were correlated with those in ELISA (r=0.899, P <0.01) and the mean bias was 1.5% in cancer patients. In conclusion, the present simple and rapid method with acceptable analytical performance can be helpful for evaluating the absolute concentration of serum cetuximab in clinical settings. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. UPLC-MS/MS-Based Profiling of Eicosanoids in RAW264.7 Cells Treated with Lipopolysaccharide

    Directory of Open Access Journals (Sweden)

    Jae Won Lee

    2016-04-01

    Full Text Available While both the pro- and anti-inflammatory effects of several eicosanoids have been widely studied, the degree of inflammation in cells that results from various eicosanoids has yet to be comprehensively studied. The objective of this study was to assess the effect of lipopolysaccharide (LPS treatment on eicosanoid content in RAW264.7 cells. An Ultra performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS-based profiling method was used to analyze the eicosanoid contents of RAW264.7 cells treated with different LPS concentrations. The profiling data were subjected to statistical analyses, such as principal component analysis (PCA and hierarchical clustering analysis. LPS treatment increased nitric oxide production and secretion of pro-inflammatory cytokines, such as tumor necrosis factor-α and interleukin-6, in a concentration-dependent manner. In total, 79 eicosanoids were identified in the cells. RAW264.7 cells treated with different LPS concentrations were well differentiated in the PCA score plot. A heatmap was used to identify the eicosanoids that were up- or down-regulated according to the degree of inflammation and LPS concentration. Thirty-nine eicosanoids were upregulated and seven were down-regulated by LPS treatment in a concentration-dependent manner. Our novel UPLC-MS/MS technique can profile eicosanoids, and can evaluate the correlations between inflammation and eicosanoid metabolism.

  2. Software Tools and Approaches for Compound Identification of LC-MS/MS Data in Metabolomics

    Directory of Open Access Journals (Sweden)

    Ivana Blaženović

    2018-05-01

    Full Text Available The annotation of small molecules remains a major challenge in untargeted mass spectrometry-based metabolomics. We here critically discuss structured elucidation approaches and software that are designed to help during the annotation of unknown compounds. Only by elucidating unknown metabolites first is it possible to biologically interpret complex systems, to map compounds to pathways and to create reliable predictive metabolic models for translational and clinical research. These strategies include the construction and quality of tandem mass spectral databases such as the coalition of MassBank repositories and investigations of MS/MS matching confidence. We present in silico fragmentation tools such as MS-FINDER, CFM-ID, MetFrag, ChemDistiller and CSI:FingerID that can annotate compounds from existing structure databases and that have been used in the CASMI (critical assessment of small molecule identification contests. Furthermore, the use of retention time models from liquid chromatography and the utility of collision cross-section modelling from ion mobility experiments are covered. Workflows and published examples of successfully annotated unknown compounds are included.

  3. HPLC-ESI-MS/MS analysis of oxidized di-caffeoylquinic acids generated by metalloporphyrin-catalyzed reactions

    Directory of Open Access Journals (Sweden)

    Michel D. Santos

    2008-01-01

    Full Text Available This paper reports an HPLC-ESI-MS/MS investigation on the oxidation of 3,5- and 4,5- dicaffeoylquinic acid using iron(III tetraphenylporphyrin chloride as catalyst. Two major mono-oxidised products of the quinic acid moiety have been identified for both compounds. However, only the 4,5-derivative afforded two different tri-oxo products. Thus, it seems that the oxidation pattern depends on the number and positions of the caffeic acid moieties present in caffeoylquinic acid molecules.

  4. Structure and dynamics of the gp120 V3 loop that confers noncompetitive resistance in R5 HIV-1(JR-FL to maraviroc.

    Directory of Open Access Journals (Sweden)

    Yuzhe Yuan

    Full Text Available Maraviroc, an (HIV-1 entry inhibitor, binds to CCR5 and efficiently prevents R5 human immunodeficiency virus type 1 (HIV-1 from using CCR5 as a coreceptor for entry into CD4(+ cells. However, HIV-1 can elude maraviroc by using the drug-bound form of CCR5 as a coreceptor. This property is known as noncompetitive resistance. HIV-1(V3-M5 derived from HIV-1(JR-FLan is a noncompetitive-resistant virus that contains five mutations (I304V/F312W/T314A/E317D/I318V in the gp120 V3 loop alone. To obtain genetic and structural insights into maraviroc resistance in HIV-1, we performed here mutagenesis and computer-assisted structural study. A series of site-directed mutagenesis experiments demonstrated that combinations of V3 mutations are required for HIV-1(JR-FLan to replicate in the presence of 1 µM maraviroc, and that a T199K mutation in the C2 region increases viral fitness in combination with V3 mutations. Molecular dynamic (MD simulations of the gp120 outer domain V3 loop with or without the five mutations showed that the V3 mutations induced (i changes in V3 configuration on the gp120 outer domain, (ii reduction of an anti-parallel β-sheet in the V3 stem region, (iii reduction in fluctuations of the V3 tip and stem regions, and (iv a shift of the fluctuation site at the V3 base region. These results suggest that the HIV-1 gp120 V3 mutations that confer maraviroc resistance alter structure and dynamics of the V3 loop on the gp120 outer domain, and enable interactions between gp120 and the drug-bound form of CCR5.

  5. Analytical Method Details (MS): SE57_MS01 [Metabolonote[Archive

    Lifescience Database Archive (English)

    Full Text Available TQD, UPLC (Waters) UPLC-QTOF-MS ESI N.A. All the solutions of authentic....1% formic acid), with a 2.5 min cycle in the isocratic mode. The ionized authentic compounds were detected ... optimal CV and CE were determined automatically for 497 of these compounds using the software QuanOptimize

  6. An analytical approach based on ESI-MS, LC-MS and PCA for the quali-quantitative analysis of cycloartane derivatives in Astragalus spp.

    Science.gov (United States)

    Napolitano, Assunta; Akay, Seref; Mari, Angela; Bedir, Erdal; Pizza, Cosimo; Piacente, Sonia

    2013-11-01

    Astragalus species are widely used as health foods and dietary supplements, as well as drugs in traditional medicine. To rapidly evaluate metabolite similarities and differences among the EtOH extracts of the roots of eight commercial Astragalus spp., an approach based on direct analyses by ESI-MS followed by PCA of ESI-MS data, was carried out. Successively, quali-quantitative analyses of cycloartane derivatives in the eight Astragalus spp. by LC-ESI-MS(n) and PCA of LC-ESI-MS data were performed. This approach allowed to promptly highlighting metabolite similarities and differences among the various Astragalus spp. PCA results from LC-ESI-MS data of Astragalus samples were in reasonable agreement with both PCA results of ESI-MS data and quantitative results. This study affords an analytical method for the quali-quantitative determination of cycloartane derivatives in herbal preparations used as health and food supplements. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. Improvement of the M/S manipulator maintenance at OSL

    International Nuclear Information System (INIS)

    Kuwana, Koichi; Ouchi, Hiroshi; Ito, Yutaka; Sato, Yoshihiro; Midorikawa, Mituhiro; Hayakawa, Tuyoshi

    2010-01-01

    The safeguards inspection samples from the JNFL Rokkasho Reprocessing Plant (RRP) are received and analyzed at the On Site Laboratory (OSL). Since the samples from the input accountancy tank of the RRP contain a lot of fission products, they are treated in a hot-cell line with a M/S (Master /Slave) manipulator. Special equipment and tools were used for the maintenance of the M/S manipulator, especially for the exchange of the M/S manipulator. However, the manipulator exchange work was not easy due to the limitation of the space in the OSL. For solution to this problem, a monorail and monorail hoist equipment was installed onto wall surface of analytical room close to each M/S manipulator, and then it made the exchange of M/S manipulator easy without special equipment and tools. Additionally, operator was freed from the burden of working space arranging for the exchange of M/S manipulator such as removing of analytical equipments. This report represents the improvement of operation for the exchange of M/S manipulator with installation of monorail and hoist equipment. (author)

  8. Spiritual Leadership: How Does the Spirit Move You?

    Science.gov (United States)

    1992-06-05

    our state of hunger . An Egyptian found in a field was taken before King David, who instructed that he be fed before questioning so that his spirit would...personality. A professor of neuropsychology at the 86 James MacGregor Burns, Leadership New York: Harper Colophon Books, Harper and Row Publishers

  9. Laser ablation ICP-MS for quantitative biomedical applications

    International Nuclear Information System (INIS)

    Konz, Ioana; Fernandez, Beatriz; Fernandez, M.L.; Pereiro, Rosario; Sanz-Medel, Alfredo

    2012-01-01

    LA-ICP-MS allows precise, relatively fast, and spatially resolved measurements of elements and isotope ratios at trace and ultratrace concentration levels with minimal sample preparation. Over the past few years this technique has undergone rapid development, and it has been increasingly applied in many different fields, including biological and medical research. The analysis of essential, toxic, and therapeutic metals, metalloids, and nonmetals in biomedical tissues is a key task in the life sciences today, and LA-ICP-MS has proven to be an excellent complement to the organic MS techniques that are much more commonly employed in the biomedical field. In order to provide an appraisal of the fast progress that is occurring in this field, this review critically describes new developments for LA-ICP-MS as well as the most important applications of LA-ICP-MS, with particular emphasis placed on the quantitative imaging of elements in biological tissues, the analysis of heteroatom-tagged proteins after their separation and purification by gel electrophoresis, and the analysis of proteins that do not naturally have ICP-MS-detectable elements in their structures, thus necessitating the use of labelling strategies. (orig.)

  10. Simultaneous and Sequential MS/MS Scan Combinations and Permutations in a Linear Quadrupole Ion Trap.

    Science.gov (United States)

    Snyder, Dalton T; Szalwinski, Lucas J; Cooks, R Graham

    2017-10-17

    Methods of performing precursor ion scans as well as neutral loss scans in a single linear quadrupole ion trap have recently been described. In this paper we report methodology for performing permutations of MS/MS scan modes, that is, ordered combinations of precursor, product, and neutral loss scans following a single ion injection event. Only particular permutations are allowed; the sequences demonstrated here are (1) multiple precursor ion scans, (2) precursor ion scans followed by a single neutral loss scan, (3) precursor ion scans followed by product ion scans, and (4) segmented neutral loss scans. (5) The common product ion scan can be performed earlier in these sequences, under certain conditions. Simultaneous scans can also be performed. These include multiple precursor ion scans, precursor ion scans with an accompanying neutral loss scan, and multiple neutral loss scans. We argue that the new capability to perform complex simultaneous and sequential MS n operations on single ion populations represents a significant step in increasing the selectivity of mass spectrometry.

  11. Multidimensional protein fractionation of blood proteins coupled to data-independent nanoLC-MS/MS analysis.

    Science.gov (United States)

    Levin, Yishai; Jaros, Julian A J; Schwarz, Emanuel; Bahn, Sabine

    2010-01-03

    In order to exploit human blood as a source of protein disease biomarkers, robust analytical methods are needed to overcome the inherent molecular complexity of this bio-fluid. We present the coupling of label-free SAX chromatography and IMAC to a data-independent nanoLC-MS/MS (nanoLC-MS(E)) platform for analysis of blood plasma and serum proteins. The methods were evaluated using protein standards added at different concentrations to two groups of samples. The results demonstrate that both techniques enable accurate protein quantitation using low sample volumes and a minimal number of fractions. Combining both methods, 883 unique proteins were identified, of which 423 proteins showed high reproducibility. The two approaches resulted in identification of unique molecular signatures with an overlap of approximately 30%, thus providing complimentary information on sub-proteomes. These methods are potentially useful for systems biology, biomarker discovery, and investigation of phosphoproteins in blood. (c) 2009 Elsevier B.V. All rights reserved.

  12. Teaching Bibliometric Analysis and MS/DOS Commands.

    Science.gov (United States)

    Dou, Henri; And Others

    1988-01-01

    Outlines the steps involved in bibliometric studies, and demonstrates the ability to execute simple studies on microcomputers by downloading files using only the capability of MS/DOS. Detailed illustrations of the MS/DOS commands used are provided. (eight references) (CLB)

  13. Simultaneous quantitation of multiple contraceptive hormones in human serum by LC-MS/MS.

    Science.gov (United States)

    Blue, Steven W; Winchell, Andrea J; Kaucher, Amy V; Lieberman, Rachel A; Gilles, Christopher T; Pyra, Maria N; Heffron, Renee; Hou, Xuanlin; Coombs, Robert W; Nanda, Kavita; Davis, Nicole L; Kourtis, Athena P; Herbeck, Joshua T; Baeten, Jared M; Lingappa, Jairam R; Erikson, David W

    2018-04-01

    The objective was to develop a method to simultaneously quantify five commonly used hormonal contraceptives (HCs) and two endogenous sex steroids by liquid chromatography-tandem triple quadrupole mass spectrometry (LC-MS/MS) and apply this method to human serum samples. We developed a method to simultaneously analyze ethinyl estradiol (EE2), etonogestrel (ENG), levonorgestrel (LNG), medroxyprogesterone acetate (MPA) and norethisterone (NET), along with estradiol (E2) and progesterone (P4), in human serum for a Shimadzu Nexera-LCMS-8050 LC-MS/MS platform. We analyzed serum collected from women self-reporting use of oral contraceptives, contraceptive implants or injectable contraceptives (n=14) and normally cycling women using no HC (n=15) as well as pooled samples from women administered various HCs (ENG, n=6; LNG, n=14; MPA, n=7; NET, n=5). Limits of quantitation were 0.010ng/mL for E2, EE2 and P4; 0.020ng/mL for ENG, LNG and MPA; and 0.040ng/mL for NET. Precisions for all assays, as indicated by coefficient of variation, were less than or equal to 12.1%. Accuracies for all assays were in the range of 95%-108%. Endogenous hormone values obtained from analysis of human serum samples are in agreement with levels previously reported in the literature for normally cycling women as well as for women taking the appropriate HC. We have developed a robust, accurate and sensitive method for simultaneously analyzing commonly used contraceptive steroids and endogenous sex steroids in human serum. This analytical method can be used for quantitating contraceptive steroid levels in women for monitoring systemic exposure to determine drug interactions, nonadherence, misreporting and proper dosing. Copyright © 2018 Elsevier Inc. All rights reserved.

  14. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... Brochure Working with MS (.pdf) Download Brochure Taming Stress (.pdf) Download Brochure Multiple Sclerosis and Your Emotions (.pdf) Download Brochure Disease Modifying Therapies Overview (.pdf) ...

  15. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... Privacy Policy Site Map Site Tour Contact Us For Professionals Researchers Physicians Nurses Rehabilitation Professionals Mental Health Professionals Health and Wellness Professionals What Is MS? ...

  16. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... About the Society Vision Careers Leadership Cultural Values Financials News Press Room MS Prevalence Charitable Ratings Corporate Support Helpful Links Donate Society Store MSConnection Blog ...

  17. Fast Simultaneous Determination of 13 Nucleosides and Nucleobases in Cordyceps sinensis by UHPLC–ESI–MS/MS

    Directory of Open Access Journals (Sweden)

    Shi-Yu Zong

    2015-12-01

    Full Text Available A reliable ultra-high-performance liquid chromatography–electrospray ionization–tandem mass spectrometry (UHPLC–ESI–MS/MS method for the fast simultaneous determination of 13 nucleosides and nucleobases in Cordyceps sinensis (C. sinensis with 2-chloroadenosine as internal standard was developed and validated. Samples were ultrasonically extracted in an ice bath thrice, and the optimum analyte separation was performed on an ACQUITY UPLCTM HSS C18 column (100 mm × 2.1 mm, 1.8 μm with gradient elution. All targeted analytes were separated in 5.5 min. Furthermore, all calibration curves showed good linear regression (r > 0.9970 within the test ranges, and the limits of quantitation and detection of the 13 analytes were less than 150 and 75 ng/mL, respectively. The relative standard deviations (RSDs of intra- and inter-day precisions were <6.23%. Recoveries of the quantified analytes ranged within 85.3%–117.3%, with RSD < 6.18%. The developed UHPLC–ESI–MS/MS method was successfully applied to determine nucleosides and nucleobases in 11 batches of C. sinensis samples from different regions in China. The range for the total content in the analyzed samples was 1329–2057 µg/g.

  18. Simultaneous Determination of 11 Compounds in Gualou Guizhi Granule and Pharmacokinetics Study by UPLC-MS/MS

    Directory of Open Access Journals (Sweden)

    Chengtao Sun

    2017-01-01

    Full Text Available A rapid and sensitive ultrafast performance liquid chromatography-tandem mass spectrometry method (UPLC-MS/MS was developed for the simultaneous determination of 11 compounds in Gualou Guizhi Granule (GLGZG, including liquiritin, isoliquiritin, liquirtin apioside, isoliquiritin apioside, liquiritigenin, isoliquiritigenin, glycyrrhizic acid, glycyrrhetinic acid, paeoniflorin, albiflorin, and paeoniflorin sulfonate in rat plasma. UPLC-MS/MS assay with negative ion mode was performed on a Waters CORTECS C18 (2.1 × 100 mm, 1.6 μm with the mobile phase consisting of 0.1% aqueous formic acid (A and acetonitrile (B in gradient elution at a flow rate of 0.25 mL·min−1. The method was linear for all analytes within the detection range (r≥0.9597. The inter- and intraday precision (RSD were 2.21–6.41% and 1.67–6.18%; the inter- and intraday accuracy (recover were 92.48–114.03% and 90.23–112.04%. And the recovery rate ranged from 81.30% to 108.22%. The matrix effect values obtained for analytes ranged from 88.91% to 113.32%. This validated method was successfully applied to a pharmacokinetics study in rats after oral administration of GLGZG.

  19. Photolysis of sulfamethoxypyridazine in various aqueous media: Aerobic biodegradation and identification of photoproducts by LC-UV–MS/MS

    Energy Technology Data Exchange (ETDEWEB)

    Khaleel, Nareman D.H., E-mail: drndahshan@yahoo.com [Sustainable Chemistry and Material Resources, Institute of Sustainable and Environmental Chemistry, Leuphana University Lüneburg, C13, DE-21335 Lüneburg (Germany); Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Suez Canal University, Ismailia 41522 (Egypt); Mahmoud, Waleed M.M. [Sustainable Chemistry and Material Resources, Institute of Sustainable and Environmental Chemistry, Leuphana University Lüneburg, C13, DE-21335 Lüneburg (Germany); Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Suez Canal University, Ismailia 41522 (Egypt); Hadad, Ghada M.; Abdel-Salam, Randa A. [Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Suez Canal University, Ismailia 41522 (Egypt); Kümmerer, Klaus, E-mail: Klaus.Kuemmerer@uni.leuphana.de [Sustainable Chemistry and Material Resources, Institute of Sustainable and Environmental Chemistry, Leuphana University Lüneburg, C13, DE-21335 Lüneburg (Germany)

    2013-01-15

    Highlights: ► Sulfonamides are one of the most extensively used antibiotics in human and veterinary medicine. ► Sulfamethoxypyridazine (SMP) underwent photodegradation in three different media. ► SMP was not readily biodegradable. ► SMP and some of its degradation products were identified by LC-UV–MS/MS. -- Abstract: Sulfonamides are one of the most frequently used antibiotics worldwide. Therefore, mitigation processes such as abiotic or biotic degradation are of interest. Photodegradation and biodegradation are the potentially significant removal mechanisms for pharmaceuticals in aquatic environments. The photolysis of sulfamethoxypyridazine (SMP) using a medium pressure Hg-lamp was evaluated in three different media: Millipore water pH 6.1 (MW), effluent from sewage treatment plant pH 7.6 (STP), and buffered demineralized water pH 7.4 (BDW). Identification of transformation products (TPs) was performed by LC-UV–MS/MS. The biodegradation of SMP using two tests from the OECD series was studied: Closed Bottle test (OECD 301 D), and Manometric Respirometry test (OECD 301 F). In biodegradation tests, it was found that SMP was not readily biodegradable so it may pose a risk to the environment. The results showed that SMP was removed completely within 128 min of irradiation in the three media, and the degradation rate was different for each investigated type of water. However, dissolved organic carbon (DOC) was not removed in BDW and only little DOC removal was observed in MW and STP, thus indicating the formation of TPs. Analysis by LC-UV–MS/MS revealed new TPs formed. The hydroxylation of SMP represents the main photodegradation pathway.

  20. Photolysis of sulfamethoxypyridazine in various aqueous media: Aerobic biodegradation and identification of photoproducts by LC-UV–MS/MS

    International Nuclear Information System (INIS)

    Khaleel, Nareman D.H.; Mahmoud, Waleed M.M.; Hadad, Ghada M.; Abdel-Salam, Randa A.; Kümmerer, Klaus

    2013-01-01

    Highlights: ► Sulfonamides are one of the most extensively used antibiotics in human and veterinary medicine. ► Sulfamethoxypyridazine (SMP) underwent photodegradation in three different media. ► SMP was not readily biodegradable. ► SMP and some of its degradation products were identified by LC-UV–MS/MS. -- Abstract: Sulfonamides are one of the most frequently used antibiotics worldwide. Therefore, mitigation processes such as abiotic or biotic degradation are of interest. Photodegradation and biodegradation are the potentially significant removal mechanisms for pharmaceuticals in aquatic environments. The photolysis of sulfamethoxypyridazine (SMP) using a medium pressure Hg-lamp was evaluated in three different media: Millipore water pH 6.1 (MW), effluent from sewage treatment plant pH 7.6 (STP), and buffered demineralized water pH 7.4 (BDW). Identification of transformation products (TPs) was performed by LC-UV–MS/MS. The biodegradation of SMP using two tests from the OECD series was studied: Closed Bottle test (OECD 301 D), and Manometric Respirometry test (OECD 301 F). In biodegradation tests, it was found that SMP was not readily biodegradable so it may pose a risk to the environment. The results showed that SMP was removed completely within 128 min of irradiation in the three media, and the degradation rate was different for each investigated type of water. However, dissolved organic carbon (DOC) was not removed in BDW and only little DOC removal was observed in MW and STP, thus indicating the formation of TPs. Analysis by LC-UV–MS/MS revealed new TPs formed. The hydroxylation of SMP represents the main photodegradation pathway

  1. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... Webinar Series Momentum Magazine Educational Videos Knowledge Is Power Live Fully, Live Well Everyday Matters Resilience: Addressing the Challenges of MS You CAN! Webcasts DVDs Books ...

  2. Misleading measures in Vitamin D analysis: A novel LC-MS/MS assay to account for epimers and isobars

    Directory of Open Access Journals (Sweden)

    Petroczi Andrea

    2011-05-01

    Full Text Available Abstract Background Recently, the accuracies of many commercially available immunoassays for Vitamin D have been questioned. Liquid chromatography tandem mass spectrometry (LC- MS/MS has been shown to facilitate accurate separation and quantification of the major circulating metabolite 25-hydroxyvitamin-D3 (25OHD3 and 25-hydroxyvitamin-D2 (25OHD2 collectively termed as 25OHD. However, among other interferents, this method may be compromised by overlapping peaks and identical masses of epimers and isobars, resulting in inaccuracies in circulating 25OHD measurements. The aim of this study was to develop a novel LC-MS/MS method that can accurately identify and quantitate 25OHD3 and 25OHD2 through chromatographic separation of 25OHD from its epimers and isobars. Methods A positive ion electrospray ionisation (ESI LC-MS/MS method was used in the Multiple Reaction Monitoring (MRM mode for quantification. It involved i liquid-liquid extraction, ii tandem columns (a high resolution ZORBAX C18 coupled to an ULTRON chiral, with guard column and inlet filter, iii Stanozolol-D3 as internal standard, and iv identification via ESI and monitoring of three fragmentation transitions. To demonstrate the practical usefulness of our method, blood samples were collected from 5 healthy male Caucasian volunteers; age range 22 to 37 years and 25OHD2, 25OHD3 along with co-eluting epimers and analogues were quantified. Results The new method allowed chromatographic separation and quantification of 25OHD2, 25OHD3, along with 25OHD3 epimer 3-epi-25OHD3 and isobars 1-α-hydroxyvitamin-D3 (1αOHD3, and 7-α-hydroxy-4-cholesten-3-one (7αC4. The new assay was capable of detecting 0.25 ng/mL of all analytes in serum. Conclusions To our knowledge, this is the first specific, reliable, reproducible and robust LC-MS/MS method developed for the accurate detection of 25OHD (Vitamin D. The method is capable of detecting low levels of 25OHD3 and 25OHD2 together with chromatographic

  3. Russell Brains Review of MS.

    Science.gov (United States)

    Murray, Tj

    2011-05-01

    In 1930 there were many conflicting views on the cause, incidence, precipitating factors, inheritance and treatment of multiple sclerosis (MS). A young, London neurologist summarized the state of understanding of the disease with his personal view of many of the uncertain areas, and clarified the thinking for the neurological community at that time. Although his later career was influential in many fields of medicine, and his personal influence was extraordinary in many areas as an author, educator, administrator, opinion leader and historian, his review was an important milestone in the history of MS.

  4. Evaluation of VITEK mass spectrometry (MS), a matrix-assisted laser desorption ionization time-of-flight MS system for identification of anaerobic bacteria.

    Science.gov (United States)

    Lee, Wonmok; Kim, Myungsook; Yong, Dongeun; Jeong, Seok Hoon; Lee, Kyungwon; Chong, Yunsop

    2015-01-01

    By conventional methods, the identification of anaerobic bacteria is more time consuming and requires more expertise than the identification of aerobic bacteria. Although the matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) systems are relatively less studied, they have been reported to be a promising method for the identification of anaerobes. We evaluated the performance of the VITEK MS in vitro diagnostic (IVD; 1.1 database; bioMérieux, France) in the identification of anaerobes. We used 274 anaerobic bacteria isolated from various clinical specimens. The results for the identification of the bacteria by VITEK MS were compared to those obtained by phenotypic methods and 16S rRNA gene sequencing. Among the 249 isolates included in the IVD database, the VITEK MS correctly identified 209 (83.9%) isolates to the species level and an additional 18 (7.2%) at the genus level. In particular, the VITEK MS correctly identified clinically relevant and frequently isolated anaerobic bacteria to the species level. The remaining 22 isolates (8.8%) were either not identified or misidentified. The VITEK MS could not identify the 25 isolates absent from the IVD database to the species level. The VITEK MS showed reliable identifications for clinically relevant anaerobic bacteria.

  5. Diagnosis and heterogeneity of MS in MRI

    International Nuclear Information System (INIS)

    Holst, B.; Fiehler, J.; Schippling, S.

    2008-01-01

    An efficient therapy of MS requires a quick and reliable diagnosis of the disease. MRI is the most leading paraclinical examination for MS diagnosis. Even though there is no pathognomic finding in MRI, there are MS characteristics with respect to morphology and localization. To exclude other neurological disorders and distinguish between different characteristics within MS, the use of contrast agent is advantageous. Postulated MRI criteria have been increasingly adjusted to the clinical routine and have become clearer, more sensitive, and more specific. Different imaging criteria will be introduced. In addition to the McDonald criteria of 2001 and 2005, new criteria will be presented in which the use of contrast agent is replaced by a second MRI and the dissemination in time and space is simplified. Different pathomechanisms which help to separate MS patients into subgroups are postulated. The diverse pathomechanisms also enable the development of new pharmaceuticals to manipulate the immunologic course in different stages. For varying therapy approaches, it is increasingly important to differentiate the heterogeneous appearance forms into subtypes. The two visible main components of the disorder in MRI are inflammation and neurodegeneration and are responsible for different clinical courses. Both are interdependent and independent of each other. We introduce a stratification which uses both components as a function of their different outcomes to compose subgroups. The previous challenge with respect to MRI was to support the diagnosis of MS via MRI criteria. A future problem will be the heterogeneity and classification of subgroups. This article gives an overview of both problems. (orig.)

  6. A LC-MS-MS method for determination of low doxazosin concentrations in plasma after oral administration to dogs.

    Science.gov (United States)

    Erceg, Marijana; Cindric, Mario; Pozaic Frketic, Lidija; Vertzoni, Maria; Cetina-Cizmek, Biserka; Reppas, Christos

    2010-02-01

    A rapid and sensitive reversed phase liquid chromatography- tandem mass spectrometry (LC-MS-MS) method is developed for the determination of doxazosin in canine plasma. The samples are prepared by precipitation of proteins using a mixture of methanol and acetonitrile, followed by freezing and evaporation of the organic solvent. The remaining dry residue is redissolved in mobile phase and analyzed by LC-MS-MS with positive electrospray ionization using the selected reactions monitoring mode. An XTerra MS C(18) column, a mobile phase composed of acetonitrile and 2mM ammonium acetate with gradient elution, and a flow rate of 400 microL/min are employed. The elution times for prazosin (internal standard) and doxazosin are approximately 8 and 10 min, respectively. Calibration curves are linear in the 1-20 ng/mL concentration range. Limits of detection and quantification are 0.4 ng/mL and 1.2 ng/mL, respectively. Recovery is higher than 94%. Intra- and inter-day relative standard deviations are below 7% and 8%, respectively. The method is applied for the determination of doxazosin plasma levels following a single administration of doxazosin base and doxazosin mesylate tablets (2 mg dose) to dogs in the fed state. The results indicate possible superiority of the mesylate salt on the plasma input rates of doxazosin.

  7. Transgender Policy: What is Fair for All Students?

    Science.gov (United States)

    Kaiser, Matthew M.; Seitz, Keshia M.; Walters, Elizabeth A.

    2014-01-01

    Ritha Smith, assistant superintendent, and Seth Hanson, principal, are faced with a difficult decision. Taylor Harper is a transgender student who identifies as male and is openly attracted to females. Taylor's parents, Lane and Morgan Harper, are lesbians; they are fully supportive of their child's identification and are well versed in their…

  8. Quantification of phytoprostanes - bioactive oxylipins - and phenolic compounds of Passiflora edulis Sims shell using UHPLC-QqQ-MS/MS and LC-IT-DAD-MS/MS.

    Science.gov (United States)

    Medina, Sonia; Collado-González, Jacinta; Ferreres, Federico; Londoño-Londoño, Julián; Jiménez-Cartagena, Claudio; Guy, Alexandre; Durand, Thierry; Galano, Jean-Marie; Gil-Izquierdo, Angel

    2017-08-15

    The genus Passiflora, comprising about 500 species, is the largest in the Passion flower family. Passiflora edulis Sims f. edulis (gulupa) is one of the most important fruits cultivated in Colombia. In recent years and due to its organoleptic and bioactive properties, its exports have significantly increased. In this work, six new bioactive oxylipins -phytoprostanes - were detected in gulupa shell by a UHPLC-QqQ-MS/MS method: F 1t -phytoprostanes and D 1t -phytoprostanes were the predominant and minor classes, respectively. Moreover, the polyphenol profile of the shell was investigated and we were able to detect and quantify phenolic compounds that have not been described previously, like luteolin-8-C-(2-O-rhamnosyl)hexoside and quercetin-3-O-(6″-acetyl)glucosyl-2″-sinapic acid. Consequently, this study provides new insights into the importance of gulupa shell as a valuable option in the design of new beverages rich in antioxidant phytochemicals, as part of a well-balanced diet, and in the process and quality control of such products. Copyright © 2017 Elsevier Ltd. All rights reserved.

  9. Matrix effect in the analysis of drugs of abuse from urine with desorption atmospheric pressure photoionization-mass spectrometry (DAPPI-MS) and desorption electrospray ionization-mass spectrometry (DESI-MS)

    International Nuclear Information System (INIS)

    Suni, Niina M.; Lindfors, Pia; Laine, Olli; Ostman, Pekka; Ojanperae, Ilkka; Kotiaho, Tapio; Kauppila, Tiina J.; Kostiainen, Risto

    2011-01-01

    Highlights: → DAPPI-MS and DESI-MSI in the analysis of drugs of abuse from urine. → DAPPI-MS has better urine matrix tolerance over DESI-MS. → Urine matrix can affect the ionization mechanism in DAPPI. → DAPPI-MS/MS can be used for screening of drugs from urine after sample pretreatment. - Abstract: We have studied the matrix effect within direct analysis of benzodiazepines and opioids from urine with desorption electrospray ionization-mass spectrometry (DESI-MS) and desorption atmospheric pressure photoionization-mass spectrometry (DAPPI-MS). The urine matrix was found to affect the ionization mechanism of the opioids in DAPPI-MS favoring proton transfer over charge exchange reaction. The sensitivity for the drugs in solvent matrix was at the same level with DESI-MS and DAPPI-MS (LODs 0.05-6 μg mL -1 ) but the decrease in sensitivity due to the urine matrix was higher with DESI (typically 20-160-fold) than with DAPPI (typically 2-15-fold) indicating better matrix tolerance of DAPPI over DESI. Also in MS/MS mode, DAPPI provided better sensitivity than DESI for the drugs in urine. The feasibility of DAPPI-MS/MS was then studied in screening the same drugs from five authentic, forensic post mortem urine samples. A reference measurement with gas chromatography-mass spectrometry (GC-MS) (including pretreatment) revealed 16 findings from the samples, whereas with DAPPI-MS/MS after sample pretreatment, 15 findings were made. Sample pretreatment was found necessary, since only eight findings were made from the same samples untreated.

  10. Matrix effect in the analysis of drugs of abuse from urine with desorption atmospheric pressure photoionization-mass spectrometry (DAPPI-MS) and desorption electrospray ionization-mass spectrometry (DESI-MS)

    Energy Technology Data Exchange (ETDEWEB)

    Suni, Niina M.; Lindfors, Pia; Laine, Olli [Division of Pharmaceutical Chemistry, University of Helsinki, P.O. Box 56, Helsinki FI-00014 (Finland); Ostman, Pekka; Ojanperae, Ilkka [Hjelt Institute, Department of Forensic Medicine, University of Helsinki, P.O. Box 40, Helsinki FI-00014 (Finland); Kotiaho, Tapio [Division of Pharmaceutical Chemistry, University of Helsinki, P.O. Box 56, Helsinki FI-00014 (Finland); Laboratory of Analytical Chemistry, Department of Chemistry, University of Helsinki, P.O. Box 55, Helsinki FI-00014 (Finland); Kauppila, Tiina J. [Division of Pharmaceutical Chemistry, University of Helsinki, P.O. Box 56, Helsinki FI-00014 (Finland); Kostiainen, Risto, E-mail: risto.kostiainen@helsinki.fi [Division of Pharmaceutical Chemistry, University of Helsinki, P.O. Box 56, Helsinki FI-00014 (Finland)

    2011-08-05

    Highlights: {yields} DAPPI-MS and DESI-MSI in the analysis of drugs of abuse from urine. {yields} DAPPI-MS has better urine matrix tolerance over DESI-MS. {yields} Urine matrix can affect the ionization mechanism in DAPPI. {yields} DAPPI-MS/MS can be used for screening of drugs from urine after sample pretreatment. - Abstract: We have studied the matrix effect within direct analysis of benzodiazepines and opioids from urine with desorption electrospray ionization-mass spectrometry (DESI-MS) and desorption atmospheric pressure photoionization-mass spectrometry (DAPPI-MS). The urine matrix was found to affect the ionization mechanism of the opioids in DAPPI-MS favoring proton transfer over charge exchange reaction. The sensitivity for the drugs in solvent matrix was at the same level with DESI-MS and DAPPI-MS (LODs 0.05-6 {mu}g mL{sup -1}) but the decrease in sensitivity due to the urine matrix was higher with DESI (typically 20-160-fold) than with DAPPI (typically 2-15-fold) indicating better matrix tolerance of DAPPI over DESI. Also in MS/MS mode, DAPPI provided better sensitivity than DESI for the drugs in urine. The feasibility of DAPPI-MS/MS was then studied in screening the same drugs from five authentic, forensic post mortem urine samples. A reference measurement with gas chromatography-mass spectrometry (GC-MS) (including pretreatment) revealed 16 findings from the samples, whereas with DAPPI-MS/MS after sample pretreatment, 15 findings were made. Sample pretreatment was found necessary, since only eight findings were made from the same samples untreated.

  11. Long-term effects of childbirth in MS

    NARCIS (Netherlands)

    D'hooghe, M.B.; Nagels, G.; Uitdehaag, B.M.J.

    2010-01-01

    Background: The uncertainty about long-term effects of childbirth presents MS patients with dilemmas. Methods: Based on clinical data of 330 female MS patients, the long-term effects of childbirth were analysed, using a cross-sectional study design. Four groups of patients were distinguished: (1)

  12. Bioavailability of Oral Hydrocortisone Corrected for Binding Proteins and Measured by LC-MS/MS Using Serum Cortisol and Salivary Cortisone.

    Science.gov (United States)

    Johnson, T N; Whitaker, M J; Keevil, B; Ross, R J

    2018-01-01

    The assessment absolute bioavailability of oral hydrocortisone is complicated by its saturable binding to cortisol binding globulin (CBG). Previous assessment of bioavailability used a cortisol radioimmunoassay which has cross reactivity with other steroids. Salivary cortisone is a measure of free cortisol and LC-MS/MS is the gold standard method for measuring steroids. We here report the absolute bioavailability of hydrocortisone calculated using serum cortisol and salivary cortisone measured by LC-MS/MS. 14 healthy male dexamethasone suppressed volunteers were administered 20 mg hydrocortisone either intravenously or orally by tablet. Samples of serum and saliva were taken and measured for cortisol and cortisone by LC-MS/MS. Serum cortisol was corrected for saturable binding using published data and pharmacokinetic parameters derived using the program WinNonlin. The mean (95% CI) bioavailability of oral hydrocortisone calculated from serum cortisol, unbound serum cortisol and salivary cortisone was 1.00 (0.89-1.14); 0.88 (0.75-1.05); and 0.93 (0.83-1.05), respectively. The data confirm that, after oral administration, hydrocortisone is completely absorbed. The data derived from serum cortisol corrected for protein binding, and that from salivary cortisone, are similar supporting the concept that salivary cortisone reflects serum free cortisol levels and that salivary cortisone can be used as a non-invasive method for measuring the pharmacokinetics of hydrocortisone.

  13. Quantitation of dialkyl phosphate metabolites of organophosphate pesticides in human urine using GC-MS-MS with isotopic internal standards.

    Science.gov (United States)

    Bravo, Roberto; Driskell, William J; Whitehead, Ralph D; Needham, Larry L; Barr, Dana B

    2002-01-01

    Human exposure to organophosphate pesticides can be estimated from the presence of urinary metabolites. An isotope-dilution gas chromatography-tandem mass spectrometry (GC-MS-MS) method was developed for quantitating the six dialkyl phosphate urinary metabolites of at least 29 organophosphate pesticides. Urine samples were spiked with stable isotope analogues of the dialkyl phosphates, evaporated using azeotropic distillation, followed by chemical derivatization of the metabolites to their respective chloropropyl phosphate esters. The chloropropyl phosphate esters were concentrated and then analyzed using GC-MS-MS. The limits of detection (LODs) of the method were in the low-to-mid picogram-per-milliliter range (parts per trillion) with coefficients of variation of less than 20%. The use of stable isotope analogues as internal standards for each of these metabolites allows for the highest degree of accuracy and precision. Additionally, the low LODs allow the use of this method in general population studies.

  14. Characterization of the Proteome of Theobroma cacao Beans by Nano-UHPLC-ESI MS/MS.

    Science.gov (United States)

    Scollo, Emanuele; Neville, David; Oruna-Concha, M Jose; Trotin, Martine; Cramer, Rainer

    2018-02-01

    Cocoa seed storage proteins play an important role in flavour development as aroma precursors are formed from their degradation during fermentation. Major proteins in the beans of Theobroma cacao are the storage proteins belonging to the vicilin and albumin classes. Although both these classes of proteins have been extensively characterized, there is still limited information on the expression and abundance of other proteins present in cocoa beans. This work is the first attempt to characterize the whole cocoa bean proteome by nano-UHPLC-ESI MS/MS analysis using tryptic digests of cocoa bean protein extracts. The results of this analysis show that >1000 proteins could be identified using a species-specific Theobroma cacao database. The majority of the identified proteins were involved with metabolism and energy. Additionally, a significant number of the identified proteins were linked to protein synthesis and processing. Several proteins were also involved with plant response to stress conditions and defence. Albumin and vicilin storage proteins showed the highest intensity values among all detected proteins, although only seven entries were identified as storage proteins. A comparison of MS/MS data searches carried out against larger non-specific databases confirmed that using a species-specific database can increase the number of identified proteins, and at the same time reduce the number of false positives. The results of this work will be useful in developing tools that can allow the comparison of the proteomic profile of cocoa beans from different genotypes and geographic origins. Data are available via ProteomeXchange with identifier PXD005586. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Use of Tricaine Methanesulfonate (MS222) for Euthanasia of Reptiles

    Science.gov (United States)

    Conroy, CJ; Papenfuss, T; Parker, J; Hahn, NE

    2009-01-01

    Tricaine methanesulfonate (MS222) injected into the intracoelomic cavity of reptiles was evaluated as a chemical euthanasia method. Three western fence lizards, 2 desert iguanas, 4 garter snakes, and 6 geckos were euthanized by intracoelomic injection of 250 to 500 mg/kg of 0.7% to 1% sodium-bicarbonate–buffered MS222 solution followed by intracoelomic injection of 0.1 to 1.0 ml unbuffered 50% (v/v) MS222 solution. A simple 2-stage protocol for euthanasia of reptiles by using MS222 is outlined. In addition, the conditions for safe use of MS222 are discussed. MS222 offers an alternative to sodium pentobarbital for euthanasia of reptiles. PMID:19245747

  16. Microdose study of a P-glycoprotein substrate, fexofenadine, using a non-radioisotope-labelled drug and LC/MS/MS.

    Science.gov (United States)

    Yamazaki, A; Kumagai, Y; Yamane, N; Tozuka, Z; Sugiyama, Y; Fujita, T; Yokota, S; Maeda, M

    2010-04-01

    Fexofenadine is a P-glycoprotein substrate of low bioavailability. It is primarily excreted into faeces as a parent drug via biliary excretion. The predictability from microdose data for the drug absorbed via transporters such as P-glycoprotein is not known. Therefore, this study assessed the predictability of therapeutic-dose pharmacokinetics of fexofenadine from microdosing data using non-radioisotope-labelled drug and liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS). In a single dose, randomized, two-way crossover study, eight subjects received a microdose (100 microg) or a therapeutic dose (60 mg) of fexofenadine. Blood samples were collected until 12 h after dosing, and assayed using LC/MS/MS. Plasma concentration-time curves of fexofenadine between microdose and therapeutic dose were similar. The mean +/- SD of C(max) normalized to 60 mg dose after microdose and therapeutic dose were 379 +/- 147 and 275 +/- 145 ng/mL respectively. The mean AUC(last) normalized to 60 mg dose after microdose and therapeutic dose were 1914 +/- 738 and 1431 +/- 432 ng/h/mL respectively. The mean dose-adjusted C(max) and AUC(last) after microdose were higher compared with those after therapeutic dose. Individual plots of C(max) and AUC(last) normalized to 60 mg dose, were similar for microdose and therapeutic dose. None of the pharmacokinetic parameters were statistically different using anova. Overall, the microdose pharmacokinetics profile was similar to, and hence predictive of, that of the therapeutic dose. For the P-glycoprotein substrate fexofenadine, the predictability of therapeutic-dose pharmacokinetics from microdose data was good. A microdose study using a non-radioisotope-labelled drug and LC/MS/MS is convenient, and has the potential to aid the early selection of drug candidates.

  17. Results of a proficiency test for multi-mycotoxin determination in maize by using methods based on LC-MS/(MS)

    NARCIS (Netherlands)

    Solfrizzo, M.; Girolamo, De A.; Lattanzio, V.M.T.; Visconti, A.; Stroka, J.; Alldrick, A.; Egmond, van H.P.

    2013-01-01

    Liquid chromatography coupled with single or tandem mass spectrometry (LC-MS/(MS)) is routinely used for the simultaneous determination of mycotoxins in food and feed although official methods using this technique have not yet been adopted by the European Committee for Standardization and the

  18. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... Become an MS Activist Take Action Current Advocacy Issues Advocacy Results Advocacy News ... d Give in Honor or Memory d Workplace Giving d Employer Matching Gifts d Gifts of ...

  19. Relapsing-Remitting MS (RRMS)

    Medline Plus

    Full Text Available ... Women's Health Unhealthy Habits Managing MS and Another Condition ... healthcare provider can feel confident that the current treatment regimen is working effectively. How does RRMS differ from progressive types ...

  20. Human radiation studies: Remembering the early years: Oral history of medical physicist Katherine L. Lathrop and physician Paul V. Harper, conducted January 26, 1995

    International Nuclear Information System (INIS)

    1995-09-01

    This report provides a transcript of an interview with Ms. Katherine L. Lathrop and Dr. Paul V. Hopper by representatives of the DOE Office of Human Radiation Research. Ms. Lathrop and Dr. Hopper were chosen for this interview because of their long-standing interest and research experience in the development of nuclear medicine. After brief biographical sketches the researchers provide a broad and interesting description of their roles in the initial uses of many radiopharmaceuticals, their experiences in human experimentation, and interactions with many other pioneers in nuclear medicine

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